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KRC

PRODUCTION & OPERATION NAPHTHA PRETREATMENT SECTION


CCR UNIT

Table of Contents

INTRODUCTION (KRCIM 71100.01)


1. Unit introduction…………………………………………………………………….1
2. Manual Structure……………………………………………………………………1

BASIC KNOWLEDGE (KRCIM 71100.02)


1. Basis of Design……………………………………………………………………..2
2. Unit Description………………………………………………………………….….3
3. Chemistry……………………………………………………………………………4

CATALYST (KRCIM 71100.03)


1. Catalysis And Catalysts…………………………………………… ………….…14
2. Naphtha Hydrotreating Catalyst……………………………………… ………...17
3. Catalyst Loading………………………………………………………… ……….17
4. Catalyst Regeneration…………………………………………………… ……...20
5. Catalyst Unloading for Unregenerate Catalyst…………………… …………..26

START-UP/SHUTDOWN OPERATIONS (KRCIM 71100.04)


1. Start-Up Requirement………………………………………………………….…27
2. Unit Purging………………………………………………………………….…….27
3. Initial Leak Test……………………………………………………………….…...34
4. Unit Drying………………………………………………………………………....36
5. Catalyst Loading…………………………………………………………….…….39
6. Air Freeing and Leak Testing…………………………………………………....39
7. Catalyst Drying………...………………………………………………………….39
8. Catalyst Presulfiding......................................................................................41
9. Establish Normal Operation...........................................................................42
10. Normal Shutdown Procedure........................................................................43

NORMAL OPERATION (KRCIM 71100.05)


1. Operating Conditions.....................................................................................44
2. Process Variables..........................................................................................44
3. Troubleshooting.............................................................................................46
4. Analysis Control.............................................................................................49
KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION INTRODUCTION
CCR UNIT KRCIM 71100.01 REV.0

Contents: This document outlines the structure of CCR (Naphtha Pretreatment


Section) operation manual. The text includes:

1. Unit Introduction
2. Manual Structure

1. Unit Introduction

1.1. General
Continuous Catalytic Reforming Unit (CCR) of Khartoum Refinery Company is built
under the expansion project of the refinery, phase II. The unit is designed by
Sinopec Engineering Incorporation. The process utilizes Axens's "State of the art"
moving catalyst bed with continuous catalyst regeneration.
The unit is designed to process 400,000 metrics tons per year and to operate at a
severity of RON 98 with an on-stream factor of 8000 hours/year.

1.2. Configuration of the Unit


This unit consists of several components, including
 Pretreatment section (unit 71100)
 Reforming section (unit 71200)
 Catalyst regeneration section (unit 71300)
 Utilities section (unit 71400)
 Waste heat boiler section (unit 71500)

2. Manual Structure
The design information and operating instructions of the Continuous Catalytic Reforming
Unit (unit71) are covered by six different volumes as follow:

KRCIM 71100 is dedicated to pretreatment section


KRCIM 71200 is dedicated to reforming section
KRCIM 71300 is dedicated to catalyst regeneration section
KRCIM 71500 is dedicated to waste heat boiler section
KRCIM 71EMP is dedicated to emergency procedures
KRCIM 71TRS is dedicated to test run scheme

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

Contents: This document outlines the general description of naphtha pretreatment


section of CCR unit. The text includes:

1. Basis of Design
2. Unit Description
3. Chemistry

1. Basis Of Design

1.1. Duty Of Unit


The hydrotreating unit aims to the removal of all the impurities from the CCR feed
naphtha as to match reforming unit feedstock specifications. Otherwise, the
poisoning of the reforming precious catalyst will take place.
These impurities are:
- Sulfur, nitrogen, water, and halogen (Fluorine, Chlorine, …)
- Diolefins and olefins
- Metals: arsenic, mercury …

1.2. Feed Specifications


The unit is designed to process 422,000 metric tons per year of mixture of coker
naphtha (80%) and SR naphtha (20%).
The main feed properties are:

Density d4 0.7224

IBP (ASTM ºC) 80 ºC

FBP(ASTM ºC) 180 ºC

Composition (wt %)

Paraffins Naphthenes Aromatics


71.42 22.35 6.23

Impurities (wt ppm)


S=13 N 0.5

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

1.3. Products Specification


 Essentially the treated naphtha (400,000 mt/a) specifications should meet the
reforming feed requirements mentioned in chapter 1.2 of KRCIM 71200.02.
 Light naphtha (22,300 mt/a) from top of stripper will be send to RFCC for
further processing.

1.4. Operating Conditions

1.4.1. Reaction section


 Reaction pressure: 2.5MPa(g)
 Reaction temperature: 340oC
 Reaction space velocity: 6 hour-1 (V)
 Hydrogen to oil ratio: 120 (V)

1.4.2. Pretreatment product separator


 Operation pressure: 2.0MPa(g)
 Operation temperature: 40 oC

1.4.3. Stripping tower


 Operation temperature: 139 oC/241 oC (top/bottom)
 Operation temperature: 1.25MPa(g)(top)
 Reflux ratio: 0.39 (for feed)

2. Unit description
The naphtha coming from GDHT unit first of all enters the pretreatment feed surge drum
D-71100, after which it is pressurized by the pretreatment feed pump P-71101A/B.
Naphtha will be blended with the hydrogen rich gas that comes from the pretreatment
recycle compressor K-71101A/B, and then enters the pretreatment reactor R-71101 after
exchanging heat with the reactor product in E-71101A/B and heated to the reaction
temperature by the heating furnace F-71101. With the action of the catalyst; sulfur,
nitrogen and unsaturated olefins in the naphtha will react with hydrogen to give rise to
hydrogen sulfide, ammonia, and saturated hydrocarbons. While the metal impurities will
be adsorbed onto the catalyst. After the reaction effluents has exchanged heat with the
feed and has been cooled by the air condenser A-71101, it will enter the separator drum
D-71101, and the hydrogen rich gas from overhead line will return to the inlet of the
pretreatment recycle compressor K-71101A/B to be pressurized and circulated, and then
reused. The liquid at the drum bottom will be sent to the stripper C-71101, which will draw
the slight amount of lighter components out of the tower top and eliminate such impurities
in the oil as sulfur, ammonia, and water. After exchanging heat with the column feed in F-
71102, the oil at the bottom of the stripping tower C-71101 will become the refined
naphtha, reformer feed. After being condensed and cooled by the surface evaporation air
cooler A-71102, the product at the top of the stripping tower C-71101will enter the reflux
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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

drum D-71103 of the stripping tower. Some of the H2S and NH3 will be discharged along
with the gas from the top of the drum D-71103 and enter the fuel gas piping network of
the unit; water is discharged from the drum boot. Light Naphtha from reflux drum bottom
is pressurized by the reflux pump P-71103A/B, some of it will be charged back into the
top of the stripping tower as reflux, while another part of it will be sent into the catalytic
cracking unit as the sulfur-containing light naphtha. A reboiler F-71102 will input heat into
the stripping tower using the fuel gas.
The pretreatment process will use the recycle hydrogen flow. Because the reaction
process only consumes a very slight amount of hydrogen, therefore a slight make-up of
hydrogen rich gas from the reforming section will be added to the inlet of the pretreatment
recycle compressor. After the hydrotreating process, a slight amount of waste hydrogen
will be vented into the fuel gas piping network through the top of the separator drum D-
71101. The pretreatment reaction pressure is controlled at the top of the separator drum.
The process flowchart of the pretreatment section is shown in B9701-71-PR1/1..

3. Chemistry

3.1. General Considerations Concerning Chemical Reactions


Chemical compounds can be greatly affected by pressure, temperature or other
factors. These changes, which lead to destruction of atomic bonds and to the
creation of new ones, are called chemical reactions.

3.1.1. Equation of a chemical reaction


Lavoisier's studies (1743-1794) led him to conclude that a chemical reaction
involves mass conservation i.e. the mass of consumed reactants is equal to
the mass of products produced.
The mass balance is commonly expressed by the equation of a chemical
reaction.
The following example illustrates the hydrodesulfurization reaction, for a
sulfur compound called thiophene.

which leads to the following equation for the chemical reaction:


1 C4H4S + 4 H2 1 C4H10 + 1 H2S
This equation shows:
the reactant (thiophene C4H4S and hydrogen H2)

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

the products (butane C4H10 and H2S)


Furthermore the numerical values (in the boxes), called the stoichiometric
factors, are attributed according to the mass conservation principle known as
the atomic conservation principle.

The table below is a different way of illustrating mass conservation.

REACTANTS PRODUCTS

C4H4 S + 4 H2 C4H10 + H2S


4 moles of carbon C 4 moles of carbon C
Atomic
12 moles of hydrogen 10 moles of Conservation
balance
1 mole of sulfur S hydrogen H
1 mole of sulfur S

1 mole of thiophene 1 mole of C4H10


Mass i.e. 84 g i.e. 58 g Conservation
balance 4 moles of hydrogen 1 mole of H2S i.e.
i.e. 8 g 34 g
total mass: 92 g total mass: 92 g

Molecular 5 moles of reactants 2 moles of products Non


balance
conservation

Note that the molecular weight of these chemicals is 84g for thiophene, 2g for
hydrogen, 58g for butane and 34g for H2S, respectively.

3.1.2. Complete reaction - equilibrium reaction


When there is no time limit, two different types of final state may be
observed, depending on the temperature, the pressure and the quantities of
each chemical compound concerned:
 one of the reactants is entirely consumed during the reaction. The
reaction is called a complete reaction.
 the final state is made up of part of each reactant and part of the
products. In this case, the reaction is called an equilibrium reaction,
and a double arrow is used in the equation.
Hydrotreating reactions are either complete reactions, or equilibrium
reactions, depending on the operating conditions (temperature and pressure).

3.1.3. Thermal effect


Chemical reactions may have a thermal effect, which modifies temperature.
Reactions may be:
 Endothermic i.e. reactions which need heat

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

 Exothermic i.e. reactions which produce heat


 Athermic i.e. reactions without any thermal effect
The dehydrogenation reactions are exothermic, i.e. are producing heat.
A consequence is a natural trend of these reactions to increase the
temperature of the reaction medium.

3.1.4. Variation in the number of moles


The equation of a dehydrogenation reaction, for example:
1 C4H4S + 4 H2 1 C4H10 + 1 H2S
shows that:
there are 5 moles of reactants (1 mole of thiophene and 4 moles of hydrogen in
this example)
there is 2 moles of product (1 mole of C4H10 and 1 mole of H2S in this
example)
The dehydrogenation reactions occur with an decrease in the number of
molecules.
A consequence is a natural trend of these reactions to decrease the pressure
if the reaction medium is in gas phase.

3.1.5. Le Chatelier's principle


This principle states that:
In an equilibrium reaction, the conversion rate increases when operating
conditions are modified in a manner contrary to the natural trends of the
reaction.
Hydrodesulfurization reactions are exothermic, with decrease in the number
of molecules, and consumption of hydrogen.
What one might expect from Le Chatelier's principle, in the case of the
hydrodesulfurization reactions, is shown in the table below:

Action required to
Characteristics Trends
increase conversion
Exothermic reaction Temperature increase Temperature
decrease
Decreasing number of Pressure decrease Pressure increase
moles from 5 (reactants) to (if vapor phase)
2 (products)
Reaction consuming Decrease in Increase in hydrogen
hydrogen hydrogen concentration of the
concentration of the medium
medium
Reaction producing H2S Increase in H2S Decrease in the H2S
concentration of the concentration of the
medium medium

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

3.2. Kinetics

3.2.1. Reaction rate definition


Experimental data show that reactions evolve at varying speed towards their
final state. This evolution is studied through the reaction rate. It is defined as
the number of moles of reactant converted per unit of time and per unit of
volume or as the number of moles of products produced per unit of time and
per unit of volume. The reaction rate can also be defined as the variation of
concentration of one of the chemical compounds per unit of time.

3.2.2. Reaction rate as a function of the operating variables


Apart from the chemicals (either reactants or products), which could have an
effect upon the evolution of the medium, the factors, which may modify the rate
of reaction, are:
 Temperature
 Pressure and proportions of chemicals

3.2.3. Temperature effect


Experimental studies show that reactions are more or less sensitive to the
temperature effect.
Whatever the absolute value, the main conclusion from temperature studies is:
When temperature rises, the rate of all the chemical reactions increases.

3.2.4. Pressure and proportions of chemicals


There is no general conclusion on the effect of pressure and the proportions
of chemicals on the rate of chemical reactions.
An excess of one of the reactants could:
 have no effect upon the overall reaction rate
 increase the overall reaction rate
 decrease the overall reaction rate

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

3.3. Chemical Reactions


For a chemical reaction, thermodynamics dictates the equilibrium that would be
reached theoretically (i.e. if there is no time limit).
Kinetics dictates the rate of reaction, i.e. the possibilities to reach a state close to
equilibrium in a limited time. In order to enhance the hydrotreating reaction rates, a
specific catalyst has been used.

Several reactions occur in the hydrotreating (HDT) process, which aim is to prepare
the naphtha feed for the downstream aromizing unit (avoid the poisoning of the
aromizing catalyst). The main purpose of the process is the removal of sulfur
compounds (desulfurization). In parallel, many other reactions take place such as
denitrification (nitrogen compounds removal), deoxygenation (oxygen compounds
removal), olefins hydrogenation (or saturation), and at a lower extend
demetallation (organometallic compounds removal).

These chemical reactions can be separated into three types:


 Hydrorefining reactions: i.e. desulfurization, denitrification, and deoxygenation
reactions, which aim to the removal of impurities: sulfur, nitrogen and oxygen,
respectively.
 Hydrogenation reactions, which aim at the saturation of the olefins and
diolefins
 Demetallation reactions, which aim at the removal of metallic impurities, but in
a different way than that of hydrorefining reactions

3.3.1. Hydrorefining reactions


3.3.1.1. Desulfurization reactions
Sulfur (S), which is a poison of the aromizing catalyst, should be removed
by desulfurization, which yields into hydrogen sulfide H2S.
Sulfur is present in the naphtha combined to hydrocarbons. This
combination leads to one of the hereafter structures, which have different
characteristics.
Mercaptans
Mercaptans are composed of the functional combination –S–H, associated
with a hydrocarbon radical represented by the letter R. They have the
following general formula:

Note that mercaptans are acid components and have an obnoxious smell.
The chemical reactions related to the removal of mercaptans are
described below:

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

For example:

Sulfides
In these compounds the sulfur is linked to two hydrocarbon radicals. The
sulfur therefore forms an intermediary between the two radicals. Sulfides
have the following general formulas:

Unlike mercaptans, these compounds have the advantage of not being


acid which mean they are not corrosive. Moreover their low volatility
reduces their smell. The chemical reactions related to the removal of
sulfides are described below:

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

For example:

Thiophenic compounds
Thiophenic compounds are found typically in cracked naphtha (especially
heavy fractions). They derive from thiophene:

These compounds are not acid. However, the desulfurization of the ring is
more difficult, since this implies the opening of the ring, before the
hydrogenation of the radical and the release of the hydrogen sulfide.
An example of desulfurization of the methyl thiophene reaction is
presented hereafter:

All the desulfurization reactions presented above are exothermic. However,


they do not lead to a noticeable temperature increase, owing to the limited
amount of reactant involved.
The desulfurization of thiophenic compounds is more difficult than that of the
mercaptans and sulfides. Generally speaking, reactions involving a single
sulfur atom are very fast, and follow first order kinetics. However, when
present in combinations they exhibit apparent reaction orders of up to 1.6.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

3.3.1.2. Denitrification reactions


Nitrogen (N), which is also a poison of the aromizing catalyst, should be
removed by denitrification, which yields into ammonia NH3.
Organic nitrogen is present in the naphtha combined to hydrocarbons.
Nitrogen compounds typically found in the feed derive from pyrrol and
pyridine.

Examples of denitrification reactions are given for methyl pyrrol and


pyridine.

The heat released by the denitrification reactions is also negligible, owing the
small amounts of nitrogen compounds (even fewer than sulfur compounds).
Note that the C – N bond is much more difficult to break than the C – S bond.
Consequently, the denitrification occurs to a much lower extent than
desulfurization.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

3.3.1.3. Deoxygenation reactions


Oxygen (O), which is also a poison of the aromizing catalyst, should be
removed by deoxygenation, which yields into water H2O.
Organic oxygen is present in the naphtha combined to hydrocarbons.
These oxygenated contaminants are not a significant problems for a
straight-run naphtha, but more prevalent in cracked and synthetic cuts.
Hereafter, an example of deoxygenation reaction of phenol:

Similarly to denitrification, deoxygenation reactions are much more difficult


than desulfurization. Heat released by these reactions is also negligible.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

3.3.2. Hydrogenation Reactions


At the temperature of the aromizing process (about 500°C), olefins result in
coke deposit on the aromizing catalyst. Therefore, these components should be
hydrogenated prior to feeding the aromizer.
Olefin hydrogenation (or saturation) consists in the addition of hydrogen to the
unsaturated hydrocarbon (double or triple bonds), yielding into a saturated
hydrocarbon. Olefins are not present in the straight-run cuts. Cracked naphtha
can contain high concentrations of olefins, however.
An example of typical olefins hydrogenation reactions are presented hereafter.

Olefin hydrogenation reactions are extremely exothermic (heat of reaction are


about 100 kJ/mol).
They are besides relatively easy, and occur on the top portion of the catalyst
bed. Branched cyclic diolefins (such as methylcyclopentadiene) are more
difficult to hydrogenate, compared to normal mono-olefins.
Not that aromatic hydrogenation is not targeted by this process. Their
hydrogenation is extremely hard, except under the most severe operating
conditions (very high temperature for example), in which case this reaction
occurs to a very low extent.

3.3.3. Demetallation Reactions


Arsenic, lead, mercury and other metals, when present, are typically in
organometallic form. After hydrogenation in the hydrotreater reactor, the
hydrogenated form reacts with the hydrotreater catalyst forming a bimetallic
compound. As a result metals are physically adsorbed by the catalyst creating
a gradient on the catalyst bed.
During the operation cycle the equilibrium level of the contaminants will
progressively move down the bed. It is good operating practice to analyze and
replace this top portion of the catalyst bed as necessary to prevent contaminant
breakthrough into the aromizer feed.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

Contents: This document outlines the catalyst basic knowledge of naphtha


pretreatment section of CCR unit. The text includes:

1. Catalysis And Catalysts


2. Naphtha Hydrotreating Catalyst
3. Catalyst Loading
4. Catalyst Regeneration
5. Catalyst Unloading for Unregenerate Catalyst

1. Catalysis And Catalysts


1.1. Substances Altering The Velocity Of A Chemical Reaction
There are two types of chemicals (that are neither reactants nor products of the
studied chemical reaction) that can produce a change in the reaction rate:
 a retarder or inhibitor is a substance that slows down or even stops the reaction
 a catalyst is a substance that accelerates the reaction
A catalyst is a substance that increases the velocity of a chemical reaction without
any change in its own structure.
This kind of substance increases both forward and backward reactions in the same
way. Thus, it is possible to reach the final Equilibrium State more quickly but, in all
cases, introducing a catalyst does not change the final equilibrium conversion for
given operating conditions.

The result is that:


 for a batch process, the introduction of a catalyst shortens reaction duration for a
given conversion
 for a continuous reaction, the use of a catalyst enables:
o increase in flow rate for a given reactor design
o decrease in the reactor size in the case of a new project

1.2. Specificity Of The Catalytic Action


A set of chemical compounds is able to provide various products under specific
operating conditions. One (or sometimes more) of these is the desired product, the
others are the by-products. We therefore seek ways of activation which can
selectively achieve the desired reaction:
 the method consisting in raising temperature by an input of heat leads to the
increase of all reaction rates. As a consequence, temperature increasing is not a
selective method of activation.
 on the other hand, activation achieved by a catalyst is selective because the
catalyst has been designed to increase the velocity of the desired reaction in
relation to other reactions.
Thus, formation of the desired product is maximized in relation to that of undesirable
by-products.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

1.3. Catalyst Characteristics


The main characteristics of a catalyst in addition to its physical and mechanical
properties are:
the activity, which is the catalyst ability to increase the rate of the desirable
reactions. It is measured by the temperature at which the catalyst must be operated
to produce a product on-specification, for a given feed, all other operating conditions
being equal
the selectivity, which expresses the catalyst ability to favor desirable reactions
rather than others
the stability characterizes the change of the catalyst performance (i.e. activity and
selectivity) over time, when operating conditions and feed are stable. It is chiefly the
impurities in the feed which affect stability. For solid phase catalyst, traces of metal
in the feed also adversely affect stability

1.4. Principle Of Heterogeneous Catalysis


The heterogeneous catalysis is a catalysis where the catalyst and the reactants
(hydrocarbons and hydrogen) are not in the same phase: in the present case, the
catalyst is a solid located in fixed beds inside the reactor, whereas the reactants
are in vapor phase. The hydrogenation reactions progress downwards through the
catalytic bed, reducing the hydrogen content of the effluent.
The catalyst consists of metal atoms (i.e. active agents) dispersed on a (porous
solid) support (or carrier). It is called a supported catalyst. The catalytic reaction
takes place on the active species, which is why good accessibility to these species
by the reactants is of prime importance. To summarize, the key parameters of such
catalysts are:
 the specific surface area of the support
 the dispersion rate of the active agents on the support
 the pore distribution of the support
These parameters, if they are satisfactory, tend to limit diffusion phenomena by
facilitating the access of reactants and departure of products.
The following figure provides a schematic representation of the cross-section of a
grain of catalyst. It contains large channels, known as "macropores" and small
channels, or "micropores". The arrows show the direction taken by reactants R to
reach the internal surface of the catalyst.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

The surface area available for contact between catalysts and reactants may be as
high as several hundreds of square meters per gram. The supports commonly used
are alumina (Al2O3) or silica (SiO2).
The catalytic reaction can be broken down into three successive steps:
 adsorption of reactant molecules on certain available sites on the surface,
known as "active sites"
 chemical reaction in the surface-adsorbed phase. This step is usually very fast,
since the chemical species formed by association with properly selected sites are
far more reactive than non-adsorbed molecules
Furthermore, the catalyst brings together these reactive species locally in the
adsorbed phase, thereby considerably increasing their probability of meeting,
which also helps accelerate chemical change.
 desorption of products formed by the reaction, thereby releasing the active sites
for re-use
The products migrate through the pores to the outside of the grain towards the liquid
or the gas homogeneous phase.
These various elementary steps in catalysis are summarized in the following
diagram.

Use of the solid catalyst in such a mechanism involves the following requirements:
 its surface must be easily accessible to the reactants, and products must be
able to move away quickly to allow maximum use of active sites
 the chemical nature of these same active sites must be appropriate for the
reactions to be catalyzed, which explains the wide variety of chemical formula for
catalysts
The metal which constitutes the active phase of the catalyst must promote the
desired reaction as selectively as possible.
Since heterogeneous catalysis is a surface phenomenon, the active metals are
those which can chemisorb all the reactants
Nevertheless, this chemisorptive condition is not sufficient because the reactants
must be neither too weakly nor too strongly adsorbed.
If adsorption is excessively weak, very few molecules are activated on the catalyst
surface and the reaction rate is very slow. If the adsorption is too strong, the
hydrocarbon and the catalyst form a very stable complex, which produces a
poisoning effect.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

2. Naphtha Hydrotreating Catalyst


2.1. Catalyst Main Characteristics
The main characteristics of the RS-1 catalyst used in the naphtha hydrotreating
reactor are summarized hereafter:

Reference RS-1
Supplier RIPP
Composition Cobalt (CoO) ≥0.04 wt %
Tungsten (WO3) ≥19 wt %
Nickel (NiO) ≥2 wt %
Presentation Trifoliate - Diameter: 1.4 mm
Surface area ≥130 m2/g
Pore volume ≥0.22 cm3/g
Bulk density 0.75-0.80 t/m3
Bulk crushing strength ≥16 N/mm

3. Catalyst Loading
3.1. Preparation Before Catalyst Loading
3.1.1. Prior to catalyst loading, the startup work such as line flushing, run-in pumps
and motor, compressor commissioning, fire heater dry-out and leaking test
should be finished. The reactor should be cleared up and free from rust,
welding, water which can contaminate the catalyst. The blinds should be added
to prevent nitrogen and gas entering the reactor section. All instrument valves
should be in good condition.
3.1.2. Prepare the loading tools, such as one crane, one forklift, two transfer hoppers,
explosion-proof light, ceramic gasket to protect reactor manway, canvas as
protection against rain, loading socks of correct diameter and sufficient length,
wooden boards, a vacuum eductor, dust masks, measuring tape, chalk, ladder,
communication facilities, fresh air mask, etc.
3.1.3. Before reactor loading, personnel must enter the reactor to mark the wall for
each layer of the ceramic balls and catalyst according to design height.
3.1.4. The bolts of outlet basket at the bottom of reactor should be fixed and the blank
flange of unloading nozzle should be installed before reactor loading. The
explosion-proof light should be installed inside the reactor.
3.1.5. The loading area and reactor platform should be clean and free from
obstruction.
3.1.6. To avoid chaos and accident, personnel who will load catalyst should be
organized and undertake their own responsibility.
3.1.7. Insert a temporary hose into reactor and supply air to it. This can provide the
protection for the personnel who enter the reactor.

3.2. Notes
3.2.1. During catalyst transferring, care should be taken to put down and unload
catalyst gently.
3.2.2. Catalyst loading should be in fine day.

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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

3.2.3. Catalyst drums should not be opened until the catalyst will be loaded
immediately. The rate of loading should be as quick as possible within
allowance to reduce exposing time of catalyst in the air which can affect
catalyst with damp.
3.2.4. Catalyst scattered on the ground or contaminated should not be loaded into
reactor.
3.2.5. While loading the catalyst, the end of the socks shall be, at any time, kept
within one meter away from the catalyst level.
3.2.6. Personnel who will load catalyst must wear clean clothes and workers in
reactor should button cuff and clean pockets to avoid something dropping into
reactor.
3.2.7. During catalyst loading, the sock should be kept moving in figure “8” pattern to
prevent the catalyst forming hills or craters. When loading each layer of ceramic
balls, the previous layer of balls should be not disturbed. And after each one-
meter level loading, the catalyst bed should be smoothly raked to keep it as
level as possible so that the loaded catalyst density is uniform throughout the
catalyst bed.
3.2.8. To avoid static producing, catalyst crashing or becoming bridged in catalyst
bed, the loading rate should be controlled. Typically the rate is about 2- 4 tons
of catalyst per hour.
3.2.9. Personnel who enter the reactor should stand on wooden boards to avoid
treading down the catalyst.
3.2.10. Retain 10ml of catalyst sample from each drum loaded for future reference.

3.3. Catalyst Loading Procedure


3.3.1. Install reactor bottom internals.
3.3.2. Load catalyst supporting ceramic balls.
To support the catalyst bed and to prevent the migration of the catalyst bed,
three layers of ceramic balls shall be loaded in proper order in the bottom of
reactor. First, 13 mm diameter ceramic balls are loaded to a level that is
100mm higher than the outlet basket. Second, a 100 mm level layer of 6 mm
diameter ceramic balls is placed on the top of 13 mm balls. Then a 100 mm
level layer of 3 mm ceramic balls is placed on the top of 6 mm balls. Each layer
of these ceramic balls should be smoothly raked to keep the layer as level as
possible. While loading a new layer, care should be taken so that the previous
layer of balls is not disturbed.
3.3.3. Catalyst Loading
The sock loading method is used in loading of RS-1 catalyst. While loading the
catalyst, the end of the socks shall be, at any time, kept within one meter away
from the catalyst level. To prevent the catalyst from forming piles, the catalyst
must be loaded gently and the catalyst bed should be smoothly raked to keep
the catalyst bed level after each one-meter level loading.
3.3.4. Install distributor basket
Install the distributor baskets at design height, which refers to figure 1.
Then the baskets should be covered until the catalyst loading is complete.
3.3.5. The covering ceramics loading
The reactor will be topped off by placing a 100mm level layer of 6mm ceramic
balls and a 100mm level layer of 13 mm ceramic balls on the top of the catalyst
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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

bed (see figure 1). After this, the distributor basket temporary covers should be
removed.
3.3.6. Place the inlet distributor and bolt up the reactor inlet top cover.

Next to catalyst loading, catalyst will undergo the following operations which is
discussed in next document KRCIM 71100.04
 Inerting
 Air tightness test
 Catalyst Drying
 Presulfiding
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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

4. Catalyst Regeneration
4.1. Introduction
It is defined as nitrogen-air regeneration that coke accumulated on spent catalyst is
burnt off with recycle nitrogen and air. During catalyst regeneration, the nitrogen is
circulated in reactor section, and the air is gradually added to it. Catalyst is
regenerated by controlling air flow rate and reactor temperature increasing rate.
4.2. Neutralization of Acidic Gases
4.2.1. Regeneration Reaction
Because the spent catalyst is the sulfide type catalyst containing much coke, a
lot of CO, CO2, SO2, SO3 will be formed during catalyst regeneration.
The main reactions of catalyst regeneration are shown below:

These acid gases formed during burning of coke can react with water at low
temperature location of reactor section. These reactions are listed below:

.
The equipments of reactor section would be seriously corroded by sulfuric acid,
sulfurous acid, carbonic acid and nitric acid at low temperature, so caustic
neutralization should be adopted during catalyst regeneration.

4.2.2. Ammonia Injection


Strong corrosive compound H2SO4 is easy to be formed from SO3 at rather high
temperature. Hence, ammonia should be injected into the reactor outlet to
remove SO3. The neutralization reaction of ammonia
and SO3 is shown below:

At the same time, injected ammonia can also react with CO2 in regeneration
gases as following:

Ammonium sulfate and ammonium bicarbonate can form crystalloid at the


temperature 65˚C and 42˚C respectively, which can form build-up in lines and
equipments. In order to remove it, the air cooler outlet temperature should be
increased properly and caustic solution should be injected to upstream of air
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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

cooler, and the injection rate of ammonia should be controlled to avoid


formation of a lot of crystalloid of ammonium bicarbonate. It is better to keep
the ammonia concentration of the recycle gas less than 20 μg/g.

4.2.3. Caustic Injection


Caustic injection is used to neutralize the SO2, CO2 and NO2 in recycle gas.
These neutralization reactions are shown as below:

Typically the caustic solution is added to the upstream of air cooler. The NaOH
containing in fresh caustic solution should be at 4-5w% and the PH of
circulating caustic solution should be at 8-10. To hold the PH of circulating
caustic at 8-10, there will be a continuous injection of fresh caustic at proper
rate and a continuous withdraw of spent caustic.

4.2.4. Corrosion Inhibitor Injection


During catalyst regeneration, it is necessary to inject 20~50 μg/g of corrosion
inhibitor into fresh caustic solution, because it can form film on the surface of
metal to protect equipments from acid corrosion.

4.3. Preparations Before Catalyst Regeneration


4.3.1. Shutdown
4.3.1.1. Decrease the reactor temperature at rate of 30°C per hour and reduce the
feed flowrate slowly.
4.3.1.2. When the reactor temperature reaches at 200°C, stop charge to reactor.
4.3.1.3. Continue recycle gas circulation at 200°C for 4 hours, this purges any
remaining liquid hydrocarbons out of the reactor section.
4.3.1.4. After about 4 hours of gas sweeping at reactor temperature of 200°C,
increase reactor inlet temperature by 20°C per hour to 320~360°C ( the
operating temperature should be less than the design value) to strip the
catalyst with hot hydrogen for 12 hours. During the period, the H 2S
concentration of recycle gas should be not less than 500ppm(v).
4.3.1.5. Decrease the temperature of reactor at the rate of 30°C per hour to150°C
after the hot hydrogen stripping is finished, then decrease the pressure of
reactor section to 0.035MPa slowly.
4.3.1.6. Relieve the hydrogen of reactor section and drain oil and water at low
point. Isolate reactor section from hydrogen, feed surge drum and stripper
section by proper blinds.
4.3.1.7. Displace the reactor section with nitrogen until the total concentration of
hydrogen and hydrocarbon in reactor section is less than 0.3v%.

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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

4.3.1.8. Pressurize the reactor section to 1.0 MPa and commission the recycle gas
compressor after the displacement has been finished. When the
compressor run well, detect the concentration of hydrogen and
hydrocarbon in recycle gas. If it can not meet the above requirement, the
reactor section needs to be displaced again.

4.3.2. Preparation
4.3.2.1. The injection system of ammonia, caustic solution and soft water should
be clean and all equipments should be in good condition.
4.3.2.2. Prepare the caustic solution containing 30% NaOH, which is mixed with
soft water to produce solution of 4~5% NaOH, anhydrous liquid ammonia,
corrosion inhibitor, which is mixed with soft water and added into caustic
solution to produce solution containing 30 μg/g of corrosion inhibitor.
4.3.2.3. Establish the catalyst regeneration flow.
4.3.2.4. Install oxygen analyzers at inlet and outlet of reactor, which should be
calibrated and ready to work.
4.3.2.5. Notify the analysis department to prepare to analyze following items:

4.4. Procedure for Catalyst Regeneration


4.4.1. Temperature Increasing Phase
4.4.1.1. Pressurize the reactor section to 1.0 MPa at rate of 2-3MPa per hour, and
then establish maximum circulation with recycle gas compressor K-
71101A/B
4.4.1.2. When the compressor run stable, commission the caustic neutralization
system. Using the fresh caustic injection pump P-71105, begin injecting
the caustic solution containing 5%NaOH into the upstream of air cooler for
HP separator D-71101. When a working level has been established in the
separator, start circulation pump (full load).
4.4.1.3. Calibrating the on-line analyzers of oxygen of reactor inlet and outlet.
4.4.1.4. Increase the reactor inlet temperature to 320°C at the rate of 20°C /h, and
holding the temperature.
4.4.1.5. Analyze the total concentration of hydrogen and hydrocarbon in recycle
gas again, which should be less than 0.3v%.

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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

4.4.2. Original burning phase


4.4.2.1. Inject air to reactor section and commission ammonia pump to inject
ammonia into reactor outlet at the same time. In our experience, the
ammonia addition rate is about 1.6 kg per hour for 10,000 kg of catalyst
regeneration.
4.4.2.2. Slowly regulate the air addition rate to control oxygen level in reactor inlet
gas between 0.20~0.25v%.
4.4.2.3. Notify analysis department to analyze samples according to analysis
schedule.
4.4.2.4. Slowly increasing the flow rate of air injection to increase the oxygen
concentration to 0.3v% gradually.
4.4.2.5. Monitor the temperature of catalyst bed after air injection. Gradually
increase reactor inlet temperature to 335°C, if the temperature rise of
catalyst bed is not noticeable when the oxygen concentration of reactor
inlet reaches 0.3v%.
4.4.2.6. If ∆T of catalyst bed is still unnoticeable, increase the oxygen content to
0.4v% and carefully monitor the temperature change of catalyst bed. After
that, if ∆T of catalyst bed is still unnoticeable, slowly increase reactor inlet
temperature at the rate of less than 5°C per hour. Stop increasing
temperature of reactor inlet immediately, when the coke of catalyst begins
burning.
4.4.2.7. Begin checking the circulating caustic at regular intervals and record the
pH, periodically measure and record the total dissolved solids and
ammonium content. As the caustic becomes spent, the pH will drop from
an initial of 14 to 12, down to 7, if allowed. Do not let the pH drop below
about 8.0. Adjust the fresh caustic addition rate as necessary to hold the
pH of circulating caustic at 8.0-10.0 and continuously discard spent
caustic.

4.4.3. Main burning phase


4.4.3.1. Increase the reactor inlet temperature to 355°C slowly when the coke on
the catalyst begins burning and the ∆T of catalyst bed is stable.
4.4.3.2. When the reactor inlet temperature reaches 355°C and the temperature in
catalyst bed is stable, slowly adjust the air injection rate so that the oxygen
content in reactor inlet gas is 0.6v% or ∆T is 60°C, whichever comes first.
4.4.3.3. Holding reactor inlet temperature at 355°C until the burning wave is
passing through the catalyst beds.
4.4.3.4. When the burning wave is passing through the catalyst bed, oxygen can
be detected in the reactor effluent gas, which will lead to increase the
oxygen content in reactor inlet gas. To maintain the oxygen level in reactor
inlet gas at 0.3v%, the air injection rate should be reduced. The fresh
caustic addition rate will also have to be reduced or stopped completely at
this time, but the caustic circulation should be continued.
4.4.3.5. Continue to raise the reactor inlet temperature at a maximum rate of 20°C
per hour to 400°C. Maintain 400°C reactor inlet temperature and wait until
the reactor outlet temperature stabilizes. Once this temperature stabilizes,
record it named T1.
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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

4.4.3.6. Slowly adjust the air injection rate so that the oxygen content in the
recycle gas is 0.6 v% or the maximum temperature in catalyst bed is
440°C, whichever comes first.
4.4.3.7. While the second burning wave is passing through the catalyst bed,
continue to hold conditions constant, including the oxygen level in gas to
reactor, until the reactor outlet drops back to the temperature T1
measured in step(5). A reduction in air injection rate will be required.
4.4.3.8. Continue to raise the reactor inlet temperature at a maximum rate of
15°C/h to 440 °C, adjust the air injection rate so that the oxygen content of
the recycle gas is 1.0 v% or the maximum temperature in catalyst bed is
less than 450°C, whichever comes first.

4.4.4. Clean Burning Phase


4.4.4.1. When the last burning wave is completed, maintain the reactor inlet
temperature at 450°C and oxygen content of the gas to reactor at 1.0v%.
If no ∆T is expected, hold the conditions for 4 hours, however, if it occurs,
reduce the air injection rate as required keeping all catalyst bed
temperature below 455°C.
4.4.4.2. Maintain the reactor inlet temperature at 450°C and the oxygen content of
reactor inlet at 1.0v%. Burning of coke is finished when following three
conditions are satisfied:
 No oxygen consumed. The oxygen concentration of reactor inlet and
outlet keeps constant.
 No CO2 generated. The CO2 concentration of reactor inlet and outlet
keeps constant.
 No obvious ∆T in the catalyst bed.
4.4.4.3. Stop addition of caustic and ammonia and continue the caustic circulation.
If the pH of circulating caustic drops below 8 during temperature
decreasing, the fresh caustic should be injected to increase the pH of
circulating caustic to 10.

4.4.5. Reactor Temperature Decreasing


4.4.5.1. Decrease reactor inlet temperatures when coke burning is finished in the
following ways:
 Decrease reactor inlet temperature at 10°C /h when it is between
450°C~400°C.
 Decrease reactor inlet temperature at 20°C /h when it is between
400°C~300°C.
 Decrease reactor inlet temperature at 30°C /h when it is between
300°C~250°C.
4.4.5.2. Gradually increase the oxygen concentration of reactor inlet to 3.0v% and
carefully watch catalyst bed temperature when reactor inlet temperature
decreases to 250°C. No catalyst bed temperature rise means that coke
has been burned up. If there is catalyst bed temperature rise, please
decrease the oxygen concentration to 0.3v% by adjusting air injection rate
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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0

and holding temperature. When catalyst bed temperature becomes stable,


gradually increase the oxygen concentration of reactor to 3.0v% again.
4.4.5.3. Shut down the caustic circulation system and drain completely. Flush the
system as often as necessary with fresh water to remove all traces of
caustic.
4.4.5.4. Continuously decrease the reactor temperature. When the reactor inlet
temperature reaches 150°C please do not decrease it further until the
neutralization system is cleaned by fresh water and reactor system is
dried.
4.4.5.5. Stop injecting air. Purging reaction system with nitrogen gas until the
oxygen concentration of reaction system is less than 0.3v% and CO 2
concentration is less than 10 ppm(v),. Stop fire heater F-71101.
4.4.5.6. If the catalyst is to be removed and screened, cool down the catalyst bed
to 50℃ or less. After the first regeneration, it is advisable to dump and
screen the catalyst. This will give an indication of the completeness of
regeneration plus an indication of the amount of fines and scale that can
expect on future regeneration.
4.4.5.7. Decreasing the pressure of reactor section to 0.035MPa at the rate of
2~3MPa/h.
4.4.5.8. Purge the reactor section with nitrogen gas continuously, then pressurize
it to 0.35MPa and hold it.

4.5. Notes
4.5.1. Do not increase reactor inlet temperature and oxygen content of recycle gas
simultaneously, otherwise, the temperature in catalyst bed is easy to exceed
the limited value.
4.5.2. During catalyst regeneration, especially when reactor temperature is being
increased, an oxidizing atmosphere should be maintained at all times. If the
oxygen concentration in the gas to reactor drops to zero, it is possible that
some catalyst reduction can occur due to the presence of CO2.
4.5.3. In order to prevent caustic cracking, the temperature of caustic injection point
should be less than 200°C and between for 140~150°C.
4.5.4. During catalyst regeneration, the maximum temperature of catalyst bed should
be less than 480 °C.

4.6. Emergency Procedures During N2-Air Regeneration


4.6.1. If, at any time, the catalyst temperatures become excessive, block in the air
injection control valve immediately.
4.6.2. If the recycle compressor fails or must be shut down, and if it is known that it
cannot be immediately restarted, then do the following:
 Block air injection immediately;
 Cut out heater fires;
 Shut down the ammonia pump, caustic addition pump and caustic
circulating pump immediately.

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PRODUCTION & OPERATION CATALYST
CCR UNIT KRCIM 71100.03 REV.0
4.6.3. In the event of caustic circulation failure, block in the air injection immediately。

5. Catalyst Unloading for Unregenerate Catalyst


The following precautions are recommended for use during unloading of unregenerate
catalyst. The main concern is that no oxygen be allowed to contact the catalyst inside
reactor, since this can result in spontaneous combustion of the iron pyrites. The
temperature generated by this combustion can be quite high, and can result in severe
damage to the catalyst and reactor internals. Of secondary, but more importance, is
protection of personnel during unloading. All personnel involved with the unloading must
be properly informed of the dangers involved and the proper safety measures.

5.1. Cool the reactor beds to less than 65°C. At the temperatures above this level,
combustion of iron pyrites is greatly accelerated and difficult to control. If the catalyst
is to be screened during unloading, the catalyst should be cooled to less than 50°C.
5.2. After cooling the catalyst beds to 65°C, the unit should be purged with N2 at least
twice. The unit should then be properly isolated and a small N 2 purge established at
the compressor discharge or preferably at the inlet to reactor. Do not open the
reactors at the top until all catalyst has been unloaded.
5.3. Be sure that several CO2 extinguishers are available.
5.4. Use only metal drums for unloading, and dump directly into drums if possible. Each
drum should be either purged with N2 during unloading or a piece of dry ice placed at
the bottom of each drum. Do not seal the drum air tight since this could result in
sudden rupture of the drum when combustion occurs. Burning of catalyst in the drum
is not serious and can be quickly extinguished with nitrogen or CO2.
5.5. When the catalyst should be screened at the same time as it is being dumped from
the reactors, nitrogen need to be purged through the dumping nozzle to the top of the
first screen to provide additional protection from pyrite ignition.
5.6. It is expected that some "sparking" of the pyrites will take place in any event.
Therefore, all workmen in the area must be supplied with face and eye protection. In
addition, they should wear long sleeve shirts with collars and cuffs tightly buttoned.
5.7. Maintain a positive flow of N2 out of the unloading nozzle throughout the unloading, if
the catalyst becomes bridged in the unloading nozzle or is not free flowing, break the
plug with a blast of N2. Do not allow air to be drawn into the reactor.
5.8. If ignition of pyrite takes place inside a reactor, stop unloading in that reactor and
increase the N2 purge to maximum until burning is stopped.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

Contents: This instruction outlines the procedure for the start-up and shutdown of the
CCR regeneration Unit. The text includes:

1. Start-Up Requirement
2. Unit Purging
3. Initial Leak Test
4. Unit Drying
5. Catalyst Loading
6. Air Freeing and Leak Testing
7. Catalyst Drying
8. Catalyst Presulfiding
9. Establish Normal Operation
10. Normal Shutdown Procedure

1. Start-Up Requirement
1.1. All overhaul activities and technical modifications influencing Start-up are completed.
All units, removal of equipment and pipeline blinds conform to process requirements.
1.2. Pressure gauges and safety valves are checked. Replacement work and installation
is completed.
1.3. All chemical raw materials are ready and sufficient.
1.4. All process lines and equipment has been purged, qualified in pressure test and
undergone final inspection according to the following procedures.
1.5. Disassembled or replaced equipment flanges are padded and screwed uniformly.
1.6. Safety valves in good condition and its set pressure meet the requirement.
1.7. Close all atmospheric relief valves and drain.
1.8. Verify all instruments are in good condition.
1.9. Utilities services are working normal.
1.10.Ensure complete fire appliances, place inflammables and explosives in fixed area,
clean sundries on site.
1.11.Contact dispatch, maintenance department, fitters, electrical maintenance and lab.
Complete corresponding support work.
1.12.Complete and examine all Start-up schemes, planning diagrams, all related
procedures sheet and work permits.
1.13.All maintained and revamped equipment has acceptance qualification sheet.
1.14.Inspection of the unit is done according to “Plant Inspection” procedure in (KRCIM
71300.04)

2. Unit Purging
2.1. Purging objective
2.1.1. Eliminate welds rods and slags, abrasive dusts, oxides and in general other
substances which might impede the normal unit operation or damage the
equipment (valves, pumps, compressors, turbines, etc.)
2.1.2. Timely find existing problems through process line. Ensure system operability.
2.1.3. Make operators further understand field flow path.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

2.2. Preparation work before purging


2.2.1. All equipment and pipelines belonging to this unit should be inspected carefully
according to purging route before purging; any reassembled or newly installed
equipment should be repositioned completely; any problem found should be
handled in time.
2.2.2. Contact with dispatch to prepare steam and water supply.

2.3. Notices For Purging


2.3.1. Proceed with purging and flushing of the unit according to instructions in
“Cleaning of Equipment and Pipeline” in (KRCIM 71200.04).
2.3.2. Media used for flushing and purging
 Pipeline for handling liquid should be flushed with water; except that
condensed water system uses condensed water for flushing, others use
fire water for flushing.
 Pipeline for handling gas should be flushed with air or nitrogen;
instrument’s pneumatic line should use purified air for purging.
 Steam pipeline should use steam of corresponding pressure level for
purging according to different pressure levels.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

2.4. Purging Scheme


2.4.1. C-71101 system purge
The reforming unit uses 1.0MPa steam as purging media. Firstly, remove the blind plate on 50-LS-711001 line, drain and
vent it until it is clean. Then, introduce steam into tower system and purge according to the following scheme:
→Top tower vent
→PG-1019
→Vent steam from drain point at corrosion inhibitor line upstream the check valve
→Flange upstream PSV-71102A/B and flange downstream bypass valve
→Tower overhead line →200-P-711025→A-71102→D-71103 →drum top vent
→Drum boot discharges to underground drain
→PG-1021 discharges steam
→50-P-711027→40-GN-711003 line 8-shaped blind plate discharges steam
→PV-1004 bypass →50-P-711028 line 8-shaped blind plate
discharges steam
→50-NF-711021 line 8-shaped blind plate discharges steam
→SN-71107 sampler discharges steam
→150-P-711029→P-71103A/B inlet drain and filters upstream flanges discharges
steam
→40-SLO-7110158-shaped blind plate discharges steam
→40-P-711056→50-P-711055 shaped blind plate discharges steam and then to
GDHT
→LV-1003 discharges steam
→50-P-711055/1→D-71106→drum bottom discharges steam to
underground drain
→Drum level glass ends
→50-SW-711002→P-71105 inlet
drain and filter upstream flange
discharges steam →40-SW-711003
line 8-shaped blind plate discharges
steam
→50-SW-711004 overflow line
discharges steam to drain
→25-KL-711001 →40-KL-714001 boundary line
8-shaped blind plate discharges steam

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

→100-P-711033→FV-1013 bypass →Flanges upstream non-return valves on P-71103A/B outlet and drain points discharge steam
→SN-71102 purges and discharges steam to the flare drum
→FT-1021 bypass →80-P-711080→FV-1014 bypass →light naphtha boundary limit line 8-shaped
blind plate discharges steam
→150-P-711024→drain downstream E-71103A tube side and slops line 8-shaped blind plate discharge steam
→drain downstream E-71103B/C tube side and slops line 8-shaped blind plate discharge steam
→150-P-711020→FV-1029 and its bypass →150-P-711019 line 8-shaped blind plate discharges steam
→25-P-711073→D-71102 bottom 8-shaped blind plate discharges steam
→FV-1007 bypass →100-P-711087→P-71101A/B outlets drain and flanges upstream non-return
valves discharges steam
→150-P-711005 →SN-71101 discharges steam
→HV-1001 discharges steam
→FV-1003 discharges steam
→100-P-711060→discharges steam upstream FV-1003
→150-P-711020/1 →150-P-711002→100-SLO-711024→8-shaped blind plate discharges steam
→100-P-712096/3→8-shaped blind plate discharges steam
→100-P-711052→100-P-711051→drain upstream E-71109 and slops line 8-shaped
blind plate discharges steam
→150-P-711002→LV-1001 bypass →FT-1001 crossover line→naphtha comes from
hydrogenation line, 8-
shaped blind plate
discharges steam
→150-P-711001/1→
naphtha from tank field,
8-shaped blind plate
discharges steam
→100-P-711001/2→
naphtha from SCR, 8-
shaped blind plate
discharges steam
→150-P-711002→D-71100→tank bottom discharges to underground drain
→top vent discharges steam
→PG-1001 discharges steam

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0
→100-NF-711002→flange upstream PSV-71100A/B and
flange downstream bypass discharge steam
→40-P-711089→PV-1001A discharges steam
→PV-1001B bypass →8-shaped blind
plate to fuel gas
pipe network
discharges steam
→8-shaped blind
plate to flare
header
discharges steam
→All liquid level gauges discharge steam
→200-P-711003 →P-71101A/B inlet drain and filter
flange discharge steam
→100-P-711004→100-P-711074→8-shaped blind plates
at hydrotreated naphtha battery limit line discharge steam
→400-P-711034→E-71103A shell side →E-71103B/C shell side →150-P-711044→FV-2006 bypass →150-P-712001 line’s 8-shaped
blind plate discharges steam
→water injection line’s 8-shaped blind plate
discharges steam
→sulfur injection line’s 8-shaped blind plate
discharges steam
→chlorine injection line’s 8-shaped blind plate
discharges steam
→100-P-711050→E-71109A/B shell side drain and
slop line 8-shaped blind plate discharges steam
→100-P-711051 globe valve discharges steam
→Underground drain and slop line 8-shaped blind plate discharge steam
→P-71102A/B inlet drain and filter flange discharge steam
→SN-71103 sampler discharges steam
→300-P-711036→P-71102A/B outlets drain and non-return valve flange discharge steam
→F-71102→FV1008, FV1009, FV1010, FV1011 discharge steam
→tower bottom liquid level gauge discharges steam
→400-P-711040→→F-71102→FV1008, FV1009, FV1010, FV1011 discharge steam

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

2.4.2. C-71101 steam purging blind plate table

No. Specifications Location Tube No. Qty. Status Remarks


1. Dg50 C-71101 bottom steam line LS-711001 1 Open 8-shaped blind plate
2. Dg40 D-71103 top nitrogen line GN-711003 1 Blind 8-shaped blind plate
3. Dg50 D-71103 overhead line to flare NF-711021 1 Blind 8-shaped blind plate
4. Dg50 D-71103 overhead line to F.G P-711028 1 Blind 8-shaped blind plate
5. Dg80 Light naphtha battery limit line P-711080 1 Blind 8-shaped blind plate
6. Dg100 Hydrotreated naphtha battery limit P-711051 1 Blind 8-shaped blind plate
line
7. Dg150 Upstream FV-2006 P-712001 1 Blind 8-shaped blind plate
8. Dg20 Chlorine injection line CL-712003 1 Blind 8-shaped blind plate
9. Dg20 Sulfur injection line CL-712007 1 Blind 8-shaped blind plate
10. Dg20 Water injection line SW-712005 1 Blind 8-shaped blind plate

2.4.3. Blowing-up purging scheme


Use nitrogen to blow-up and purge prehydrotreatment system. Pipelines above DN150 should undergo blowing-up purging.
Blowing-up plate pressure is 0.3MPa.
1. Close all instruments’ primary valves; instruments easily damaged with vibration must be disconnected from purged
pipeline.
2. Remove all orifice plates on pipelines
3. Announce the blowing-up area as a hazardous area and isolate it with a guard tape.
4. Use 0.8MPa nitrogen as a blowing-up purging media.

2.4.4. Prehydrotreatment system blowing-up scheme


Introduces 0.8MPa nitrogen from outlet and inlet pipelines of K-71101A/B (close K-71101 outlet valve, install blind plate at K-
71101 inlet filter upstream flange, blowing-up purging media should not contact compressor body)
 At D-71102 top pipe, turn the inlet elbow to atmosphere; the blowing-up flow is: 0.8MPa nitrogen from 40-GN-711001
enters K-71101A/B inlets respectively→150-P-711021 and 150-P-711021/1→D-71102 top inlet. Close other connected
pipelines valves for isolation;

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

 After D-71102 top inlet is purged to clean, connect it and enter the next blowing-up port. At D-71101 top hydrogen line,
remove flange and install temporary nozzle; the blowing-up flow is: 0.8MPa nitrogen from 40-GN-711001 enters K-
71101A/B inlets respectively→150-P-711021 and 150-P-711021/1→D-71102 top outlet →D-71102→150-P-
711018→150-P-711015→D-71102 top inlet. Close other connected pipelines valves for isolation;

A secondary procedure is: Fill D-71101 with steam before installation of instrument devices and purge according to the
following flow: 150-P-711015→150-P-711018→D-71102→150-P-711021 and 150-P-711021/1 and discharge steam before K-
71101A/B inlets. Close other connected pipelines valves for isolation
 At R-71101 reactor top, turn the inlet elbow to atmosphere; the blowing-up flow is: 0.8MPa nitrogen to 40-GN-
711001→40-GN-711002→100-P-711022→200-P-711008→E-71101B/A shell side 250-P-711010→F-71101→250-P-
711013→R-71101 reactor top. Close other connected pipelines valves for isolation;

2.4.5. Blind plate table for blowing-up purging of prehydrotreatment unit


No. Specifications Location Qty. Tube No. Status Remarks
1. Dg40 K-71101A/B 1 GN-711001 Open 8-shaped blind
plate
2. Dg150 K-71101A/B inlets 2 P-711021 Blind Temporary blind
plate
3. Dg80 HV1001 1 P-711005/1 Blind 8-shaped blind
plate
4. Dg150 Downstream FV1003 1 P-711007 Blind 8-shaped blind
plate

2.4.6. Flushing of corrosion inhibitor pipeline


Inject water into D-71105 tank to a certain height, then open drain at P-71107 line. After flushing to clean, start up P-71107
pump to flush the line to C-71101 top. Open the drain before hand valve on line 20-Cl-711003 for discharge.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

3. Initial Leak (Air Tightness) Tests

3.1. Air Tightness Objective


Air tightness objective is to further inspect the quality of valve, flange, pipeline,
equipment, and welding seam using gas media (This unit uses nitrogen) to inspect
the leak sources in the system with field observation soap test method under the
regulated pressure.

3.2. Air-Tight Preparation


3.2.1. Air tightness test must be done after unit finishes purging, the pipe fittings such
as reassembled flanges, blind plates, and orifice plates etc. repositioned, the
existing problems have been rectified and improved and all flows reset.
3.2.2. Inspect the unit’s equipment, process pipelines, flanges, washer blind plates,
valves, safety valves, instruments, motors and pumps, etc. any problem should
be solved before air tightness test begin.
3.2.3. Contact with dispatcher to put the nitrogen source for air tightness into effect so
as to guarantee there is enough nitrogen supply.
3.2.4. Contact with dispatch to make preparation for transportation assurance of air
tightness gases
3.2.5. Contact with instrument to make air tightness to instruments related equipment
simultaneously with process system.
3.2.6. Prepare air tightness tools such as precision pressure gauge, spanner, soapy
water, brush, ear syringe, big and small barrels, etc. and organize personnel to
inspect and record by areas; workshop appoints special persons responsible
for handling of leakage points.
3.2.7. Inspect whether the air tightness points leak; use brush to brush soapy water or
use ear syringe to spray soapy water on air tightness points to observe whether
there is bubbles; if any, it means that the point is leakage point; then, mark it
with chalk or slate pencil and contact personnel to handle it in time.
3.2.8. For small space air tightness points, adhesive paper can be used to block the
flange, then, open a small hole on the adhesive paper, and then, inspect
whether the small hole leaks gas.
3.2.9. For the air tightness for drain points, their joints can be inserted into soapy
water for inspection.

3.3. Locations For Air Tightness Inspection


Air tightness inspection should be made to the system’s pipelines, equipment,
valves, flanges, pipe plugs, pressure gauges, instrument connecting positions,
pipeline welding seams, etc. They can be divided into reactor upper cap, lower outlet
flange, furnace inlet and outlet tubes, flanges in combined heat exchanger, high-
pressure separating tank liquid level gauge, pressure instrument flanges, etc.
according to locations.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

3.4. Safety Considerations

3.4.1. Pressure boosting speed should be slow and air tightness test pressure should
comply with the regulations strictly without overpressure.
3.4.2. Any leak source found should be marked in time and the maintenance
personnel should be contacted for handling.
3.4.3. Pay attention to inspect whether there is interflow between systems and avoid
equipment overpressure strictly. Watch out for gas expansion in the system
and consequent equipment overpressure because of ambient air temperature
change.
3.4.4. During air tightness test, commands should be given uniformly and personnel
in all areas should contact with each other.
3.4.5. During air tightness test of each system, at least two pressure gauges should
be used to observe pressure with required pressure gauge precision of
magnitude 0.4, 1.5-2 times of the highest air tightness pressure.
3.4.6. Handling of leak sources under pressure is not allowed.

3.5. General Instructions

3.5.1. Initial leak tests will be performed under KRC or Engineering company
responsibility and the general instructions hereunder shall only be used as a
reminder.
3.5.2. The initial leak tests can be performed using air or nitrogen depending upon
local facilities. The test pressure will be the air or nitrogen system pressure or
the unit (or section of unit) design pressure, whichever is the lower.
3.5.3. The unit is isolated with blinds from adjacent sections containing hydrocarbons
(liquid or gaseous), and from utilities systems where pressure is lower than air
(or nitrogen) pressure.
3.5.4. The pressure rise must be checked on several manometers and possibly
checked on a pressure recorder. Leaks must be carefully located and
tightened. Their location must be recorded.
3.5.5. The leak test is satisfactory when the pressure decrease is lower than
0.005 MPa/hour over a period of 4 consecutive hours.
3.5.6. The air (nitrogen) used for leak tests should be purged out of the unit using low
points drains to remove free water, if any.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

3.6. Airtightness Flow

K-71101A/B outlets E-71101B/A (shell) F-71101 R-71101


E-71101 A/B (tube) A-71101A/B D-71101 D-71102
K-71101A/B inlets

 Airtightness phase and standard pressure tapping point: D-71101


Airtightness Airtightness Pressure drop Hydrogen Airtightness
media pressure/MPa (MPa/h) compressor Status time/h
1.0 0.02 running 2
Nitrogen
2.45 0.005 stop 4

 When introducing vaccuum, close all pressure gauges and pressure lead wires.
Install vacuum gauge at D-71101 to start up ejector. When introducing vaccuum in
prehydrotreatment system, it is up-to-standard when D-71101 pressure reaches
0.003KPa (gauge pressure); then, introduce nitrogen slowly to break the vacuum.
 After vacuum test, blind the vacuum line blind plate; then, prepare positive pressure
airtightness.

4. Unit Drying
4.1. Drying Objective
4.1.1. To avoid damaging the catalyst with water
4.1.2. To shorten the duration of the low severity operation after first oil in.
4.1.3. Unit dry out is conducted simultaneously with the heater refractory drying,
which can save commissioning time.
4.1.4. The objective of furnace drying is to remove the natural water, crystallines.
Drying will calcinate materials contained in the furnace refractory. Accordingly,
intensity and service life of refractory materials will increase.
4.1.5. Furnace drying and system drying should be done simultaneously, namely,
using nitrogen circulation method. On one hand, nitrogen flow through the
furnace tubes will ensure no tubes overheating will occur; on the other hand,
circulating this hot nitrogen through the unit will remove excess moisture which
might have remained from the construction and flushing.
4.1.6. During furnace drying and system drying, potential internal and external
expansion problems will be discovered. Moreover, the plant operability will be
confirmed.
.

4.2. F-71101 Furnace Drying And Prehydrotreatment System Drying


4.2.1. Strictly read and follow KRCIM 71200.07
4.2.2. Close recycle compressor K-71101A/B outlet and inlet valves.
4.2.3. Line-up nitrogen circulation flow according to the following flow and
simultaneously, make isolation work to avoid pressure interflow.
K-71101A/B→E-71101→F-71101→R-71101→E-71101→A-71101A/B→D-
71101→D-71102→K-71101A/B
4.2.4. Introduce N2 into K-71101 inlet and via compressor bypass to the system.
Perform N2 inerting to reaction system until O2 content is < 0.5% (V).
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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

4.2.5. N2 increases the reaction system pressure to 0.35MPa.


4.2.6. Start up K-71101 according to regulations to establish system nitrogen
circulation and keep full load operation and use air cooler to cool down and
condensdate gas before separator.
4.2.7. Use steam to purge furnace hearth for 15min before ignition (steam
introduction should remove water completely with slow speed to avoid
damaging the refractory materials) and perform explosive gas analysis. After
analysis is up-to-standard, start the furnace according to furnace operation
method.
4.2.8. Adjust flame distribution and damper air quantity; reduce air damper and flue
damper as possible under the condition that enough air demanded by
combustion is available to keep furnace hearth negative pressure within -2-
4mmH20 and guarantee uniform distribution of heat quantity inside furnace, and
the temperature difference measured by two thermocouples is not more than
10°C.
4.2.9. During furnace drying and heating up, pay close attention to furnace outlet
temperature and furnace tube pipe wall temperature; the furnace outlet
temperature uses the temperature measured by TI1004A thermocouple as
reference. It is required to be no more than 450°C. The two groups of
temperature difference should be not more than 5℃.
4.2.10. When convection bank inlet flue gas temperature reaches 150°C, begin to
use air preheater system.
4.2.11. When furnace hearth temperature reaches 200°C, contact with related
departments to fasten the high temperature positions.
4.2.12. At each heating up phase during furnace drying, operation personnel should
make emptying and discharging at all low-point drain and high points,
especially make water discharge at the low-temperature positions such as the
downstream of feedstock heat exchanger E-71101 (shell) inlet and
prehydrotreatment product separating tank D-71101, compressor inlet knock-
out drum, etc. If the total water discharge is smaller than 100ml/h, it can be
considered that the system has been dried completely; otherwise, low-point
drain should be done continuously.
4.2.13. When furnace drying and drying finish, extinguish the furnace according to
operation procedure, and stop air preheater blower.
4.2.14. The reaction system continues cooling circulation; when reactor R-71101 inlet
temperature reduces to 55°C, stop K-71101 and close N2 supplying valve
according to regulations and prepare loading work of prehydrotreatment
catalyst.

4.3. F-71102 Furnace Drying (Note: Same procedure is be used for F-71205 drying)
4.3.1. Preparation work
 Flushing and purging of heat carrying system finishes.
 Electricity, instrument air, steam, nitrogen, and gas are smooth and enough
supply is guaranteed.
 Strictly read and follow KRCIM 71200.07

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

4.3.2. Furnace drying steps:


4.3.2.1. Inject furnace drying media
 Close valves on steam branched lines irrelated to furnace drying to
avoid steam flowing to other system.
 Use 1.0MPa steam as a cooling fluid. The flow of cooling fluid,
especially through the convection section, should not be too large or
flue gas will be wet and so the furnace refractory. As steam is used as
the cooling fluid in the tubes, a small fire should be established in the
furnace to warm the tubes and setting before introducing steam into
cold tubes. Light several burners until the flue gas thermocouple
registers 150 ̊C. By this time sufficient heat is contained in the tubes to
prevent steam condensation. This would prevent water hammer.
Provision to vent steam should be available.
 Discharge condensate and introduce steam into furnace tubes; steam
valve should be opened slowly.
4.3.2.2. Ignition and heating up
4.3.2.2.1. Inspect gas pipeline carefully
4.3.2.2.2. Use steam to replace the gas pipeline; O2 content < 0.5% by
sampling analysis means that the replacement is up-to-standard.
Discharge all condensed water inside the pipe;
4.3.2.2.3. Introduce gas in upstream of the burner valve.
4.3.2.2.4. Use steam to purge furnace hearth for 15min before ignition (steam
introduction should remove water completely with slow speed to
avoid damaging the refractory materials) and perform explosive gas
analysis. After analysis is up-to-standard, ignite the furnace
according to operation method.
4.3.2.2.5. Follow up drying curve using the temperature at TI1020A as
reference. Drain water from all low points
4.3.2.3. Cool and extinguish furnace :
1) After keeping temperature at 450°C finishes, cool down at rate of
25°C /h; when furnace hearth temperature reduces to 250°C,
extinguish the burner and pilot burner according to procedure
Close all fire doors, air and flue dampers
2) Use steam to purge gas pipeline and add blind plate on gas
pipeline.
3) When furnace hearth temperature reduces to 100°C, open air
and flue damper for natural ventilation.

After furnace hearth temperature reduces to normal temperature below 40°C


naturally, open the manhole, inject air; after O2 content in the furnace hearth is
analyzed to be up-to-standard, overall inspection can be done.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

5. Catalyst Loading
Please refer to chapter 3 of KRCIM 71100.03

6. Air Freeing and Leak Testing


6.1. Preparations
6.1.1. Notify the supervisors of utility systems to assure that water, electric, gas and
air are available. Contact analysis, instrument and electricity department etc. to
arrange startup cooperation.
6.1.2. All the equipments should be in good condition.
6.1.3. All instruments should be inspected and ready for use.
6.1.4. The source of nitrogen should meet requirements as following:
nitrogen content is required to exceed 99.5v%, in which the oxygen
concentration should be less than 0.3v% and the hydrogen and hydrocarbons
concentration should be less than 0.3v%.
6.1.5. The process flow is proved correct by three-grade inspection. Blinds should be
added in proper location for leak testing.
6.1.6. Get tools ready for leak testing, such as soap solution, brush and tools for
repairing.

6.2. Air Freeing


6.2.1. Pressurize the reactor section with nitrogen to 0.35MPa at outlet of recycle gas
compressor, and then depressurize it to 0.035MPa.
6.2.2. Perform the above step (1) two more times until the oxygen concentration is
below 0.5v%.

6.3. Leak Testing


6.3.1. The purpose of leak testing is to provide assurance of a startup without serious
leaks. However leaks often develop after equipment starts to warm up to
operating temperature, when piping and vessels expand. Operators should be
alert during startup and initial operation for the development of leaks.
6.3.2. Confirm the flow of leaking test and provide suitable blinds to isolate the
various sections as required by different pressure ratings.
6.3.3. Requirements: leak testing should proceed under guidance of unit operating
manual.
6.3.4. Raise the system pressure to the required pressure at the set rate, and check
the unit thoroughly. When there is no leakage and static pressure drop meets
requirements, depressurize the system to 1.5MPa.

7. Catalyst Drying
7.1. Preparations
7.1.1. Prehydrotreatment hydrogen-system inerting is fulfilled. Oxygen content <0.5%,
D-71101 pressure reduced to 0.8MPa.
7.1.2. Prepare one 1000ml measuring flask and one 5 liter water flask.
7.1.3. Make sure that sufficient nitrogen supply is available and analyze nitrogen
purity in advance. It is required that the content of water in the nitrogen rich gas

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

should be less than 300µg/g, total hydrogen and hydrocarbons content less
than 0.3v% and oxygen content less than 0.3v%
7.1.4. H2, gas and all kinds of hydrocarbons should be isolated from the reactor
during catalyst drying. Accordingly, make sure blinds are located at:
 H2 inlet into the unit (50-P-712050/3)
 Fuel gas line at top of D-71101 (50-P-711061)
 All feedstock inlets to unit
7.1.5. F-71101 ignition according to regulations, control temperature in every stage
according to following requirements. Meanwhile, under the conditions of N 2
environment, pressure as 0.8MPa, full circulation of compressor K–71101.
Drain water every hour at D-71101& D-71102 and complete measurement.

7.2. Operation Conditions For Catalyst Drying


 Pressure of HP separator: 1.5MPa
 Medium: nitrogen
 Nitrogen circulation: in maximum compressor load

7.3. Procedure
The drying procedure includes three phases:

7.3.1. Phase of temperature rising:


7.3.1.1. Fire charge heater F-71101 according to instructions in KRCIM 71200.07
and raise the reactor inlet temperature at a maximum rate of 15 °C per
hour until the temperature in catalyst bed reaches 120°C. Hold the
temperature for 4 hours.
7.3.1.2. Raise the reactor R-71101 inlet temperature at a maximum rate of 15℃per
hour until the highest temperature in the catalyst bed reaches 250°C. If
the temperature in any point of catalyst bed is below 230°C, raise the
reactor inlet temperature to ensure the temperature of the whole catalyst
bed exceeds 230°C.

7.3.2. Phase of temperature holding at 250°C:


7.3.2.1. Hold the temperature in the catalyst bed at 250°C for at least 6 hours.
7.3.2.2. During this period, flanges may be tightened under the temperature and
drain out the water at intervals of 2 hours, measure it and record the
weight. Decrease the temperature if there is no water drained out from
separator in successive operations (at least twice).

7.3.3. Phase of temperature decreasing


7.3.3.1. Decrease the catalyst bed temperature with nitrogen circulation until the
highest temperature in the catalyst bed drop to below 150°C, No water
drained from separator indicates accomplishment of the catalyst drying.
7.3.3.2. Note: Do not introduce hydrogen into unit until two conditions reach the
requirement: the highest temperature in the catalyst bed must be lower
than 150°C, and the oxygen content in the gas sample from the system
must be less than 0.5v%.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

8. Catalyst Presulfiding

8.1. Sulfiding Agent And Carrier Oil


It is preferable to use straight run naphtha with a maximum end point of 180°C and
bromine number less than 2gBr/100g as carrier oil. DMDS (Dimethyl sulfide) or CS 2
(Carbon disulfide) can be used as the sulfiding agent. The carrier oil and sulfiding
agent should be analyzed in advance.

8.2. Operating Conditions


 Pressure: Operating pressure
 LHSV: 3.0 h-1
 H2/oil 100-200v/v

8.3. Procedures For Presulfiding


8.3.1. Depressurize the reactor section to 0.035 MPa and then pressurize it to 0.35
MPa with hydrogen (hydrogen should be analyzed in advance) at a maximum
rate of 1.0 MPa per hour. Analyze the gas from the HP separator D-71101. If
the hydrogen content in the recycle gas does not reach 80v%, the reaction
section should be vented and pressurized with hydrogen until the hydrogen
concentration in the HP separator exceeds 80 v%.
8.3.2. Pressurize the reactor section to operating pressure with hydrogen at a
maximum rate of 1.0 MPa per hour and establish hydrogen circulation.
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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

8.3.3. When the hydrogen circulation is stabilized and the highest temperature in the
catalyst bed is less than 150°C, introduce carrier oil into the reactor.
8.3.4. Gradually adjust the charge rate according to unit condition until LHSV comes
up to 3.0 h-1
8.3.5. Within first 2 hours, if the resultant oil is dirty, drain the oil directly to the waste
oil tank and then divert the clean oil to feed surge drum to establish oil
circulation.
8.3.6. Raise reactor inlet temperature at the rate of 20°C /h until the highest
temperature in the catalyst bed reaches 175°C. Then start injection of DMDS
and hold the temperature at 175°C for 2 hours.
8.3.7. The presulfiding procedure and sulfiding agent rate are shown in the table
below.

8.3.8. Two criteria for the accomplishment of catalyst presulfiding:


 The H2S concentration in the recycle gas keeps on rising and exceeds
5000ppm(v);
 No water is drained out from the HP separator D-71101 twice in sequence.

8.3.9. Notes
 When the reactor inlet temperature reaches 230°C, the H2S concentration
should be in the range of 500 - 5000 ppm (v).
 Analyze H2S content of recycle gas twice per hour and hydrogen purity
every 4 hours, which should be over 80v%.

9. Establish Normal Operation


9.1. After the catalyst presulfiding, stop injection of DMDS and keep circulation of carrier
oil for about 2 hours.
9.2. Change the flow circuit; introduce the resultant oil from separator D-71101 to stripper
C-71101, and charge the feed surge drum D-71100 with normal feedstock. After
adjusting the reactor section and stripper to normal operation, analyze the
hydrotreated product from stripper bottom. It can be fed to reforming unit when it
meets the requirement.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71100.04 REV.0

9.3. Normal Operation Conditions:


 Reactor R-71101 pressure: not less than1.8 MPa
 LHSV: less than 6.0h-1
 H2/oil: not less than 90 Nm3/m3
 Reaction temperature: 280 - 320°C

10. Normal Shutdown Procedure

10.1. Shutdown If The Catalyst Doesn’t Need To Be Regenerated


10.1.1. After reforming feed cut, change C-71101 to circulation line, meanwhile
reduce R-71101 inlet temperature to 200˚C at the speed of 15- 20˚C / h and
reduce the charge rate gradually. However attention should be paid that
reducing charge rate will result in rapid coke accumulation on catalyst, so the
procedure should be followed: (first lowering the temperature and then
decreasing the charge rate). In this period, recycle gas circulation should be
continued.
10.1.2. Stop P-71101 and cut off feed, maintain D-71101 pressure not less than
1.8MPa. Continue recycle gas circulation at 200℃ for at least 4 hours, this
sweeps any remaining liquid hydrocarbons out of the reactor section. Try to
maintain pressure as long as possible using H2 addition line. Keep D-71101
liquid level at 30% during oil sweeping period, afterwards reduce all oil in D-
71101 to C-71101, close liquid control valve.
10.1.3. After gas sweeping is over, reduce R-71101 inlet to 150˚C, continue
circulation, when bed temperature less than 60˚C, stop K-711101. Then shut
off charge heater F-71101 burners
10.1.4. Reduce system pressure to flare upto 0.05MPa. Connect nitrogen from K-
71101 outlet for system inerting, until hydrogen hydrocarbon content of
sampling analysis is less than 1%.
10.1.5. When reaction section is cooled down, also cool C-71101 at the speed of 25-
30˚C/h. After feed is cut-off from prehydrotreatment, column are changed to
total reflux operation, gradually cooled down until reboiling is stopped, feed all
D-71103 oil into C-71101. Column bottom oil is reduced to offspec line. Close
onspec battery limit valve

10.2. Shutdown If The Catalyst Need To Be Regenerated


Please refer to chapter 4 of KRCIM 71100.03

ISSUE DATE: 20/03/06 - 43 -


KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION NORMAL OPERATION
CCR UNIT KRCIM 71100.05 REV.0

Contents: This document outlines the normal operating instructions of naphtha


pretreatment section of CCR unit. The text includes:

1. Operating Conditions
2. Process Variables
3. Troubleshooting
4. Analysis Control

1. Operating Conditions
1.1. Reaction System
 Design feed rate: 61, 897 kg/h
 Air speed: 6h-1
 Hydrogen oil volume ratio: 150
 Reaction temperature: 280-340˚C
 D-71l01Temperature: 40˚C
 D-71l01Pressure: 2.2MPa
1.2. C-71101
 Temperature top / bottom: 125/220˚C
 Tower top pressure: 1.2MPa
 Feed temperature: 141˚C
 Feed rate: 59560
 Reflux ratio (feed) 1.86
 Reflux temperature: 40˚C
 Tower bottom heat load: 6132 KW
 Tower bottom product rate: 50, 000 kg/h

2. Process Variables
2.1. Reaction System
2.1.1. Reaction temperature
Reaction temperature is a major approach to regulate oil quality generated from
prehydrotreatment reaction, and it is an adjustable operation parameter. Too
low temperature, will not guarantee hydrotreating depth and remove impurities.
Accordingly generated oil will be disqualified. High temperature facilitates
removing impurities and olefin saturation. However, over high reaction
temperature will intensify hydrocracking reaction, cause catalyst carbon deposit
and reduce activity and life time as well as increase energy consumption.
Reactor inlet temperature can be lowered in SOL(Catalyst Start of Life) due to
higher catalyst activity. Catalyst activity will falloff after some time indicating
EOL(Catalyst End of Life); reaction temperature can be increased.
In actual operation, reactor inlet temperature shall be properly regulated
according to product and feedstock quality.
Always ensure small temperature fluctuations in operation. 2 – 3˚C every time
when lifting temperature.
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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION NORMAL OPERATION
CCR UNIT KRCIM 71100.05 REV.0

2.1.2. Reaction pressure


Increasing reaction pressure to force hydrotreating reactions, increase refining
depth, facilitate to remove impurities, keep the activity of catalyst and extend
catalyst life. Nevertheless, over high reaction pressure will increase investment
and operating expenses and energy consumption. Usually hydrotreating
pressure depends on N2 content in raw material.
In actual operation, reaction pressure is not regulated generally. The only thing
is to keep stable pressure. The unit controls product separator's pressure at
1.95MPa through PICl002 and use hydrogen to compensate any pressure drop.

2.1.3. Space Velocity


Space velocity can be divided into volume space velocity and wieght space
velocity, which indicates contact time of feed and catalyst. Low space velocity
will result on a long contact time between feed and catalyst surface increasing
reaction temperature and severity of reactions;. So, after space velcity
variation, reaction temperature should be properly regulated.
Remember:
Always decrease reactor inlet temperature first and decrease feed flow rate
afterwards.
Always increase feed flow rate first and increase temperature afterwards
The unit's design space velocity is 6h-1 (LHSV).

2.1.4. Hydrogen-to-oil ratio


Hydrogen gas consumed in naphtha hydrogenation process is to guarantee
certain hydrogen-to-oil ratio leading to a better hydrogenation effect, preventing
activity reduction due to catalyst carbon deposit. If hydrogen-to-oil ratio is
increased, hydrogen partial pressure inside system will increase facilitating
hydrotreatment reactions, preventing coke deposits on catalyst and extending
catalyst service life. Moreover, hydrogen gas plays the role of heat-carrying
agent, bring reaction heat out of reactor and avoid catalyst over temperature.
But, excessive hydrogen-to-oil ratio will cause fall of reaction depth, increase of
heating furnace and cooling system load with no obvious advantage for
hydrotreatment.
In actual operation, hydrogen-to-oil ratio is limited by compressor discharge
rate and can not be regulated frequently. When feed rate is high, hydrogen-to-
oil ratio is often insufficient causing disqualified product quality. In such case,
increase reaction temperature for compensation, but this will shorten the life of
catalyst, so, keeping suitable hydrogen-to-oil ratio is very necessary.
Hydrogen oil volume ratio designed for the unit is 150.

2.2. C-71101
2.2.1. Pressure
Tower pressure is maintained through controller PICl004 to control the pressure
of reflux drum D-71103. During operation, if tower top pressure is reduced,
temperature rises and tower bottom oil get heavier; otherwise, tower bottom oil
get lighter.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION NORMAL OPERATION
CCR UNIT KRCIM 71100.05 REV.0

2.2.2. Temperature
Fractions quality takes regulating parameters as a major approach. In case of
column depressurization, properly reduce tower bottom temperature, otherwise
initial boiling point of tower bottom oil will rise.. Meanwhile, timely regulate
according to the change of feed quality and control tower bottom temperature
through F-71102 outlet temperature.

2.2.3. Reflux ratio


Reflux ratio is an important method to regulate fractionation effect.. Reflux rate
is controlled through controller FICl013 on reflux line.

2.2.4. Liquid level


Liquid level is an expression of system material balance. The height of tower
bottom liquid level will influence product quality, yield and operation balance.
Over high liquid level will also cause carrying over phenomena. Too low level
will cause tower bottom evacuation and destroy equipment. So, liquid level
under operation shall be stable, generally maintain around 60%. Keep reflux
drum level at 40- 60%.

3. Troubleshooting

3.1. C-71l01 bottom temperature controlled by F-71102 outlet temperature


Influencing factor Remedies
Fuel gas composition Regulate gas composition and drain
changed or mixed with fuel oil oil from knock-out drum
Unsteady feed Control liquid level and stabilize feed
Tower pressure change Use PV1004 to control reflux drum
pressure
Unsteady reflux rate Check reflex pump. Stabilize reflux
rate
Feed contain water Enhance tank dehydration or change
feeding tank
Reflux contain water Enhance D-71101/D-71103
dehydration

3.2. Cascade control between R-71101Inlet temperature and fuel gas pressure
Influencing factor Remedies
Fuel gas composition change According to composition change,
regulate fuel gas flow rate
Unsteady Feed Investigate. Find whether filter is
clogged. Stabilize feed
Unsteady hydrogen flow rate Check whether K-71101 fails and
troubleshoot
Feed contain water Enhance tank dehydration or change
feeding tank
Unsteady D-71101 pressure Use PV1002 and hydrogen make-up
control line to control D-71101 pressure
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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION NORMAL OPERATION
CCR UNIT KRCIM 71100.05 REV.0

3.3. C-71101 pressure controlled with pressure control valve PV1004 on D-71103
gas outlet
Influencing factor Remedies
Feed rate fluctuation Control liquid level and stabilize feed
rate
Feed property change Regulate operation and check water
Tower bottom temperature Stabilize reboiling furnace operation,
fluctuation stabilize tower bottom temperature
Reflux rate unsteady Check reflex pump normal or not,
regulate reflux rate
A-71102A/B cooling effect Check air cooling belt and regulate
poor cooling water rate

3.4. C-71101 level control


Influencing factor Remedies
Tower pressure change Stablize pressure
Tower bottom temperature Stabilize tower bottom temperature
fluctuation
Feed or reflux with water Enhance tank dehydration or change
feeding tank
Feed property change According to composition change,
properly regulate operation

3.5. Prehydrotreatment system pressure fluctuation


Influencing factor Remedies
Circulating hydrogen Switch to standby compressor
compressor malfunction
causes unsteady air
discharge
Prehydrotreatment feed Regulate and control stable feed
fluctuation
Furnace outlet temperature Enhance furnace stable operation
fluctuation
PIC1002 malfunction Contact instrument maintenance
D-71101 Liquid level Stable operation can reduce the
fluctuation fluctuation of liquid level

Make-up hydrogen pressure Regulate make-up hydrogen quantity at


surge booster outlet

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION NORMAL OPERATION
CCR UNIT KRCIM 71100.05 REV.0

3.6. Arsenic, lead & copper content exceed limits in hydrotreated naphtha
Influencing factor Remedies
Too high arsenic, lead & Contact dispatch, change feedstock
copper content in feedstock
Catalyst activity falls Increase reaction temperature.
E-71101A/B Feed Feed reformer with desulphurized naphtha and
exchanger leak treat the exchanger leakage
Low reaction temperature Increase reaction temperature or pressure
or pressure
Test analysis error Contact lab for reanalysis

3.7. Hydrotreated naphtha sulfur & nitrogen is disqualified


Influencing factor Regulation method
Reaction temperature too low, Increase reaction temperature
reaction depth is insufficient
Reaction pressure too low, Increase hydrogen-to-oil ratio, so as to
denitrogenation is poor increase reaction hydrogen partial pressure
High sulfur content in Properly control reaction temperature,
feedstock meanwhile report total value and change
feeding tank
High nitrogen content in Contact dispatch, urge gasoline
feedstock hydrogenation
E-71101A/B Feed exchanger Feed reformer with desulphurized naphtha
leak and treat the exchanger leakage

Stripping tower operation is Regulate stripping tower operation


abnormal
Test analysis error Contact lab for reanalysis and verification

3.8. Water disqualified in hydrotreated Naphtha


Influencing factor Regulation method
D-71101 water is not properly D-71101 control water drum interface,
drained, or interface failure check water level manually
C-71101Improper tower Regulate operating temperature or pressure
bottom temperature or
pressure control
Test analysis error According to AI-2001, determine reanalysis
or not.

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KRC NAPHTHA PRETREATMENT SECTION
PRODUCTION & OPERATION NORMAL OPERATION
CCR UNIT KRCIM 71100.05 REV.0

4. Analysis Control
4.1. Recommended Methods And Frequency
The frequencies given here below are related to routine operation.

Stream Test Item Test Method Frequency


SN
Name SEI SEI SEI
Relative
ASTM D4052 1/W
Density
Distillation °c ASTM D86 1/W
Sulfur,ppm ASTM D5453 1/W
SN- Pretreatment
Nitrogen,ppm ASTM D4629 Occas
71101 Feedstock
Bromine
SH/T0630 1/W
Index
Composition
SH/T0239 1/W
(PONA)
Separator H2S Detector Tube 1/D
SN-
Overhead
71105 Composition Q/SHO18.212 1/W
Gas
SN- Separator
PH GB/T6920 Occas
71106 Bottom Water
Relative
ASTM D4052 1/W
Stripper Density
SN-
Reflux Drum Composition
71102 SH/T0239 Occas
Liquid (PONA)
Mercaptans ASTM D3227 Occas
Stripper Composition Q/SHO18.212 Occas
SN- Reflux Drum
71107 Overhead H2S Detector Tube Occas
Gas

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KRC
PRODUCTION & OPERATION REFORMING SECTION
CCR UNIT

Table of Contents

INTRODUCTION (KRCIM 71200.01)


1. Unit introduction..............................................................................................1
2. Manual Structure.............................................................................................2

BASIC KNOWLEDGE (KRCIM 71200.02)


1. Basis Of Design..............................................................................................3
2. Unit Description.............................................................................................11

PROCESS THEORY (KRCIM 71200.03)


1. Thermodynamics And Kinetics......................................................................14
2. Chemical Reactions.......................................................................................15
3. Catalyst..........................................................................................................24
4. Process Variables..........................................................................................37
5. Supplements..................................................................................................42

PREPARATION FOR INITIAL START-UP (KRCIM 71200.04)


1. Plant Inspection.............................................................................................46
2. Cleaning of Piping and Equipment................................................................57

START-UP OPERATIONS 1 (KRCIM 71200.05)


1. Start-Up Requirement....................................................................................67
2. Unit Purging...................................................................................................67
3. Initial Leak Test..............................................................................................83
4. Unit Dryout.....................................................................................................89
5. Catalyst Loading............................................................................................93
6. Second Leak Test And Partial Inerting........................................................102
7. Supplements................................................................................................103

START-UP OPERATIONS 2 (KRCIM 71200.06)


1. First Startup Of The Unit..............................................................................127
2. Catalyst Circulation, Heating and Drying Procedures..................................128
3. Final Inerting................................................................................................138
4. Reforming Section Startup...........................................................................140
5. Oil In.............................................................................................................143
6. Regeneration Startup...................................................................................148
7. Unit Restart..................................................................................................154
8. Supplements................................................................................................158

FURNACES OPERATION (KRCIM 71200.07)


1. Dryout General Instructions.........................................................................169
2. Start-up Procedure.......................................................................................172
3. Daily Operation Of Heating Furnaces..........................................................174
4. Troubleshooting...........................................................................................175
5. Shutdown.....................................................................................................176
KRC
PRODUCTION & OPERATION REFORMING SECTION
CCR UNIT

OPERATING CONDITIONS & CONTROL (KRCIM 71200.08)


1. Operation Influencing Parameters...............................................................178
2. Principles Of Key Parameters Control.........................................................183
3. Adjustment Of Operating Conditions...........................................................184
4. Troubleshooting...........................................................................................185
5. Operation Conventional Control..................................................................190
6. Analysis Control...........................................................................................191
7. Supplements................................................................................................194

SHUTDOWN PROCEDURE (KRCIM 71200.09)


1. Overall Shutdown Operation........................................................................202
2. Short Duration Normal Shutdown Scheme..................................................202
3. Normal Shutdown Scheme..........................................................................204
4. Normal Shutdown With Catalyst Unloading.................................................207
KRC REFORMING SECTION
PRODUCTION & OPERATION INTRODUCTION
CCR UNIT KRCIM 71200.01 REV.0

Contents: This document outlines the structure of CCR (Reforming Section)


operation manual. The text includes:

1. Unit Introduction
2. Manual Structure

1. Unit Introduction

1.1. General
Continuous Catalytic Reforming Unit (CCR) of Khartoum Refinery Company is built
under the expansion project of the refinery, phase II. The unit is designed by
Sinopec Engineering Incorporation. The process utilizes Axens's "State of the art"
moving catalyst bed with continuous catalyst regeneration.
The unit is designed to process 400,000 metrics tons per year and to operate at a
severity of RON 98 with an on-stream factor of 8000 hours/year.

1.2. Unit Function


The purpose of the CCR unit is to produce a high octane number reformate, which is
a main component of the gasoline pool, and a hydrogen rich gas.
CCR unit feed is hydrotreated coker Naphtha that has low potential aromatics
content (26.98 wt%) mixed with straight run Naphtha. Due to the presence of
contaminants in all cases, more or less elaborated naphtha pretreating is always
necessary.
CCR unit is a catalytic reforming process of naphtha, based on AXENS’s licensed
technology. It includes two sections:
• The naphtha catalytic reforming itself, including, reactors heaters, effluent recovery
and stabilization.
• The catalyst circulation and regeneration which involve solid handling and moving
bed technology.
The reforming reactions take place in moving bed catalytic reactors from which the
catalyst is withdrawn, then regenerated and recycled. The catalyst circulation and
regeneration are performed on a continuous basis with full automatic control of all
the operations.
A high temperature (in the range of 500°C) is required to promote the chemical
reactions which improve octane number; Hence the need for a preheating of the
feed.
Moreover, some of the desirable reactions are highly endothermic. This leads to split
the bulk of the catalyst into several reactors with intermediate heaters.
The high performance of the CCR unit process is largely owed to low pressure
operation coupled with high temperatures; which, in conventional fixed bed reactors

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KRC REFORMING SECTION
PRODUCTION & OPERATION INTRODUCTION
CCR UNIT KRCIM 71200.01 REV.0

would lead to very short cycle length. Hence CCR unit involves continuous catalyst
regeneration.
Continuous regeneration eliminates the need of shutdown for regeneration of the
earlier fixed bed reformers. It also minimizes the amount of catalyst in the unit, while
allowing high reformate yield and quality.

1.3. Configuration Of The Unit


This unit consists of several components, including
 Pretreatment section (unit 71100)
 Reforming section (unit 71200)
 Catalyst regeneration section (unit 71300)
 Utilities section (unit 71400)
 Waste heat boiler section (unit 71500)

2. Manual Structure
The design information and operating instructions of the Continuous Catalytic Reforming
Unit (unit71) are covered by six different volumes as follow:

KRCIM 71100 is dedicated to pretreatment section


KRCIM 71200 is dedicated to reforming section
KRCIM 71300 is dedicated to catalyst regeneration section
KRCIM 71500 is dedicated to waste heat boiler section
KRCIM 71EMP is dedicated to emergency procedures
KRCIM 71TRS is dedicated to test run scheme

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KRC REFORMING SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

Contents: This document outlines the general description of reforming section of


CCR unit. The text includes:

1. Basis Of Design
2. Unit Description

1. Basis Of Design

1.1. Duty Of Unit


The naphtha feed steam is treated at very low pressure in three adiabatic reactors
over a moving bimetallic catalyst bed in a hydrogen environment.
This catalyst is withdrawn at a fixed rate from the reaction section to be regenerated
in a continuous catalyst regeneration unit and returned to the reaction section. This
is unit 71300 of this project and is covered in a separate volume of this manual.
There are three primary products from this reforming section:
 a reformate with high aromatics content,
 a rich hydrogen gas,
 an LPG stream or C3-C5 cut, depending on the requested operation in the
stabilization section.
There is also a light ends stream to fuel gas which is predominantly C 1-C2
components from the hydrocracking reactions.
The design, operation and control strategies of this unit are such as to maximize the
production of aromatics and to ensure consistent quality of the rich hydrogen gas as
this may impact on the performance of the upstream and downstream hydrogen
users

1.2. Feed Specifications


The plant shall be designed to process 400,000 metric tons per year of mixture of
naphthas. The Plant shall be designed to operate from 60 to 115 % of its design
capacity, based on 8000 operating hours per year.
The feed to the Catalytic Reformer consists of the following hydrotreated naphtha
mixture:
Straight Run Naphtha 20.0
Hydrotreated Coker Naphtha 80.0
100.0 wt %

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KRC REFORMING SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

The following table summarizes the characteristics of the Reformer feed

Capacity, t/y 400,000


Capacity, BPSD 10,410
Sp. Gr. 0.725

Composition, wt P N A
%
C5 - 3.74 0.37 0.00
C6 8.93 0.14
2.27
C7 13.32 4.81 0.90
C8 17.32 7.00 2.00
C9 15.98 5.59 2.25
C10 8.99 2.12 0.94
C11 + 3.12 0.19 0.00
Total 71.42 22.35 6.23

1.2.1. Impurities
The reforming catalyst is a high purity alumina based catalyst, impregnated with
platinum and promotors. It is highly sensitive to impurities in the feedstock.
Some are considered reversible poisons, others irreversible.
Following table lists the maximum allowable limits of impurities in the feed. It is
critically important than the performance of the naphtha hydrotreating is such
that the impurity levels in the reforming feed do not exceed these levels.
Discussions regarding feed poisons and their effects will be discussed further in
this book.

Maximum contaminant levels in reforming feed

Contaminant wt ppm
Sulphur 0.5
Nitrogen (organic) 0.5
Water 5
Arsenic 5 ppb
Olefins 0
Diolefins 0
Metals 5 ppb
Halogens (F, C1) 1

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KRC REFORMING SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

1.3. Studied Cases


Two cases have been studied, related to the catalyst operations:
 Start of Life (SOL) operation.
 End of Life (EOL) operation.

1.4. Products Specification


There are essentially three primary products:
 a reformate with high aromatics content,
 an hydrogen rich gas,
 an LPG stream.
There is an additional purge gas stream to fuel gas from the LPG absorber drum.
This is mostly C1, C2 light ends from the cracking reactions.

1.4.1. Reformate
The reformate is the product collected at stabilizer bottoms which the
specification is shown in the following table:
SOL/EOL
Spgr 0.796
RVP, kPa 33.1
RON C 98
MON C 88
C4 content, wt% 1.0 maxi
ASTM distillation, °C
IBP 45
10% 70
50% 127
90% 165
EBP 205
Flowrate (kg/h) SOL 44 082
EOL 43 379

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KRC REFORMING SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

1.4.2. Hydrogen rich gas


Composition, mol %
SOL EOL
H2 92.7 91.0
C1 2.1 2.7
C2 1.3 1.7
C3 1.3 1.7
C4 1.3 1.6
C5+ 1.3 1.3
Total 100.0 100.0
Molecular weight 5.0 5.5
HCl content, vppm 0.5 maxi 0.5 maxi
(1)
Flowrate (kg/h) 4 232 4 471
(1)
at the outlet of chloride absorbers

1.4.3. LPG

Composition, wt %
SOL EOL
C2- 5.6 5.4
C3 26.6 24.8
C4 66.9 68.9
C5+ 0.9 0.9
Total 100.0 100.0
Spgr 0.536 0.538
Flowrate (kg/h) 1 157 1 615

1.5. Battery Limit Conditions


Pressure, MPa g Temperature,
°C
Heavy naphtha feed 1.2 110
Hydrogen rich gas 2.0 40
Reformate 0.6 42
LPG 1.3 39
C1-C2 cut to fuel gas 1.5 (*) 42
(*) Before PV valve.

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PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

1.6. Utilities Conditions And Site Information

1.6.1. Climatic Data


 Maximum temperature: 46.7°C
 Design maximum ambient temperature: 45°C
 Design minimum temperature: 6.2°C
 Relative humidity
- Average: 27%
- Maximum: 44%
 Barometric pressure
- Minimum: 96.3 kPa
- Maximum: 96.9 kPa
- Average: 96.56 kPa
1.6.2. Steam

Pressure Temperature
Medium pressure
Minimum 3.3 MPa g 380°C
Normal 3.5 MPa g 400°C
Maximum 3.7 MPa g 420°C
Low pressure
Minimum 0.9 MPa g 220°C
Normal 1.0 MPa g 250°C
Maximum 280°C

1.6.3. Water
Cooling water - supply
Minimum: 0.40 MPa g 32°C
Maximum: 0.50 MPa g 32°C

Cooling water - Return


Minimum: 0.25 MPa g 42°C

Boiler feed water


Minimum 1.7 MPa g for low pressure
Normal: 5.0 MPa g for medium pressure
Demineralized water (regeneration)
Normal: 0.40 MPa g ambient
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KRC REFORMING SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

1.6.4. Air
Pressure Temperature
Plant Air
Minimum: 0.60 MPa g
Normal: 0.80 MPa g

Instrument Air (for catalyst regeneration)


Normal: 0.80 MPa g
Dew point: -10°C

1.6.5. Nitrogen

Availability: 0.8 MPa g


or 2.5 MPa g
Quality: Purity : 99.99 %

1.6.6. Fuel
Fuel gas
Minimum: 0.30 MPa g
Normal: 0.35 MPa g
Maximum: 0.40 MPa g

1.6.7. Flare header pressure

Normal: 0.05 MPa g


Design: 2.50 MPa g

1.7. Reforming Operating Conditions


1.7.2. Reactors Operating Conditions
In order to maintain the expected performance, the reforming reactors are
designed to operated under specific conditions for Start Of Life (S.O.L.) and
End Of Life (E.O.L.).

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KRC REFORMING SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

SOL EOL
Reforming reactors inlet/outlet temperature
st
1 reactor R-71201 514/393 529/418

2nd reactor R-71202 514/430 529/452

3rd reactor R-71203 514/446 529/466

*
Space velocity, WHSV h-1 1.9 1.9

Recycle ratio** 1.5 1.5

Reactor average operating pressure, 0.35 0.35


MPa g

* Ratio of kg/hr of fresh feed to kg of catalyst inside of the three reactors.


** Ratio of pure H2 mol/h in the recycle gas to mol/h of fresh feed.

1.7.3. Stabilizer Column operating conditions


SOL/EOL
Top temperature, °C 79
Bottom temperature, °C 234
Top pressure, MPa g 1.600
Bottom pressure, MPa g 1.630
Reflux drum temperature, °C 40
Reflux drum pressure, MPa g 1.550
Reflux/feed ratio wt 0.30/0.34

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KRC REFORMING SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

1.7.4. Yields
The estimated ex-reactors yields are expressed including recycle gas :

SOL, wt % EOL, wt
%
H2 5.34 5.02
METHANE 1.08 1.37
ETHANE 1.38 1.75
PROPANE 2.68 3.38
NBUTANE 3.41 4.29
IBUTANE 2.18 2.75
NPENTANE 2.53 2.50
IPENTANE 4.84 4.77
NHEXANE 2.46 2.40
IHEXANES 7.65 7.48
METHYLCYCLOPENTANE 0.75 0.73
CYCLOHEXANE 0.00 0.00
BENZENE 2.13 2.07
C7 PARAFFINS 7.45 7.23
C7 NAPHTENES 0.07 0.06
TOLUENE 8.91 8.63
C8 PARAFFINS 3.97 3.84
C8 NAPHTENES 0.04 0.04
C8 AROMATICS 17.56 16.98
C9 PARAFFINS 0.68 0.66
C9 NAPTHENES 0.01 0.01
C9 AROMATICS 16.93 16.36
C10+ PARAFFINS 0.00 0.00
C10+ NAPHTENES 0.00 0.00
C10+ AROMATICS 7.94 7.68
C5+ 83.92 75.29
Total 100.00 100.00

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KRC REFORMING SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71200.02 REV.0

2. Unit Description

2.1. Introduction
Naphtha feed to a Catalytic Reforming unit typically contains C6 to C10 paraffins,
naphthenes and aromatics. The purpose of this reforming process is to produce
aromatics from naphthenes and paraffins either for use as a high octane gasoline
blending component or as a source of specific aromatic compounds.
Naphthenes convert rapidly and efficiently to aromatics. Paraffins do not, requiring
higher severity conditions and even then conversion is slow and inefficient.
In this process, conversion is achieved by passing the naphtha over a slow moving
bimetallic catalyst bed in three adiabatic reactors, in the presence of hydrogen at
relatively high temperature and low pressure. Operating under these conditions of
low pressure and high temperature, the rate of coke laydown on the catalyst is
relatively high. A semi-regenerative type process is impractical in this case, a
continuous catalytic regeneration unit is necessary. In this process, catalyst is
withdrawn from the reaction section at a fixed rate, regenerated in the continuous
catalytic regeneration unit and returned fresh to the reaction section.
The rate of catalyst withdrawal and regeneration ensures a consistently highly active
catalyst with a low carbon content and controlled chloride/water content. This
maximises yields of both reformate and high quality hydrogen off-gas.

2.2. Process Flow Description

2.2.1. Reaction section


The Reformer Feed enters the reforming unit battery limits. A chloriding agent
(C2Cl4) and water are injected before the flow control letdown valves to control
the water-chloride equilibrium (if the continuous regenerator is out of service)
for optimum reforming catalyst performance. A sulfiding agent is injected
continuously in the feed to prevent metallic coking in the reactors. After letdown
through the feed flow control valves, the naphtha is mixed with recycle
hydrogen from K-71201 in the exchanger E-71201. This is a plate type heat
exchanger designed for minimum pressure drop and maximum heat recovery
against reactor effluent. The combined naphtha feed and recycle hydrogen are
preheated here against the third reactor effluent and then are further heated to
the required first reactor inlet temperature in preheater F-71201.
In the first reactor R-71201, the reactions are predominantly endothermic and
therefore the reactor effluent requires reheating in the first interheater F-71202
to the required inlet temperature of R-71202. The reactions in R-71202 are less
endothermic but still require reheating in F-71203 before entering the third
reactor R-71203. The effluent leaves reactor R-71203 at approximately 446-
466°C depending on the position in the cycle and at 0.375 MPa g.
In the three reactors the feed contacts the reforming catalyst which is divided
approximately in the ratio 20/30/50. In the continuous regeneration process the
catalyst circulates continuously:
 in the reactors, in the space between the scallops and the central pipe
from the top to the bottom,
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CCR UNIT KRCIM 71200.02 REV.0

 from one reactor bottom to the top of the next one,


 from the last reactor to the regeneration unit for regeneration,
 from the regeneration unit, the regenerated catalyst returns to the 1st
reactor.
In the regeneration unit, the catalyst is regenerated by means of an automatic
regeneration loop system. Catalyst circulation is achieved either by gravity flow
or by gas lift systems. A detailed description of the regeneration unit is provided
in the corresponding volume.
Leaving R-71203, the effluent, after heat exchange in E-71201 against reactor
feed, is cooled by air exchange in A-71201 before entering the separator drum
D-71201. A portion of the separated gas is compressed by the recycle gas
compressor K-71201 driven by a steam turbine and is recycled to the reactors.
The remaining gas which constitutes the hydrogen production gas is routed to a
boosting and recontacting section to improve hydrogen purity and recover liquid
yield.
The separated liquid is pumped by P-71201 to be recontacted in the
recontacting section.

2.2.2. Boosting and recontacting section


The hydrogen production gas from D-71201, mixed with the reduction gas
coming from the Regeneration and Circulation Section - Unit 71300, is routed to
the H2 rich gas compressor K-71202A/B through a knockout drum D-71207. K-
71202A/B provides a two stage compression of the H2 production gas from
0.210 MPa g to 2.140 MPa g. An interstage air cooler A-71203 and knockout
drum D-71202 are required between the stages to cool the compressed stream
and remove the condensed hydrocarbons. The condensed liquid, on level
control of D-71202 is pressured back to the reactor effluent upstream of D-
71201. The compressed hydrogen is recontacted with the separated liquid from
D-71201. The reaction section primary pressure control point is on D-71201
and is controlled via a kick back loop from the interstage drum D-71202 to
upstream of D-71207. This is the control point the operator uses to control the
third reactor R-71203 pressure.
The recontacted mixture is then air cooled in A-71204. The target temperature
is 40°C in the recontacting drum D-71203. These conditions of the final stage
separator for the hydrogen production gas are designed for a high content of
hydrogen in the hydrogen rich gas product.
A portion of the separated hydrogen rich gas is withdrawn for regeneration
purposes. The remaining gas is sent to the chloride absorbers D-71206 A/B
before supplying the H2 rich gas users outside battery limits at limits at 2.00
MPa g.
The separated liquid in the recontacting drum D-71203 is sent under level
control to the LPG recovery and stabilization section.

2.2.3. LPG recovery and stabilization section


This separated liquid is then contacted with stabilizer off-gas and allowed to
separate in D-71205, the stabilizer absorber drum. The purpose of this step is
to recover the maximum quantity of LPG, i.e. C3 and C4's from the stabilizer
overheads.
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Vapor from D-71205 is routed to fuel gas under pressure control. This stream is
predominantly light ends i.e. C1 and C2's and this controls the stabilizer
operating pressure. Separated liquid from this drum is pumped by P-71204
through the stabilizer feed/bottom exchanger E-71208 to enter the stabilizer C-
71201. The stabilizer operating at an average of 1.70 MPa g, reduces the C4 in
the reformate to less than 1.0 wt %. The stabilizer is reboiled with a fired
reboiler F-71205, circulating with reboiler pump P-71202, with temperature
control on stabilizer.
C-71201 overheads are partially condensed in air cooler A-71202 and
subcooled to collect in D-71204, the stabilizer reflux drum. The overhead vapor
is routed back to D-71205 for LPG recovery. The separated liquid is pumped by
P-71203 under flow control back to the top of C-71201 as reflux. A split stream
of the liquid is withdrawn as LPG from P-71203, discharge under level/flow
control and is routed to LPG battery limit.
Bottoms from the stabilizer after partial cooling in the stabilizer feed/bottom
exchanger constitutes the reformate which is sent under flow control with level
reset to battery limits.

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Contents: The aim of the information given in this document is to provide enough
theoretical basic background to support the instructions given in the
chapters that follow: Startup of the unit, Operation of the unit, Shutdown
of the unit.
The objective is to help the operators to better understand the reasons
of the operating instructions and enable them to make wise decisions,
should the circumstances deviate from what is covered in the operating
instructions.

1. Thermodynamics And Kinetics


2. Chemical Reactions
3. Catalyst
4. Process Variables
5. Supplements

1. Thermodynamics And Kinetics


For any chemical reaction the thermodynamics dictates the possibility of its occurrence
and the amount of products and unconverted reactants. Under certain conditions (P, T)
some reactions are 100% completed i. e., all the reactants are converted into products.
Others are in equilibrium i.e., part of the reactants only are converted. The amount of
products and reactants at equilibrium depends upon the operating conditions and is
dictated by the thermodynamics. Note that the thermodynamics does not mention the
time required to reach the equilibrium or the full completion of a reaction.
Kinetics dictates the rate of a chemical reaction (i.e., the amount of feed that disappears
in, say, one second). Kinetics (rate of reaction) is dependant upon operating conditions
but can also be widely modified through the use of properly selected catalysts. One
reaction (or a family of reactions) is generally enhanced by a specific catalyst.
In other words, thermodynamics dictates the ultimate equilibrium composition assuming
the time is infinite. Kinetics enables the prediction of the composition after a finite time.
Since time is always limited, when reactions are competing, kinetics is generally
predominant.
A catalyst generally consists of a support (earth oxide, alumina, silica, magnesia...) on
which (a) finely divided metal(s) is (are) deposited.
The metal is always responsible for the catalytic action. Very often, the support has also a
catalytic action linked to its chemical nature.
A catalyst is not consumed but can be deactivated either by impurities in the feed or by
some of the products of the chemical reactions involved, resulting in coke deposit on the
catalyst.

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2. Chemical Reactions

2.1. Desirable Reactions


Reactions which lead to an increased octane number and to high purity hydrogen
production. These are the reactions to promote.

The heat of the reactions mentioned hereafter as well as their relative rate are
necessary to understand the process. They are listed for the ease of reference in
Table 1, below. A catalyst is being used to promote the desirable reactions at the
expense of the adverse ones through its action on reaction kinetics.

TABLE1
Reforming reactions heat of reaction - relative rate of reaction
Reactions Heat of reaction Relative rate
(1) KCAL/MOLE (2) approx.
Naphthenes dehydrogenation - 50 30
Paraffin dehydrocyclization - 60 1 (base)
Isomerization: Paraffins +2
3
Naphthenes +4
Cracking + 10 0.5
(1) Heat of reaction < 0 = endothermic reaction.
(2) For pressure below 1.5 MPa.

2.1.1. Desirable reactions with hydrogen production

Naphthenes dehydrogenation
Naphthenic compounds i.e. cyclohexane, methylcyclohexane,
dimethylcyclohexane up to C10 naphthenes are dehydrogenated respectively
into benzene, toluene, xylenes, C9 and C10 aromatics with the production of 3
moles of hydrogen per mole of naphthene.
The cyclohexane reaction, for instance, writes as follows:
CH CH
2
HC CH HC
2 2 CH
+ 3H
2
HC CH HC CH
2 2
CH CH
2
Cyclohexane Benzene

Note: Cyclohexane and benzene are generally schematically represented as follows:

Cyclohexane Benzene

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Thermodynamically the reaction is highly endothermic and is favored by high


temperature and low pressure. In addition, the higher the number of carbon
atoms, the higher the aromatics production at equilibrium.
From a kinetic view point, the speed of reaction increases with temperature
(Fig. 2) and is not affected by the hydrogen partial pressure (Fig. 1). The rate of
reaction is high compared to other reactions (table 1). It also increases with the
number of carbon atoms.

At the selected operating conditions the reaction is very fast and almost total. It
is promoted by the metallic function of the catalyst. Since it yields a high octane
product, promoting this reaction is most desirable. Refer to octane number
below:

RON MON
Cyclohexane = 83 77.2
Methylcyclohexane = 74.8 71.1
1.3 dimethylcyclohexane = 71.7 71.
Benzene = 114.8 > 100
Toluene = 120 103.5
m-Xylene = 117.5 115.
RON: Research Octane Number
MON: Motor Octane Number

The table below shows the effect of parameters on dehydrogenation reactions

Effect on dehydrogenation due to


Increase of
Thermodynamics Kinetics
Pressure decreases non affected
Temperature increases increases
H2/HC ratio (1) slightly decreases slightly decreases
(1)Ratio of pure hydrogen (mole) to hydrocarbon feed (mole)

Paraffins dehydrocyclization
This is a several step process which applies either to the normal paraffins
(linear) or ISO-paraffins (branched). It involves a dehydrogenation with a
release of one hydrogen mole followed by a molecular rearrangement to form a
naphthene and the subsequent dehydrogenation of the naphthene. The
molecular rearrangement to build a naphthene is the most difficult reaction to
promote but the subsequent aromatization of the naphthene yields a noticeable
octane increase.

The reaction can be summarized as follows:

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CH CH CH CH CH CH
2 2 2 2 2
+H
CH CH CH CH CH CH CH 2
3 2 2 3 3 CH 2 3

C H C H
7 16 7 14

CH CH
2 2
CH CH CH CH
2 2
H C CH
2 3
CH CH CH CH
3 2 3 CH CH
2 2

Met hylcyclohexane

CH CH CH CH
2 2
C
H C CH CH
3 HC CH + 3H
2 3 2

CH CH CH CH
2 2
T oluene

The paraffin dehydrocyclization step becomes easier as the molecular weight of


the paraffin increases, however the tendency of paraffins to hydrocrack
increases concurrently (Fig.3).
Kinetically, the rate of dehydrocyclization increases with low pressure and high
temperature (Fig.1&2), but altogether, at the selected operating conditions, this
rate is much lower than that of naphthene dehydrogenation (30/1). The reaction
is promoted by both catalytic functions, metallic and acidic.

Effect of parameters on paraffin dehydrocyclization


Effect on dehydrocyclization due to
Increase of
Thermodynamics Kinetics
Pressure decreases decreases
Temperature increases increases
H2/HC ratio slightly decreases slightly decreases

2.1.2. Desirable reactions without hydrogen production

Linear paraffins isomerization


Reaction is as follows:

C H
7 16 C H
7 16

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These reactions are fast, slightly exothermic and do not affect the number of
carbons. The thermodynamic equilibrium of isoparaffins to paraffins depends
mainly of the temperature (see table hereafter). The pressure has no effect.
Iso-N paraffin equilibria
Carbon atom C4 C5 C6 C7 C8
% Isoparaffin at 44 58 72 80 88
500°C

The paraffins isomerization results in a slight increase of the octane number.


From a kinetic view point (Fig.1&2) high temperature favors isomerization but
hydrogen partial pressure is indifferent. These reactions are promoted by the
acidic function of the catalyst support.

Napththenes isomerization
The isomerization of an alkylcyclopentane into an alkylcyclohexane involves a
ring rearrangement and is desirable because of the subsequent
dehydrogenation of the alkylcyclohexane into an aromatic. Owing to the
difficulty of the ring rearrangement, the risk of ring opening resulting in a
paraffin is high.
The reaction is slightly endothermic. The reaction can be summarized as
follows:

Alkylcyclopent ane Alkylcyclohexane


(Ethylcyclopentane) (Methylcyclohexane)

Theoretically, at the selected operating temperature (about 500°C) the


thermodynamics limits the alkylcyclohexane formation. But the subsequent
dehydrogenation of the alkylcyclohexane into an aromatic shifts the reaction
towards the desired direction. This type of reaction is also easier for higher
carbon number. The octane number increase is significant when considering
the end product (aromatics) as shown:

RON MON
Ethylcyclopentane = 67.2 61.2
Methylcyclohexane = 74.8 71.1
Toluene = 120 103.5

2.2. Adverse Reactions


Reactions which lead to a decreased octane number, a decrease in hydrogen purity
or a loss in products yield. These are the reactions to minimize.

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Cracking
Cracking reactions include hydrocracking and hydrogenolysis reactions.
Hydrocracking affects either paraffins (normal or iso) or naphthenes. It involves both
the acid and metallic function of the catalyst. It is, to some extent, a parallel reaction
to paraffin dehydrocyclization.
It can be schematized by a first step of dehydrogenation which involves the metallic
function of the catalyst, followed by a breakage of the resulting olefin and the
hydrogenation of the subsequent short chain olefin. The second reaction is
promoted by the acidic function of the catalyst.

(m)
+H
2
C H C H
7 16 7 14

(a)
+
+H
2
C H
7 14 C H C H
4 8 3 8

(m)
+H
2
C H C H
4 8 4 10

(m) Catalyst metallic function


(a) Catalyst acidic function

The first reaction involves the same reactants as the dehydrocyclisation and is
likewise catalysed by the metallic function.
Hydrocracking also affects the naphthenes, the overall reaction can be
summarized as follows:

+H
2
C H
6 14
CH - C H
3 5 9

or

+H
2
C H
CH - C H 7 16
3 6 11

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At the selected operating conditions, hydrocracking reaction could be almost


complete. Fortunately it is somewhat limited by its kinetics. Compared to its
desirable concurrent reaction (dehydrocyclization), hydrocracking becomes
significant as the temperature increases. It is also favored by high pressure.
The main effects of hydrocracking are:
 a decrease of paraffins in the reformate which results in an increase of the
aromatics percentage (i.e. an increase in octane) and a loss of reformate.
 a decrease in hydrogen production.
 an increase of LPG production.

Hydrogenolysis
This undesirable reaction has some similarity with hydrocracking since it involves
hydrogen consumption and molecule breakage. But it is promoted by the metallic
function of the catalyst and leads to lighter hydrocarbon C1 + C2 - even less
valuable than LPG (C3 + C4).
It can be schematized as follows:
+H CH +
4
2
C H C H
7 16 6 14
or

+H C H +
2 6
C H 2
7 16 C H
5 12
Like hydrocracking it is exothermic and favored by high pressure and high
temperature.
Both hydrogenolysis and hydrocracking may induce runaway reactions owing to their
exothermicity.

Hydrodealkylation
Hydrodealkylation is the breakage of the branched radical (-CH3 or -C2H5) of an
aromatic ring.
Xylene (two radical groups) can be dealkylated into toluene (one radical group)
which in turn can be dealkylated to benzene.
The standard representation is:

+H + CH
4
2

Xylene T oluene

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+H + CH
4
2

T oluene Benzene
Hydrodealkylation consumes hydrogen and produces methane. It is favored by high
temperature and high pressure and promoted by the metallic function of the catalyst.
At the operating conditions and with the selected catalyst this reaction is not
significant.

Alkylation
Alkylation is a condensation reaction which adds an olefin molecule on an aromatic
ring. It results in an aromatic with an increased molecular weight. The reaction writes
as follows:

CH
3
+ CH = CH - CH HC
2 3
CH
3
Benzene Propylene Isopropylbenzene
This reaction, promoted by the catalyst metallic function, is not hydrogen consuming.
But it leads to heavier molecules which may increase the end point of the product. In
addition the high molecular weight hydrocarbons also have a high tendency to form
coke. This reaction must be avoided.

Dismutation
Two toluene rings (one branched CH3 radical) can dismute to produce one benzene
ring (no branched radical) and one xylene ring (two branched radicals), as shown:

+ +

T oluene T oluene Benzene Xylene


This reaction, promoted by the catalyst metallic function, occurs only in very severe
conditions of temperature and pressure. This reaction is negligible with the selected
catalyst at the selected operating conditions.

Coking
Coke formation on the catalyst results from a very complex group of chemical
reactions, the detailed mechanism of which is not fully known yet.
Coke formation is linked to heavy unsaturated products such as polynuclear
aromatics (or polycyclics which can be dehydrogenated) resulting either from the
feed or from the polymerization of aromatics involved in some of the reforming
reactions (dehydrocyclisation, dismutation,...). Traces of heavy olefins or diolefins
may also result from the reforming reactions (dehydrocyclization, alkylation, for
instance) and promote coke formation.

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A high end boiling point of the feed likely means greater amount of polyaromatics
and then a higher coking tendency. Since polymerization is promoted by high
temperature, poor distribution in a reactor favors local high temperatures and coke
build up.
Coke deposit on the catalyst support reduces the active contact area and greatly
reduces catalyst activity.
Low pressure unfortunately favors coke formation (see Fig. 1). This is why a low
pressure reforming (which has a lot of advantages) requires a continuous
regenerated catalyst. In CCR the continuous catalyst regeneration loop maintains a
controlled low coke content on the catalyst while operating at low pressure.

2.3. Kinetic Analysis Of The Chemical Reactions

The effect of the main operating conditions on the rate of the reactions involved in
the reforming process using the selected catalyst (Refer to “Catalyst selection and
description”) is summarized below.

2.3.1. Effect of hydrogen partial pressure

Figure 1 show, with a logarithmic scale, the relative rate of the various reactions
as a function of hydrogen partial pressure. The dehydrogenation rate is used as
reference and taken at 100 (Log 100 = 2). Other reaction rates are measured
against this reference.
At 1.0 MPa hydrogen partial pressure, the dehydrogenation of naphthene is
about 10 times, faster than isomerization, 30 times faster than
dehydrocyclization and 50-60 times faster than cracking (hydrocracking and
hydrogenolysis).
At relatively high pressure (above 2.0 MPa) the rate of coking is low compared
to the other reactions but it increases noticeably at lower pressure.
To sum up, figure 1 shows that there is an incentive to operate at low
pressure: cracking rate will be reduced and dehydrocyclization rate
increased.
On another hand thermodynamics also favors low pressure for
dehydrogenation and dehydrocyclization. The only drawback of low pressure is
the high coking rate but this is compensated by continuous catalyst
regeneration.

2.3.2. Effect of temperature

Temperature influences the rate of the various reactions as shown in Fig 2.


Energy of activation is linked to the slope of the curves. Dehydrogenation has a
moderate energy of activation ( ~ 20 Kcal. mole -1) as does isomerization
( ~ 25 Kcal. mole -1) and consequently temperature only slightly increases the
rate of these reactions. Cracking and coking have higher energy of activation
(45 and 35 Kcal. mole -1 respectively). The rate of these undesirable reactions
is more significantly increased by temperature.

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To sum up, a higher temperature clearly favors the undesirable reactions


more than the desirable one. However a controlled temperature rise is
required during the catalyst life to maintain catalyst activity and therefore
product octane.

2.3.3. Effect of carbon number

The kinetic study of the chemical reactions becomes even more complicated
owing to the presence of molecules with different numbers of carbon atoms.
As is the case for thermodynamic equilibriums, it appears that the rates of the
reactions are affected by the length of the chain of the reactant. Figure 3
presents the rates of dehydrocyclization and cracking of C6 to C10 paraffins
related to that of n-heptane, as a function of the number of carbon atoms of
reactant.
Figure 3 shows that the cracking reaction rate, (the curve represents in fact the
sum of hydrocracking and hydrogenolysis), increases regularly with the number
of carbon atoms, whereas dehydrocyclization rate exhibits a sudden increase
between hexane and heptane as well as between heptane and octane, while
the variation between the higher homologues remains relatively slight.
To sum up, the dehydrocyclization of C6 paraffins to benzene is more
difficult than that of C7 paraffin to toluene, which itself is more difficult
than that of C8 paraffin to xylenes. Accordingly the most suitable fraction
to feed a reforming process is the C7-C10 fraction.

CONCLUSIONS:
From the above analysis it can be concluded:
 Dehydrogenation reactions are very fast, about one order of magnitude
faster than the other reactions.
 Low pressure favors all desirable reactions and reduces cracking. To
compensate the detrimental effect of low pressure on coking, low
pressure reformer requires continuous catalyst regeneration.
 An increase in temperature favors the kinetics of dehydrogenation,
isomerization, dehydrocyclization, but accelerates the degradation
reactions (cracking, coking) even more. Consequently an increase in
temperature leads to an increased octane associated with a decrease in
reformate yield.
 The reaction rates of such important reactions as paraffins
dehydrocyclization increase noticeably with the number of carbon atoms.
Cyclization is faster for C8 paraffin than for C7, and for C7 than for C6.
Consequently the C7 - C10 fraction is the most suitable feed.

2.4. Catalyst Distribution In Reactors


Thermodynamics and kinetics have shown that there is an optimum operating
temperature range, approximately 450°C-520°C in order to simultaneously favor the
rate of the desirable reactions and limit the undesirable ones to an acceptable level.
For each specific case, the most appropriate operating temperature is selected

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taking account of the feed quality (PNA, distillation range ...) and product
requirement (octane).
Owing to the great endothermicity of the most important and desirable reactions
(naphthenes dehydrogenation and paraffins dehydrocyclization) this optimum
temperature cannot be sustained through out the whole catalyst volume. In addition,
dehydrogenation is also, by far, the fastest reaction, which means that the
temperature drops very sharply over the first part of the catalyst. In order to restore
the catalyst activity, when temperature has dropped to a certain level which depends
upon the reactions involved, the reactor feed is reheated. To achieve this, the
catalyst is distributed in three reactors and intermediate heaters are provided.
Figures 4 and 5 illustrate this question, Figure 4 shows for a given feed (Paraffins:
45% LV, Naphthenes 45% LV, Aromatics 10% LV) the profile of the amount of P.N.A
along the catalyst volume. In this case there is no need to have more than 20% of
the catalyst in the first reactor because the naphthenes dehydrogenation results in a
temperature too low to sustain the reaction any longer. The reactor effluent is
reheated to allow for the naphthenes hydrogenation to continue and the paraffin
dehydrocyclization to start. Over the next 30% of catalyst, distributed in the 2 nd
reactor, temperature drops again to a level where reheating is required to enable the
paraffin hydrocyclization to proceed.
The catalyst distribution in this case is:
R1 = 20%
R2 = 30%
R3 = 50%
Each specific case has, obviously, a specific catalyst distribution.
In a somewhat simplified but practical way, for operational guidance, the main
reactions take place in the various reactors in the following order:
1st reactor:
 Dehydrogenation
 Isomerization
2nd reactor:
 Dehydrogenation
 Isomerization
 Cracking
 Dehydrocyclization
3rd reactor:
 Cracking
 Dehydrocyclization

3. Catalyst
3.1. Activity, Selectivity, Stability
The main characteristics of a catalyst other than its physical and mechanical
properties are:
The activity which expresses the catalyst ability to increase the rate of the reactions
involved. It is measured by the temperature at which the catalyst must be operated
to produce a reformate of a given octane number, for a given feed and given
operating conditions.

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The selectivity expresses the catalyst ability to favor desirable reactions rather than
others. It is practically measured by the C5+ reformate and hydrogen yields, for a
given feed and octane number, and given operating conditions.
The stability characterizes the change with time of the catalyst performance (i.e.
activity, selectivity) when operating conditions and feed are stable. It is chiefly the
coke deposit which affects stability, through its inhibition of the catalyst acidity and
decrease of metal contact area. Traces of metal in the feed also affect stability
adversely.
Stability is generally measured by the amount of feed treated per unit weight of
catalyst (i.e. m3 of feed per kg of catalyst). C5+ wt reformate yield at steady
conditions is also an indirect measure of the stability.

3.2. CCR Reforming Catalyst Characteristics


The catalysts are a multimetallic catalyst consisting of platinum plus metal promoters
on an alumina support.
Its main features are:
 High purity alumina support having a strong resistance to attrition
 High stability and selectivity due to the platinum associated with other metals
(promoters)
 High regenerability idealy suited for the continuous regeneration operations
The association of the above mentioned qualities with the continuous regeneration
gives the following advantages:
 High reformate yield
 High hydrogen yield
 High stream factor
 Low catalyst inventory

3.3. Catalyst Activity Mechanism


The catalyst affects reaction rates through its two different functions: metallic and
acidic, which promote different type of reactions.
Dehydrogenation and hydrogenation reactions are enhanced by the catalyst metal.
Structural rearrangements of the molecules (from linear to cyclic for instance) which
involve a reorganization of the carbon bonds are primarily catalyzed by the acidic
function of the support.
Because of its high activity in hydrogenation and dehydrocyclization, platinum has
been selected for the base catalytic metal. Promoters have been added to improve
catalyst selectivity and stability.
The support is high purity alumina (acidic function) which is chiefly active for the
cyclization of the paraffins to aromatics.
In short, the main reactions involved in reforming processes are catalyzed
essentially either by the support or the metal functions, as indicated below:

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Dehydrogenation Metallic function


Dehydrocyclization Metallic + acidic functions
Isomerization Acidic function
Hydrogenolysis Metallic function
Hydrocracking Metallic + acidic function

3.3.1. Metallic function


For a maximum catalyst activity, the metal must be highly dispersed on the
alumina support and under the minimum possible particle size (actual figure is
in the range of 1.10-6 mm). This high dispersion and micrometric particle size,
which result from the special manufacturing process, must be maintained
during the catalyst life by the use of proper operating conditions .

A decrease of the performance of the metallic function can be caused by :


 a poisoning of the metallic phase
 an alteration of the metallic phase on the support
Indeed, a sintering of the metallic phase may occur during the first regeneration
step (coke burning), due to local high temperatures and high level of partial
pressure of water. The oxychlorination step, which is led right after coke
burning, allows a good re-dispersion of this metallic phase.

3.3.2. Acidic function

A certain level of acidity of the catalyst support is required to promote some of


the desired reactions (isomerization, dehydrocyclization) which consequently
lead to a maximization of the desired performance (reformate production,
hydrogen or octane number yields). The optimum level of acidity changes
somewhat with these desired performance.
The acidity of the catalyst is dependant on the amount of chlorine which is fixed
on the catalyst at the manufacturing stage. In operation, the chlorine content of
the catalyst varies with the recycle gas moisture and the elution of chlorine by
water, which happens mainly during the coke burning step, due to the formation
of combustion water. That’s why this level must be adjusted during
oxychlorination and maintained in the optimum range of 0.9% to 1.1% wt.
A simplified representation of the catalyst support chemical structure and the
processes of chlorination and chlore elution by water is as follows:

OH Cl OH OH
elution
Al Al + H 20 Al Al + ClH
chlorination
O O

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The simplified theory, generally accepted today, is that the optimum acidity
level (which varies with the requested performance) is a function of ratio of the -
OH bonds to the Cl- bonds, which are adsorbed at the catalyst surface. This
ratio, in turn, is a function of the water and HCl content in the recycle gas,
because of the equilibrium which exists between water and HCl in the recycle
and OH- and Cl- bonds on the catalyst.
Good acidity of the catalyst is controlled by the balance between H 2O and HCl.
An excess of water in the recycle will shift the balance towards excess of OH-
and thus reduce the activity.
Conversely, if the amount of water in the recycle is too low (an infrequent
case) the catalyst is reputed too dry, and the OH- to Cl- balance is shifted
towards Cl-. In other words, the catalyst is over-chlorinated, which means its

acidic function is exacerbated (trend to hydrocracking). Of course, over-


chlorination of the catalyst may result merely from the accidental presence of
chlorine, or uncontrolled addition, in the feed.
There are a couple of other occurrences worth mentioning:
 If a catalyst is excessively dry (i.e. it has been operated with a deficiency
of water for some time) it will exhibit a very high acidic function indicated
by in an increased hydrocracking activity.
 If a catalyst (especially in case of excessively dry catalyst) undergoes a
water upset (amount of water in the recycle over 50 ppm vol.) a situation
may occur where the water displaces the chlorine from the first reactors
towards the last reactor with a subsequent temporary increase of the
acidic function and hydrocracking activity in the last reactor.
To conclude, for an optimum operation of the reforming Unit:
The water content in the recycle must be maintained between 15 to 25
ppm volume and the associated HCl content should be approximately 1
ppm volume. Note that the determination of the HCl content is not very
reliable.
The chlorine content of the regenerated catalyst must be maintained
between 0.9 to 1.1% wt. Operators can adjust the chlorine injection rate in the
oxychlorination zone of the regenerator, based on catalyst analysis.

3.3.3. Alteration of catalyst activity

The causes and consequences of catalyst activity loss (due to an unbalance of


either the acidic or metallic function) are listed in Table 2. Remedial actions are
covered in 3.4 (Catalyst contaminants).

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TABLE 2
Decrease of acidic Increase of acidic Decrease of metallic
function function function

a) Elution of chlorine due a) Over chlorinated a) Temporary reversible


to high water content in catalyst due to: poisoning by sulfur
the recycle – regeneration b) Permanent poisoning by
b) Nitrogen compounds chlorination metals (Refer to Catalyst
(loss of Cl through – chlorine in the feed contaminants)
CAUSES

NH4Cl) refer to Catalyst – or too low water in c) Poor regeneration


contaminants recycle conditions and/or
b) High water content in reduction
the recycle (upset) on
a very dry catalyst
(the acidic function
increase is temporary)
a) Decreased octane a) Slight increase in a) Large decrease in octane
b) Decreased LPG octane b) Decreased delta T in first
CONSEQUENCES

production b) Decrease in liquid reactor


c) Increased Cl production product and H2 yields c) Decreased C1 + C2
related to C1-C4 cut c) Increased LPG production
d) Increased recycle gas production d) Increased liquid
purity d) Decreased C1 production
e) Increased liquid product production related to e) Large decrease of H2
yield C1-C4 cut production
e) Decreased recycle f) Decreased recycle gas
gas purity purity

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CCR UNIT KRCIM 71200.03 REV.0

3.4. Catalyst Contaminants


Catalyst contaminants are classified in two categories. Temporary poisons (also
called sometimes inhibitors) and permanent poisons.
Temporary poisons are those which can be removed from the catalyst without a
shutdown and for which the catalyst proper activity and selectivity is restored once
the contaminant disappears.
The effect of temporary poisons, if the operators wants to maintain the operating
conditions prevailing before the poisoning, is a temporary decrease of performance.
The most common temporary poisons (inhibitors) of reforming catalysts are
sulfur, organic nitrogen, water and oxygenated organics, halogens.
Coke, in a regenerative unit, although it could fall within this category is treated
separately.
Permanents poisons are those which induce a loss of activity which cannot be
recovered, even with a regeneration and which is so severe that the catalyst must be
replaced.
For conventional fixed bed catalysts as well as for continuously regenerated
catalysts, the main permanent poisons are arsenic, lead, copper, iron, nickel,
chromium.
In order to ensure the optimum use of the catalyst, a proper design shall include:
 The removal of poisons from the feed prior to its introduction to the unit ;
 The necessary procedures to remove, as far as possible, the temporary
poisons from the contaminated catalyst.
Impurities from the feed are removed by pretreating units. However their efficiency is
never complete, and generally limited depending upon the type of impurities to be
removed. In addition, a poor adjustment of the operating conditions of the pretreating
unit results in a decreased efficiency.
A smooth and successful operation of this reforming unit requires the proper
adjustment and control of the operating conditions of the pretreating unit.

3.4.1. Temporary poisons


Sulfur
Sulfur is the most common impurity found in the feed of any reforming unit. The
maximum allowable concentration is 0.5 ppm wt expressed as S. Whenever
possible, operation at lower sulfur content will provide additional catalyst
stability and selectivity.
Mechanism
Poisoning is caused by H2S, either contained in the unit feed, or resulting from
the decomposition, on the catalyst, of sulfur compounds contained in the feed.

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H2S reacts with platinum according to the equilibrium reaction:

Pt + H2S PtS + H2
and consequently it reduces the activity of the catalyst while decreasing the
metallic contact area.
The same type of reaction occurs with H2S towards the other catalyst
promoters, and further reduces the catalyst activity.
Effect of sulfur contamination
Sulfur contamination inhibits the metal function of the catalyst. This is indicated
by:
 A decrease in hydrogen and liquid product yields
 A decrease in recycle purity
 An increase in hydrocracking (LPG yield increase)
 A reduced temperature drop in the reactors
Prevention and causes of contamination
Sulfur removal is achieved by pretreating the naphtha feed, which results in
H2S production. Poor operation of the pretreater is generally the cause of sulfur
poisoning of the reforming catalyst:
 Either low activity of the hydrotreater catalyst
 Or too low hydrotreater reactor temperature
which leads to an insufficient sulfur removal. Unsatisfactory operation of the
hydrotreater stripper can also result in dissolved H2S being fed to the reforming
unit.
An additional protection to avoid H2S upsets to the reforming unit is to provide
a sulfur guard reactor on the feed.
Detection
Analytical methods are available to detect sulfur in the unit feed. A very easy
way, however, is to check sulfur content in the recycle gas using Draeger
tubes. The H2S content in the recycle which corresponds to the 0.5 ppm wt in
the feed, is approximately 1 ppm (volume).
Remedies:
When the sulfur content in the recycle gas increases, the reactor inlet
temperature must be reduced.
Typically for an H2S level of 5 vol. ppm in the recycle the reactor inlet
temperature must be lowered to 480°C ; the reformer feed must be reduced
accordingly to maintain product quality (octane number). These conditions must
be maintained until the cause of the upset has been found and corrected.
The high severity operating conditions can only be resumed when the H 2S
content in the recycle gas is lower than 1 ppm vol.

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Nitrogen
Nitrogen is less frequently present in the reforming feed than sulfur. Scarcely
present in straight run naphtha, nitrogen is a usual impurity of cracked naphtha
and may also result from injection of amine based corrosion inhibitors.
The maximum allowable concentration in the feed is 0.5 wt ppm expressed as
organic nitrogen.
Mechanism
In fact, organic compounds containing nitrogen are responsible for inhibition but
nitrogen gas itself (N2) has no detrimental effect.
Contamination is due to NH3 formed by decomposition of compounds
containing organic nitrogen, on the catalyst. Then NH3 which is alkaline, reacts
with chlorine decreasing the acidic function of the catalyst and producing
ammonium chloride NH4Cl. This compound is volatile in the conditions of the
reactors and is eliminated inducing a loss of chlorine.
The reaction can be schematized as follows:
Cl OH Cl Cl OH OH

NH3 + H O2 + Al Al Al
Al Al Al + HCl + NH
3
O O O O

and HCl + NH NH Cl
3 4
Effect of nitrogen contamination
Nitrogen contamination reduces the acidic function and is indicated by:
 A decrease in octane
 An increased hydrogen production
 A reduced reactor temperature drop
On top of this, ammonium chloride in the recycle gas can deposit in coolers,
separators compressors etc. creating mechanical problems.
It is worth remembering that 0.5 ppm wt of organic nitrogen in the feed leads to
approximately 2 T/year of NH4 Cl for a 1 106 T/y unit.
Prevention and causes of contamination
Organic nitrogen removal is also achieved by naphtha pretreating of the feed.
But it shall be emphasized that nitrogen removal is more difficult than sulfur.
Efficient nitrogen removal often requires the use of a specific catalyst, also
active for desulfurization, but generally operating at higher hydrogen partial
pressure. Naphtha, with high nitrogen content must not be fed to a pretreater
not designed for it.

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Cracked naphthas are generally characterized by high organic nitrogen


content, consequently cracked naphthas shall never be introduced to a
pretreater designed to process straight-run feeds without getting
technical advice from the licensor.
In the pretreating unit, decomposition of nitrogen compounds gives NH 3.
However the amount is generally limited and easy to remove by stripping. The
corrosion inhibitor (amine based), usually injected in the pretreatment stripper
shall be selected to be decomposed at the condition of the stripper to avoid
contamination of the stripper bottom product (Reforming feed). In fact, the
presence of nitrogen compounds in the feed is typically due to a low activity of
the pretreatment catalyst towards denitrification.
Detection
There is no available method for ammonia detection in the recycle gas. Thus
laboratory analyses need to be performed on the feed to detect nitrogen
compounds.
Remedies
When nitrogen contamination is detected operators must:
 Increase the chlorination agent injection in the regenerator to increase
the chlorine level of the regenerated catalyst up to 1.4 to 1.5% wt.
 Not try to make up for the drop in octane number of the reformate by an
increase of the reactor inlet temperature. This will only increase the loss
of chlorine.
 Take the necessary actions to lower the nitrogen content down to the
acceptable figure of 0.5 ppm wt.

Water and oxygenated organic compounds


Oxygenated organic compounds (methanol, MTBE, TAME, phenol...) are
converted into water at reactor conditions.
Water is not exactly a poison since some water is necessary to activate the
acidic function of the catalyst. However, in usual practice, elimination of water
from reforming feed is a major concern of operators, because an excess of
water leads to a decrease in catalyst activity.
Water is often present in naphtha feeds, moreover water is frequently injected
in reforming feed hydrotreaters. The maximum allowable content is 4 ppm (wt)
in the feed which corresponds to approximately 20 ppm volume in the recycle
gas for typical conditions (P = 0.4 MPa a ; T = 40°C at the separator).
Mechanism
Water affects the acidic function of the catalyst, as previously explained
Prevention and causes of contamination
Water removal in usually achieved in the stripper of the feed hydrotreater.
Generally contamination by water results from a poor operations of this
equipment.

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Detection
Since water contamination is a major concern of the operator, on line analyzer
is usually provided in the recycle gas line.
Operating experience shows that the optimum water content in the recycle gas
must be within a range of 15 to 25 ppm (vol.). The associated chlorine level will
then be between 1 to 2 ppm vol.
Above 50 ppm vol. of water, the reactor inlet temperature must be lowered to
reduce the chlorine elution from the catalyst. The following figures are generally
accepted:
 50 ppm water Temperature < 480°C
 100 ppm water Temperature < 460°C
Below 10 ppm of water in the recycle gas, the catalyst acidic function is
enhanced. Water injection must be used: 1 ppm wt in the feed results in an
increment of 2 to 5 ppm vol. in the recycle.
Remedies
In case of water upset,
 Adjust chlorine injection to make up for the increased chlorine loss
 Decrease reactor inlet temperature as indicated above
 Restore operating conditions upstream of the unit to reduce water
contamination
 Check amount of oxygenated compounds in the feed

Halogens (chlorine, fluorine)


The maximum allowable amount in the unit feed is 0.5 ppm wt for each of them.
Mechanism
The presence of chlorine in the feed modifies the acidic function of the catalyst
and promote the hydrocracking reaction. Once chlorine is eliminated, the
proper chlorine balance of the catalyst can be restored.
The effect of fluorine is similar but it is more difficult to remove from the
catalyst.
Effect of chlorine, fluorine contamination
Hydrocracking reactions are enhanced causing:
 Lower liquid product yield
 Higher LPG and C1 yields
 Slightly higher octane
Prevention and causes of contamination
Chlorine and fluorine are sometimes present in crude owing to the field
production techniques. They are normally eliminated in the pretreatment stage.

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3.4.2. Permanent poisons

Permanent poisons have been defined as contaminants which irreversibly


damage the catalyst.
Table 3 hereunder lists the main permanent poisons as well as their acceptable
level and their most likely source.

TABLE 3
Poisons Max. level (wt) Source
Arsenic 5 ppb max Cracked Naphthas
Lead 5 ppb max Recycled slops
Copper < detection limit Corrosion
Mercury 5 ppb max Naphtha - condensates
Iron < detection limit Corrosion
Silicon < detection limit Additives (foaming)
Nickel < detection limit Corrosion
Chromium < detection limit Corrosion

Mechanism
Most metals poison the metal function (platinum and promoter) of the catalyst.
Metal poisons tend to affect the first reactor, then to break through and affect
nd
the 2 reactor. The first reactor is typically the reactor where the poisoning is
first detected.
Effect of metal contamination
Metal contamination is characterized by:
 A dramatic decrease of the T in the first reactor associated with an
increased T in the second reactor
 A decrease in octane number
 An increase in liquid product yield
 In addition, mechanical problems may result from the collection of
corrosion products (scale, rust...) in the first layer of the first catalyst bed,
or the accumulation of scale, rust in the dead ends, of the first reactor
Prevention and causes of contamination:
The contaminants and the source of contamination are listed in Table 3 above.
Prevention consists of adequate hydrotreating and appropriate material
selection to limit corrosion.
Metal poisons are generally partially retained on the upstream hydrotreating
catalysts. However the retention capacity is limited and breakthrough may
occur. Such a breakthrough would result in a very harmful situation for the unit
since theses poisons would not be eliminated by the catalyst regeneration.
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It is very important to check periodically the metal content of the hydrotreater


feed and product. It enables to monitor the performance of the hydrotreater with
regard to demetallization and also to be warned of a possible metal
breakthrough of the hydrotreatment catalyst, providing the maximum metal
retention of the hydrotreatment catalyst is known. When the metal loading of
the hydrotreater catalyst is nearing this figure, the hydrotreatment catalyst
needs be replaced.
3.4.3. Coke
The coke which deposits on the catalyst is a temporary poison since its
detrimental effect is reversible through regeneration. Owing to its paramount
importance in catalytic reformers, coke formation is treated separately.
Mechanism:
Polynuclear aromatics are the assumed precursors of coke formation. They
result either from slight amounts of polynuclear aromatics in the feed
(depending upon the nature of the crude and the end point of the feed) or from
the aromatics producing reactions of the reforming process itself. Some diolefin
intermediates of reforming reactions are also potential coke precursors.
Coke deposit affects the catalyst activity by reducing the contact area between
catalyst and the reactants.
The normal coke content of the catalyst lies between 4 to 6% by weight.
“Normal” means through-put, feedstock quality and severity within the range
defined in the relevant section of the process book, and catalyst circulation
within the design operating range.
Catalyst with noticeably higher coke content can be handled provided a few
precautions are taken (Refer Adjustment of operating conditions).
Somewhere below 3% wt of coke, the operation of the regeneration may
become unsteady and it is recommended to momentarily shut it down.
Prevention and causes of contamination:
Since coke formation is inherently associated with the reforming reactions,
there is no real way to avoid it. One can only minimize it.
Coke will be reduced by a decrease of reactor temperature (i.e. if severity is
reduced) and an increase in hydrogen circulation. Low total pressure, to the
contrary, favors coke formation. Hence the need for a continuous regeneration
for reforming units which operate at high severities (high temperature) and low
pressure.
Another parameter to watch, to minimize coke is the feed end point, in order to
limit heavy polyaromatics amount. The maximum allowable feed end point must
not exceed 180° C (ASTM D86). When the feed results from a mixture of
different streams, each stream must comply with the 180°C end point.

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AR / CR SERIES CATALYSTS CUMULATIVE POISONS LIMIT


(Beyond these limits catalyst performances start to deteriorate)

S wt ppm = ~ 300
Pb wt ppm = ~ 200
As wt ppm = ~ 200
Zn wt ppm = ~ 400
Co wt ppm = ~ 400
Cr wt ppm = ~ 400
Mo wt ppm = ~ 400
Cd wt ppm = ~ 400
Cu wt ppm = ~ 400
Fe wt ppm = ~ 3000
Si wt ppm = ~ 400
Na wt ppm = ~ 300
Ca wt ppm = ~ 300
K wt ppm = ~ 300

3.5. Axens’ CR 401 Catalyst Properties

For the reforming catalyst, CR 401 from Axens is used.

CR 401 is a bimetallic, platinum-tin, reforming catalyst developed to produce high

octane gasoline from straight run naphtha.

CR 401 has been designed for continuous regeneration reforming process :

 High selectivity offering maximum C5+ and hydrogen yield at very low
pressure.

 High mechanical strength offering minimum abrasion in catalyst transfer

 through lifts between reactors.

 High regenerability based on a very low surface area decrease after


numerous regenerations.

Low coke make offer the possibility to increase throughput without revamping of

regenerator.
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4. Process Variables
4.1. Independent Variables
The process variables are:
 Pressure
 Temperature
 Space velocity
 Hydrogen partial pressure or H2/HC recycle ratio
 Quality of the feed
The above are independent variables: each of them can be fixed by the operator -
within the operating range of the equipment - independently from the others.
For one set of independent variables, there is only performance of the unit i.e. one
set of values for:
 Product yields
 Product quality (octane)
 Catalyst stability (coke make)
In this chapter we examine the effect on the unit performance of each independent
variable taken separately.

4.1.1. Pressure
Hydrogen partial pressure is the basic variable because of its inherent effect on
reaction rates. But for the ease of understanding total reactor pressure can be
used. Reactor pressure is most accurately defined as the average catalyst
pressure. Due to catalyst distribution in the reactors, it is usually close to the
last reactor inlet pressure.
All the hydrogen producing reactions i.e. dehydrogenation, dehydrocyclisation
are enhanced by low pressure.

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The lower the pressure the higher the yields of both reformate and hydrogen for
a given octane number. This is the reason for minimizing unit pressure drop
and operating at the lowest practical pressure. Low pressure however
increases the coke make.
Operators action on pressure is limited:
 Operating pressure rise is limited by equipment design pressure
 Operating pressure lowering is limited by recycle compressor design
power and intake volume

4.1.2. Temperature

Catalyst activity is directly related to reactor temperature. Thus the most direct
operating variable available for the operator, to control product quality and
yields, is the reactor inlet temperature.
In the CCR unit the coke amount on the catalyst is maintained at a constant low
level through the continuous regeneration. Consequently a temperature
adjustment is required only:
 To change the reformate octane
 To process a different feed quantity
 To process a different feed quality
 To balance a temporary loss of activity due to a temporary poisoning
 To balance catalyst ageing which occurs slowly over several years
An increase of the reactor inlet temperature results in :
 An increased conversion of the non aromatic compounds of the feed
mainly the paraffins
But since the hydrocracking reaction is more favored than the cyclization of
paraffins, the end result is:
 An increased octane but a decrease in reformate yield
 An increase of the coke deposit

4.1.3. Space Velocity


The space velocity is the amount of liquid feed, expressed in weight (or in
volume) which is processed in one hour, divided by the amount of catalyst,
expressed in weight (or in volume). Weight (volume) of feed and catalyst must
be expressed with the same unit.
Weight Hourly Space Velocity: WHSV = Weight of feed(per hour)
Weight of catalyst

Volume of feed at 15 C (per hour)


Liquid Hourly Space Velocity: LHSV =
Volume of catalyst

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The inverse of the liquid hourly space velocity i.e. (LHSV)-1 is linked with the
residence time of the feed in the reactor. The space velocity then affects
directly the kinetics of the reforming reactions.
A decrease in the space velocity means an increased residence time, hence a
higher severity which results in increased octane, lower reformate yield, higher
coke deposit.
When changing feed rate, an important recommendation derives from the
above:
Always decrease reactor inlet temperature first and decrease feed flow
rate afterwards.
Always increase feed flow rate first and increase temperature afterwards.

4.1.4. Hydrogen to hydrocarbon ratio and hydrogen partial pressure


The H2/HC ratio is the ratio of pure hydrogen in the recycle gas (mole/hour) to
the feed flow rate (mole/hour).
H2 Pure hydrogen (mole/hour) in recycle
=
HC Naphtha flow rate (mole/hour)
Hydrogen partial pressure is linked to the H2/HC ratio. Since there is, in
practice, little flexibility in the total pressure, hydrogen partial pressure is mainly
adjusted through recycle flow.
Recycle hydrogen is necessary in the reformer operation for purposes of
catalyst stability. It has the effect of sweeping the reaction products and
condensable materials from the catalyst and supplying the catalyst with readily
available hydrogen. An increase in H2/HC ratio will move the naphtha through
the reactors at a faster rate and supply a greater heat sink for the endothermic
heat of reaction. The end result is an increased stability.
A lower H2/HC ratio decreases the hydrogen partial pressure and increases
coke formation. Within the typical operating range, the H 2/HC ratio has little
influence on product quality or yields. It is not a variable that the operator
typically adjusts, it is set by design based on an economic balance between
equipment sizing i.e. recycle compressors, fired heaters and the regeneration
unit.
Moreover, for a given unit, the amount of recycle is limited by the recycle
compressor characteristics (power, suction flow).

4.1.5. Feed quality


Distillation range
Light fractions have a poor naphthenic and aromatic content and consequently
a high C6 paraffinic content. Cyclization of C6 paraffins to aromatics is more
difficult than cyclization of C7 or C8 paraffins, as discussed before.

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Hence, for a required octane number, the lighter the feed the higher the
required severity or, conversely, at constant severity, low initial boiling point
results in lower aromatic and hydrogen yields.
In recent years, the restriction of benzene content in gasoline has resulted in
selecting feed with IBP above 82°C (180°F) to eliminate cyclohexane.
Heavy fractions have a high naphthenic and aromatic hydrocarbons content,
thus they need a lower severity to obtain good yields. But these fractions
contain also polycyclic compounds which produce a high coke deposit on the
catalyst. High final boiling point of the feed is favorable up to a certain level,
detrimental above. An end boiling point above 180°C (350°F) is generally not
recommended.
Chemical composition
The detailed chemical composition of the feed is determined by gas
chromatography analysis. This analysis is necessary to predict the aromatics
and hydrogen production as well as the severity of the operation.
Even if not sufficient for a complete prediction, an index of characterization of
the feedstocks related to the actual and potential aromatics content of the feed,
proved very useful. N + 2A has long been used (N and A volume % of
naphthenes and aromatics in the feed). AXENS now uses 0.85 N + A which is
found to be more representative.
The higher this index, the lower the severity of operation to meet the same
product specifications. The lower this index (i.e. the higher the paraffins
content), the higher the severity of operation to meet the same product
specifications as the dehydrocyclization of paraffins becomes important.
Impurities in the feed
The catalyst activity can be reduced, either temporarily or permanently by
poisons contained in the feed (refer to “Catalyst contaminants”). Table 4
specifies the maximum allowable amount of each contaminant.

TABLE 4
Maximum allowable impurities (wt) in the feed

Component Max. allowable (wt)


Sulfur (as sulfur) 0.5 ppm max
Organic nitrogen (as nitrogen) 0.5 ppm max
Water or oxygenated products 4. ppm max
Chlorine 0.5 ppm max
Fluorine 0.5 ppm max
Arsenic 5 ppb max
Lead 5 ppb max
Copper 5 ppb max

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PRODUCTION & OPERATION PROCESS THEORY
CCR UNIT KRCIM 71200.03 REV.0
Mercury 5 ppb max
Iron < detection limit
Silicon < detection limit
Nickel < detection limit
Chromium < detection limit
Sodium < detection limit
Cadmium < detection limit
Potassium < detection limit

4.1.6. Summary
Table 5 summarizes the theoretical effect on the unit performance of each
independent process variable taken separately.

TABLE 4
EFFECT OF PROCESS VARIABLES

Increased RONC Reformate yield Coke deposit

Pressure

Temperature

Space velocity

H2/HC ratio

A + 0.85 N

Naphtha
End boiling point
Quality

Initial boiling point

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PRODUCTION & OPERATION PROCESS THEORY
CCR UNIT KRCIM 71200.03 REV.0

5. Supplements

 Fig 1: Relative rate of reaction Vs Hydrogen partial pressure

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PRODUCTION & OPERATION PROCESS THEORY
CCR UNIT KRCIM 71200.03 REV.0

 Fig 2: Relative rate of reaction Vs Temperature

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PRODUCTION & OPERATION PROCESS THEORY
CCR UNIT KRCIM 71200.03 REV.0

 Fig 3: Relative rate of reaction Vs No. of carbon atoms

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PRODUCTION & OPERATION PROCESS THEORY
CCR UNIT KRCIM 71200.03 REV.0

 Fig 4&5: Catalyst distribution in the reactors

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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

Contents: The information described hereafter concern the preliminary operations


prior to the first start-up of the Unit, that is those activities required to
bring the facilities to a "ready for Commissioning" condition after
Construction Completion. At that stage these Precommissioning
activities are implemented by the Construction Contractor
Precommissioning team, as they are part of his scope of work and
responsibility, and witnessed by KRC Personnel.
Unit operators may have to repeat some of the specific prior-to-start-up
activities detailed here, which are fully integrated in the start-up
sequence of this Unit, during subsequent Start-Up, especially after major
overhaul. The following topics are discussed:

1. Plant Inspection
2. Cleaning of Piping and Equipment

1. Plant Inspection
The plant should be carefully checked to assure that it is constructed according to the
applicable plans, drawings and specifications. A check against the P&ID's is done for
piping, equipment and instrumentation. A, "punch list" of missing, incomplete, or incorrect
items is then prepared for correction.
This check is carried out during the final stages of construction work, under the direction
of the Pre-commissioning group in charge of the unit. Typically, this checking (which can
be called conformity to P&ID's check) is useful when construction progress is 70% or
above. Several checks can be made simultaneously depending upon the completeness of
each section or system of unit at that time.
Smooth Start-Up will depend on a large degree on the thoroughness with which the unit is
checked out beforehand. Every installation details must be checked against the design
specifications and standards and for good construction practice.

1.1. Equipment Inspection


1.1.1. Vessels, Exchangers And Reactors

General Inspection
A general inspection of the equipment is made against the design drawings
after erection. This check includes:
 Verification of temperature/pressure and vacuum rating on nameplate
 Verification of lining condition (if applicable)
 Nozzle location, size, flanges face
 Thermowell location and length of immersion
 Cleanliness

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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

Sliding Supports
When equipment experiences a temperature change it undergoes thermal
growth. Supports are provided to allow and guide this growth. It is therefore of
great importance that all supports are inspected and special attention is given
to large horizontal vessels and heat exchangers

Interference with structures


When equipment and structure are submitted to a high temperature difference,
it is important doing the following activities:
 Check that relevant lines and expansion joints are free to move in
directions. Be sure shipping stops are removed on the expansion joints if
any
 Check that the platforms and other structures will not interfere with the
free expansion of the equipment in any direction
 Check that instrument piping, electrical conduit and other equipment is in
no danger of binding

Internal Inspection
Drums and vessels will be inspected internally by observation with a light. The
bottom manhole should be left open in case tools or other materials are
accidentally dropped down
 Check that no scaffolding or trash remains in the vessel
 Vessels and tower internals must be inspected carefully and checked
against the design documents to ensure that the installation was
properly carried out. This check should include:
 Trays: number, location, type, spacing, levelness, weir height,
downcomers, valve number and operation, support bolting.
(Tightness testing is usual for chimney trays). Especially check
that all valves on valve type tray are clean and free to move.
 Check that weep holes, where provided, are not plugged.
 Distributors: location, alignment, size and number of openings.
 Vortex breakers: type, size and orientation
 Demisters: size, material and support
 Check that baffles in the bottom of the columns are correctly fitted, type,
orientation and levelness
 Check that instrument nozzles are clear. Check those, which are
accessible from inside the vessel, on the aeration air. Those, which are
accessible only from the outside, will be checked during the air tightness
test that will be implemented prior to inerting by observing that the
instrument vent valve is passing air

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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

For reactors typical internal checks are the following:


 Inlet distributors and quench distributors: metallurgy, type, size, opening
sizes, freedom to expand.
 Vapor/liquid collection and distribution trays: tightness, vertical
positioning, liquid tightness of bubble caps and risers, metallurgy,
dimensions, packing, supports, welding, levelness, cleanliness.
 Catalyst support grids: metallurgy, grid type and dimensions, screen type
and size, supports, welding.
 Catalyst unloading nozzles: metallurgy, orientation, length.
 Thermowells: orientation, length, and metallurgy.
 It must be verified that sufficient quantities of bolts, washers and hold
downs of the proper size and metallurgy are available to reassemble any
disassembled portions of the reactor internals.

Cleaning
All vessels, columns, drums, tanks, etc. have to be inspected and cleaned if
required, before final closure, boxing-up.
The Pre-commissioning team witnesses the final cleaning, especially if the
relevant vessel has been integrated in a cleaning sequence.
If the capacity is used as a buffer capacity, make sure that air is evacuated
from the vessel to lines and not reverse.
When the vessel is used as "collecting device", it must be finally closed only
after cleaning.
Vessel cleaning is normally performed in different ways according to the
equipment materials.
Equipment internal materials are generally the following:
 Carbon steel
 Stainless steel
 Carbon steel lined with different coating material

Accordingly the following cleaning procedure will be applied:

Carbon Steel Equipment


 Carbon steel equipment will be brushed or wiped when required with
brush to remove scale flakes if any, rust, protection oil, etc. before final
closure. After successful inspection, the equipment will be closed
definitely with final gasket.
 During precommissioning phase all activities relevant to piping
connected with such equipment will be done with care in order to avoid
fouling of the equipment (piping cleaning will be done by disconnecting
the piping at the flange connections of equipment and the equipment
nozzles for the first cleanings. Flushing will not be directed into vessels
or columns containing internals).
 Storage tanks must be clean of any corrosion scales or rust flakes and
dust. Depending on the initial condition of these tanks a cleaning by
means of sand blasting may have to be performed. Afterwards these
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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

tanks must be put under nitrogen atmosphere to prevent corrosion (or


dry air if nitrogen is not available).

Stainless Steel Equipment


 Stainless steel equipment will be cleaned by using cloth rag before final
check (wire brush should not be used). After successful inspection, the
equipment will be closed definitely with the final gasket.

Carbon Steel with Lining


 Such equipment will be cleaned by using a water spray, to prevent lining
damages
 For equipment on which internals have to be installed during
precommissioning phase, final inspection will be done after internals
installation

Final Inspection
Vessels final closure (boxing-up) will occur after blowings/flushings are
implemented during the precommissioning phase. Therefore, a vessel may be
required, after a first inspection for conformity against design and drawings, to
be closed temporarily by the precommissioning group until final inspection.
After blowing/flushing (if required), cleaning and dryout, a final vessel
inspection should be done.
Carefully inspect for cleanliness. After a positive final inspection result, vessel
shall be immediately closed, and a "Final Box Up Certificate" will be signed

1.1.2. Pumps

1.1.2.1. Initial Checking


The most critical period in the life of a pump is during its initial start and for
several minutes immediately thereafter. Proper installation and start-up is
essential for trouble free performance. Before the equipment is ever
started it should be checked as follows:
1.1.2.1.1. Review carefully the manufacturer's operating instructions.
1.1.2.1.2. Check that the overall installation is complete.
1.1.2.1.3. Verify that the pump and driver are properly aligned.
1.1.2.1.4. Verify that cooling water piping is connected and in service where
required: pedestals, bearing jackets, stuffing boxes, etc. Run cooling
water through bearing housing, stuffing boxes, etc, until flushed clear.
1.1.2.1.5. Check gland or seal oil piping. Conventionally packed pumps in hot
service are generally furnished with gland oil. When a pump is
furnished with mechanical seals, verify that all components of the
flushing system such as strainers, separators, restriction orifices and
coolers have been correctly installed and are clean. It is very
important that the flush system be clean as the loss or dirty flush can
cause the loss of seals.
1.1.2.1.6. Verify that bearing shafts are clean and properly lubricated. All
bearings should be flushed clean and the correct lubricant in the

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CCR UNIT KRCIM 71200.04 REV.0

proper quantity must be provided. Records for type of lubricant used


and date of lubrication follow up will be recorded.

1.1.2.1.7. Temporary strainers are provided for the suction of each pump to be
installed on the pump side of the suction block valves. These
strainers should be installed after the suction lines are flushed. These
should be cleaned frequently to keep lines free of foreign matter. The
strainers should be cleaned frequently by alternating pumps where
possible. Except on severe services, which may require installation of
fine mesh on both pumps A and B, it is normally sufficient to equip
only one pump with fine mesh (on all "A" pumps for instance).
Consequently, "A" pumps will be the ones preferentially started
during initial startup.
1.1.2.1.8. Then when temporary strainers are not anymore required they should
be removed and only the permanent strainer installed to prevent
further possible pump damage
1.1.2.1.9. Pumps are not field hydrostatically tested.

1.1.2.2. Running Tests


1.1.2.2.1. When piping systems are sufficiently complete (the system or sub-
system can be released from construction activity to
precommissioning and commissioning activity for dynamic
operations) some pumps will be put into operation to determine
whether they are in good mechanical condition and to verify proper
installation of support systems and test running. Keep in mind that
medium other than the design fluid is not always possible.
1.1.2.2.2. Typical example is the case for LPG pumps when use of water leads
to adverse effect that may damage mechanical seals and introduce
water in the system where drastic drying is being implemented before
start-up.
1.1.2.2.3. The circulating fluid for test running a pump, when applicable, is often
water. Due to differences in specific gravity between water and the
design fluid care must be taken not to overload the motors on motor
driven pumps. The amperage on motor driven centrifugal pumps
should be monitored. If the amount of current drawn is too high the
discharge valve should be throttled until the amperage drawn by the
motor is acceptable, keeping in mind that the pump minimum flow
should always be achieved.
1.1.2.2.4. Running test of pumps will be done when applicable only. The
precommissioning/ commissioning group will do the selection of the
pumps subject to running test with water.

The following steps should be adhered to when test running a centrifugal


pump:
1.1.2.2.5. Operating personnel should be familiar with the literature furnished
by pump and driver manufacturers and should follow any special
instructions therein.
1.1.2.2.6. Open up the suction valve from source.
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CCR UNIT KRCIM 71200.04 REV.0

1.1.2.2.7. Check that the seal does not leak (if packed seal check that packing
nuts are not too slack) and that the seal flushing and cooling water
connections are correctly made.
1.1.2.2.8. Rotate centrifugal pump shaft by hand to test for free rotation but
never if the starter switch is not locked.
1.1.2.2.9. Confirm that the alignment check has been made on the pump shaft,
driver shaft and coupling.
1.1.2.2.10. Check that the coupling guard is secured over shaft.
1.1.2.2.11. Check that the grounding clip and wire is secured from motor to
grounding point.
1.1.2.2.12. Check that a discharge pressure gauge is installed and functioning.
1.1.2.2.13. Check that the electrician has tacked the pump power supply in
substation.
1.1.2.2.14. Check that if a pump is on a closed recirculation loop from a vessel,
the vessel is vented to atmosphere to prevent any possibility of
damage by pulling vacuum. A specific procedure will be issued with
marked down PID's for pump running with water prior to actual
start-up.
1.1.2.2.15. When a run with water has been planned the loop system should
be carefully isolated from the rest of the sections. The water make-
up should be sufficient to fill the whole loop and still leave a good
head available to the pumps.
1.1.2.2.16. Check arrangements to vent the pump for priming, if the pump is
not self venting.
1.1.2.2.17. Verify that special connections such as bleeds and drains are
properly installed.
1.1.2.2.18. Strainers must be installed before aligning pumps. A strainer is
provided for each pump suction line during start-up. To avoid pump
damage during flushing with water the strainers may be lined
temporarily with 20 mesh screens or as specified by the pump
manufacturer. Remove this temporary screen after water flushing is
completed and fit the permanent one.
1.1.2.2.19. To prevent equipment damage multistage centrifugal pumps in light
product service (specific gravity less than about 0.8) should not be
running with water.
1.1.2.2.20. All valves in the loop should be opened except for control valves
(manually closed from the control room) and the discharge valve of
the pumps. The operator at the control panel should then be
informed that the system is ready for operation.
1.1.2.2.21. If possible do not start the motor on a centrifugal pump with the
discharge valve open as this also throws an excessive load on the
motor (except if specified to start with fully open valve as auto start
cases).
1.1.2.2.22. When a hot pump is being kept hot by circulation of a stream
through it from an adjacent pump, the shaft of the motor may be
turning slowly in the direction opposite to normal rotation. If a pump
is running in this manner and is started up, an excessive load is
thrown on the motor. Therefore, if a standby pump is already slowly
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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

rotating, cut off or reduce the circulation before starting up. As a


general rule, do not start-up and shutdown any motor more
frequently than necessary since this could cause damage to the
motor rotor, especially for high horsepower motors (not more than 3
starts per hour for medium or high voltage motors are
recommended).
1.1.2.2.23. The board operator should be on duty and coordinate the start of
the pump.
1.1.2.2.24. Ensure the pump is full of liquid after proper casing venting. The
pump can now be started. Crack opens the discharge valve and
switch on. The pump will come up to speed. The discharge
pressure gage should be checked immediately.
1.1.2.2.25. If no pressure is shown the pump should be stopped to find the
cause. If discharge pressure is satisfactory, the discharge valve
should be opened slowly to give the desired flowrate. From then,
the operation should be controlled from the control room. The pump
should not be run with the discharge block valve closed. Note any
vibration or abnormal running condition.
1.1.2.2.26. The field operator should check for leaks in the system, overall
pump performance and pump overload.
1.1.2.2.27. The bearings of pumps and drivers should be checked for signs of
heating. All oil levels should be rechecked and the stuffing box
should be checked for heating.
1.1.2.2.28. The packing gland (for non-mechanical seal type pumps) should be
loosened or tightened as required. It is desirable to allow
considerable leakage in the stuffing box at the beginning to permit
packing to run in. Heating of pump casing may be attributed to
internal rubbing.
1.1.2.2.29. The pump should be run for approximately 1 hour, then shut off to
make any adjustment necessary and to check parts for tightness.
Since it is not possible to run the pump at operating temperature, a
final check could be made during normal operating by switching to
spare pump.

The following steps should be adhered to when test running a


reciprocating pump or a Dosing Pump:
1.1.2.2.30. Check all previous points for centrifugal pumps except hand
rotation.
1.1.2.2.31. Check that the correct relief valve has been installed relieving from
the discharge line to the suction line.
1.1.2.2.32. Check that the manually adjustable stroke control is lubricated and
moving freely.
1.1.2.2.33. Check that the normal operating level of oil is shown in the sight
glass.
1.1.2.2.34. Fully open the discharge valve.
1.1.2.2.35. Switch the reciprocating pump on and off, observe the stroke and
listen for any loud rubbing noises.

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CCR UNIT KRCIM 71200.04 REV.0

1.1.2.2.36. All pumps should be watched closely during preliminary circulation


and particularly when first started. When bearings or packing boxes
begin to overheat (usually this means hot to the touch) or other
indications of trouble appear shutdown immediately for inspection.
Keep a record of pump running time, strainer inspections and
condition, and final removal of the strainer.
1.1.2.2.37. Never run a reciprocating pump with a closed discharge

1.1.3. Compressors And Turbines Drivers


1.1.3.1. Detailed operating instructions for the compressor and turbine driver are
furnished by the manufacturer. Initial starting and breaking in of the
machine should normally be under the supervision of the manufacturer's
representative (only for first start-up).
1.1.3.2. The manufacturer's representative will precheck the compressor, driver
and lube and seal oil (centrifugal compressors) system prior to initial
machine run-in. Some of the items covered are (but not limited to):
1.1.3.3. Checking compressor driver alignment.
1.1.3.4. Checking for proper base grouting and equipment support.
1.1.3.5. Removing flushing oils from bearings and seals.
1.1.3.6. Checking all seal bearing clearances (done previously when fitting).
1.1.3.7. Checking suction and discharge piping for proper vibrational support.
1.1.3.8. Flushing of lube oil, seal and hydraulic oil networks.
1.1.3.9. Adjusting centrifugal compressor seal oil system for smooth operation,
including alarms and functional test of trips (witnessed by
precommissioning team).
1.1.3.10. Installing of orifices in the sour oil trap and oil receiver purge lines.
1.1.3.11. Running in main and auxiliary lube and seal oil pumps. Establishing
normal oil levels in all tube and seal oil systems.
1.1.3.12. Once the precheck is completed, the compressor and driver should be
ready for operation. Since these machines are important and expensive
pieces of process equipment, their proper operation cannot be
underestimated. Manufacturer's recommendations should be consulted
for a more thorough discussion of any item mentioned here.

1.1.4. Air Coolers/Condensers Fans


1.1.4.1. After the motors have been run uncoupled, a static check must be
implemented prior to run the fan.
1.1.4.2. Confirm that the electrical discipline has test-run the motors uncoupled
prior to asking for operational acceptance. Then make the following
checks:
1.1.4.3. Check the electrical report for the motor amperage.
1.1.4.4. Check that the protection grease has been removed and is replaced by
the correct grease Check that the belts are all on the pulley.
1.1.4.5. Check that all debris has been removed from the air-coolers area.
1.1.4.6. Check that there is no loose or live electrical wiring.
1.1.4.7. Check that all air fan platform grating is in place and secured.
1.1.4.8. Check that all stop and start switches are fully installed.

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CCR UNIT KRCIM 71200.04 REV.0

1.1.4.9. Check that the correct motor oil has been put in and the storage protection
(light) oil removed if any.
1.1.4.10. Check the fan motor for proper rotation and grounding (never when the
motor is energized)
1.1.4.11. Set the fan blade pitch as per manufacturer's specification. Once the fan
is in operation, if motor amperage is too high or too low, pitch
readjustment may be required.
1.1.4.12. Set the vibration shutdown switches to give the permitted safe vibration
level
1.1.4.13. If the fan is belt driven adjust the drive belts for proper tension and check
belt condition. Confirm that the fan safety shields are in place.
1.1.4.14. Remove protection plywood that may have been laid on the tubes.
1.1.4.15. Check operation of louvers (if any).
1.1.4.16. When all above checks have been made, proceed to a 4 hours (except
otherwise agreed duration) test run and check the following points:
1.1.4.17. Check that the amperage of the motors is in the normal range.
1.1.4.18. Check for any noise from the bearings or other.
1.1.4.19. Check for any screeching or abnormal noises from the pulleys (belts
may be too tight, which will affect bearings).
1.1.4.20. Check that all belts remain on the pulleys (belts that constantly come off
could indicate offset pulley).
1.1.4.21. Check that air fan blades are not making any abnormal noise.
1.1.4.22. Check that air fans on the same cell are all turning at approximately the
same speed
1.1.4.23. Stop the air fans one by one and stand underneath to observe and
check the following:
1.1.4.24. Check that no abnormal noise occurs on the rundown.
1.1.4.25. Check that the air fans slowly come to a stop in a smooth manner.
1.1.4.26. Check by hand that the motor has not overheated.
1.1.4.27. If the motor is inside the safety screen cover and if motor overheating is
suspected or another intervention on the fan is required never remove
the safety screen by yourself.
1.1.4.28. Inform the Electrical Specialist which will follow the normal safety
procedure of electrical isolation in the substation by tagging off and
locking shut the electrical breaker for the motors.
1.1.4.29. Complete the run-in before using the air cooler condenser for any heat
transfer duty.

1.1.5. Fired Heaters


Inspection and checking of the following main points has to be carried out
before refractory drying.

Instrumentation
1.1.5.1. Controllers, regulators, and recorders for flows, pressures and
temperatures: correct zero adjustment or designed values, normal
position, connections.
1.1.5.2. Thermocouples: length, location, and correct connection of cables.
1.1.5.3. Connections for controls (pressures, temperatures) and sampling.
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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

1.1.5.4. When not being used, connections should be closed off with threaded
plugs or blind flanges.
1.1.5.5. Carry out tests on all instruments that are part of the safety control
system.
1.1.5.6. Ensure that the necessary checking of the burners control system has
been performed.
1.1.5.7. Ensure that minimum stop positions have been set up on fuel gas and
combustion air systems (if any).

Stack Damper
1.1.5.8. The full-open and the minimum opening position of the damper should be
checked visually. The movement of the damper must be free and
unobstructed. Incorrect positioning will materially affect furnace operation
and may result in a great deal of difficulty in firing at higher rates.
1.1.5.9. Check the pneumatic actuator controls for proper operation (if any).

1.2. Instrumentation Preparation

1.2.1. Commissioning of instruments will be carried out as the plant comes on stream.
Most attention will be directed towards liquid flow measurements: differential
pressure instrument piping must be drained to eliminate accumulated dirt and
water and the instrument zero must be adjusted to obtain a correct zero reading
on the scale on the control board instrument. Controllers must be tuned;
interface level transmitters must be zero checked; scale, weld slag and trash
must be removed from stricking control valves; other malfunctions must be
corrected. Inspection and commissioning of analyzers should include attention
to sample line lengths, analyzer enclosures, auxiliary equipment, such as
carrier gas for chromatography and other items as indicated in the instruction
manual for the particular analyzer.
1.2.2. Analyzers should be inspected, calibrated and commissioned in accordance
with procedures and instructions in the instruction manual for the analyzer. An
instrumentation engineer has to review installation and supervise calibration
and initial start-up. A vendor representative might be required for some specific
analyzers.
1.2.3. Chromatographs should be inspected to make sure that all external piping and
wiring are complete and that no parts have been lost or damaged in shipment.
1.2.4. Functional test for instrument loops have to be done prior to start-up to ensure
correct
1.2.5. operation of safety devices. ESD system interlocks and local/remote actions.
1.2.6. Proceed to the following checking. First, before energizing field instrumentation
and proceed to energized loop checks, confirm that the following static checks
are actually
1.2.7. implemented:
1.2.8. Clean air lines before connecting to instruments
1.2.9. Clean the instrument air supply headers by blowing with clean, dry air, and
check them for leak tightness.
1.2.10. Verify that pneumatic tubing is hooked up, that instrument air is available at
the instrument.
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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

1.2.11. Check piping from instruments to process piping and equipment for leak
tightness.
1.2.12. Isolate or remove in line components such as control valves, positive
displacement meters and turbine meters for pressure and leak testing if
specified tight shut off (already done in workshop normally.)
1.2.13. Reinstall these items after successful testing of the system.
1.2.14. Check orifice plate bore diameters versus documents.
1.2.15. Install orifice plates after completion of testing, draining, flushing and cleaning
of lines.
1.2.16. Isolate or remove inline components for flushing and cleaning operations.
Reinstall and/or reconnect after completion of cleaning and flushing
operations.
1.2.17. Verify correct positions and installation of inline instrumentation (control valve
flow direction and fall position, orifice plate installed in correct relation to flow
etc).
1.2.18. Perform all non-operating tests that ensure instrument operability: remove
shipping stops, check pointer travel, verify and adjust the instrument's
capability to measure, operate, stroke etc., in the direction and manner
required by the process application (direct or reverse controllers etc).
1.2.19. Perform functional loop checks and demonstrate correct operation (a
precommissioning record sheet with the relevant loop diagram).
1.2.20. Fully pressurize and energize the transmitting and control signal systems by
opening process connections at primary sensors and regulators and by
making control mode settings for automatic operation of equipment as the
process unit is charged and brought on stream.
1.2.21. On the DCS check operability of the system and interfaces to other
subsystems.
1.2.22. Thermocouple wiring should be inspected for proper polaring at the
thermocouple head. Point-by-point verification or the switch identification at
the temperature indicator on the operator's board can be accomplished by
selecting a point to be checked, opening the circuit at the thermocouple head
and checking the temperature indicator to see if it drives upscale or otherwise
indicates an open circuit. The same applies for temperature recorder
controller instruments on the control board. Loop checking involves checking
inputs and should be simulated at the transmitter and the control board
instrument should be watched for response. The controller output should be
adjusted manually and the control valve watched for response. Special
attention should be given to split-range loops and complicated systems
(machinery/DCS interface, etc).

1.3. Heating, Ventilation Air Conditioning Equipment

1.3.1. Verify conformity of the installation with drawings, specifications, safety rules,
supplier instructions.
1.3.2. Verify the free rotation of fans and motors.
1.3.3. Verify the correct installation of anti-vibrations mountings and sealing
compound of fire dampers, if any.
1.3.4. Verify that leakage and blades of dampers run freely.
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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

1.3.5. Verify that dampers actuators are in good running order.


1.3.6. Verify that air flow direction in preheater is correct.
1.3.7. Perform ductwork leak tests.
1.3.8. Start the unit test sequences, interlocks, vibrations.
1.3.9. Start air flow and make balancing test (air distribution adjustment).
1.3.10. Adjust room's temperature and pressurization.

1.4. Telecommunications
1.4.1. Inspection of all telecommunication equipments is performed to ensure
compliance with specifications, drawings, Codes of Practice, regulations and
manufacturer's particular requirements. In general, inspections should ensure
satisfactory jointing and continuity of all conductors, satisfactory alignment and
tightness of bolting, acceptance levels of insulation, and a high standard of
cleanliness.
1.4.2. Main telecommunication systems are:
 Message switch system
 Radio communication system
 Telephone network.

2. Cleaning Of Piping And Equipment


2.1. General
2.1.1. Lines and equipment cleaning is intended to eliminate welds rods and slags,
abrasive dusts, oxides and in general other substances which might impede the
normal unit operation or damage the equipment (valves, pumps, compressors,
turbines, etc.)
2.1.2. Cleaning is usually carried out either by hand cleaning for large equipment and
lines having a diameter higher than (or equal to) 24", by water flushing, by air
blowing, chemical cleaning or any other cleaning method as described
hereafter.
2.1.3. ln accessible piping (in terms of impossibility to access inside for hand
cleaning) will be cleaned using fire water or any other hydraulic or power
flushing, or by air or steam blowing including lines to and from storage. When
an exchanger is included in a cleaning circuit, the inlet line is first disconnected
and the piping connect to it cleaned. After sufficient cleaning the exchanger
must be reconnected for washing the outlet piping.
2.1.4. It must be noticed that this is not always possible, as some lines between
exchangers are impossible to disconnect without complete removal of the line.
In such case, the identified line has been subject to joint inspection between the
construction team and precommissioning group, after or before hydrotest
inspection (drainage of the hydrotest medium) to confirm the line is sufficiently
clean for final installation.
2.1.5. For the circuits which are not equipped with a pump, a fire hose or a capacity
(used as a reservoir) may be used for washing or as buffer capacity for air
blowing.
2.1.6. Flush the pumps suction line through the strainer door/flange.
2.1.7. When the initial washing is completed, reconnect the suction piping of the
pumps and continue the washing of the Iines during the running-in of the pump
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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

(if applicable) until no more collected fragments In the strainers at the pump
suction.
2.1.8. Even if water flushing method would be foreseen, it is impossible to have the
proper and required velocity to clean lines over a certain size with water,
without unreasonably sized temporary facilities (process pumps do not allow
such flows).
2.1.9. The cleaning of lines and associated equipment, which forms the various
systems to be mechanically completed and made ready for start-up, will be
treated during the construction and precommissioning phases in two steps:
(1) During the construction phase, preliminary pipes protection and checking is
implemented to avoid pipelines retaining construction materials until the actual
cleaning takes place when practically feasibly and applicable with the required
efficiency.
(2) Then to reach the readiness for start-up, a cleaning is implemented for each
system/subsystem. This cleaning will use efficient methods, which could be
implemented only after part of the plant is available.
As a summary, only step 1 above can be implemented at the hydraulic test
stage of the work. The cleaning at step 2 of course will be performed as soon
as the site facilities allow for it, the optimum being that both are implemented in
sequence.
2.1.10. To make easier the understanding, the sequence of events, the cleaning
steps that will be applied are the following:
 The prefabricated piping spools will be transferred to the site for
installation duly protected at all open ends with plastic
caps/wrapping.They will be visually checked for any foreign material as
tools, gloves, etc, which will be removed.
 For big lines, construction group carries out inspection after each spool is
welded, and a manual rubbing/wiping is performed, if necessary.
 After the hydrotest, the hydrotesting medium (mainly water) is drained,
through drain valves or one open flange at the maximum rate, so that dirt
is as much as possible removed.
 When a system or part of the hydrotested system (so called Test Pack) is
released, a provisional reinstatement is implemented. This is with
exceptions list agreed by precommissioning group and construction to
allow the use of permanent facilities (columns/vessels/pipes themselves)
to perform the actual cleaning to meet the precommissioning cleanliness
requirement.
 Some of this cleanings may need the utilities, (such as instrument air,
utility air, service water, etc.). In this case of course utilities should have
been precommissioned before with the normal required checks.
 Above step is the period of time where the unit is actually cleaned and is
followed by final reinstatement and conformity to PID checks, air tightness
test, etc.

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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

2.2. Water Flushing


2.2.1. Water flushing will be performed using clean water.
2.2.2. Brackish or salt water must not be used for flushing of systems containing
stainless steel parts. In these cases demineralized water or condensate should
be used.
2.2.3. When stainless steel lines are flushed, it is important to rinse properly with
demineralized water. Therefore it may happen that some lines are flushed with
utility water and then, over a short time, rinsed with demineralized water:
2.2.4. The following guidelines should be observed for flushing operations:
 All possible lines should be used during the flushing operation to
facilitate complete system cleanout (main headers first, then
subheaders).
 Temporary strainers are to be installed in the suction lines of all pumps
before any liquid is allowed to pass through them from newly constructed
lines. If this is not done, scale, weld metal or slag, stones etc, may
freeze or damage centrifugal pump impellers. The screens serve to trap
such dirt in a place where it can be conveniently removed.
 When possible, main and spare pumps can be run at the same time and
used to circulate water for the purpose of removing dirt and scale via the
pump suction strainers.
 When practical, lines should always be flushed away from a vessel
rather than into a vessel. Any vessel that has been flushed or blown into
should be opened and manually cleaned following flushing.
 Flushing should be preferentially from the highest elevation to the lowest
elevation. This restrain is not compulsory for blowing
 Vessels and systems should be vented when filling or emptying to
prevent vacuum pulling.
 During flushing, maximum volume and velocity should be used to ensure
thorough cleaning, the rate of flushing medium should be regulated at
the source.
 Control valves should be rolled out of the piping system during flushing
to prevent damage, except some butterfly valves that can remain
installed if wide open.
 Orifice plates should be installed after cleaning is completed.
 Instruments (i.e. pressure gages and transmitters, differential flow meter
transmitters, moisture and other in-line analyzers, etc.) should be
positively isolated from the system during cleaning.
 All drains should be flushed through to check for blockage. .
 Where possible, open-end lines should be flushed through. This is the
case of process units provided with end flanges for all utilities lines which
make easier either flushing/air blowing steam blowing. Flow should not
be restricted drastically.
 Pump suction and discharge lines should be flushed while protecting the
pump casing (by flushing through the open strainer or a metal plate at
pump flange).
 Lines should be flushed in the following sequences, where possible:
 first the main header, then each sub-header, at last, each branch line.
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PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

 Always flush through a by pass when it exists, to an open end before


flushing through equipment.
 Lines should not be flushed into exchangers without flushing at the inlet
first. Only when the inlet is checked clean, and when the exchangers is
not equipped with a bypass, flushing is allowed to pass through the
exchangers if required to proceed further.
 Flushing should continue in each line or piece of equipment until the
water is reasonably clean (or as clear as the make-up water).
2.2.5. Unit Piping and instruments Diagrams should be used as a cleaning check off
record to ensure that lines are flushed cleaned including lines to and from
tankage.
2.2.6. After completion of the flushing operations, the water should be kept in the unit
to facilitate pump run-in if this was not done during the flushing operation and if
run-in of pumps with water is applicable. If pump run-in has been completed or
will not follow the flushing operation immediately, all water should be drained
from the unit. If necessary, break flanges at low points to facilitate drainage and
airblow as required removing as much water as possible.
2.2.7. It is essential that a flushing path is defined in an agreed procedure and it is
adhered by all personnel in charge to perform the operation in the field. The list
of breakpoints should be made known to the construction group as early as
possible to avoid putting final gaskets in place of temporary gaskets and also to
have the required amount of correctly rated and sized gaskets in the hands of
the precommissioning team.
2.2.8. The wall charts should be kept up to date and the final gaskets should add up
to the same amount as the temporary gaskets received (ideal situation).
2.2.9. Close follow-up eliminates problems during start-up and identical procedures
can be used in removing all temporary blinds after the completion of the
hydrostatic test. A color code system can be very useful at this stage (for
flanges equipped with temporary gaskets).

2.3. Air Blowing


2.3.1. Cleaning of circuits will be carried out by air blowing for lines and pieces of
equipment which have to be kept free from water and for some big piping (due
to unacceptable weight. or too large quantity of water required or water flushing
not efficient).
2.3.2. By experience, the air blowing method is usually also extended and applicable
to lines, as this leads to good results and dry conditions are obtained rapidly.
2.3.3. Air blowing will be carried out with compressed air. Air blowing of a circuit
should be performed by using temporary connection with compressed air
network, in a continuous manner for small lines or by using vessels (drum,
column, etc.,) as holdupIbuffer capacity to get a quick air release. The vessel
will be pressurized with compressed air, then the air will be released through
the circuit (of course first, check that design pressure of the vessels is in
accordance with compressed air maximum operating pressure). This design
pressure is reminded in the specific procedure to be applied to each system.
2.3.4. In some huge systems, it is sometimes not possible to use valves to blow the
relevant lines. In this case, a bursting disc (made of cardboard or aluminium

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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

sheet) can be used to proceed to a sudden depressurization (ensure that no


equipment may be damaged).
2.3.5. This will be the case for some lines in the process unit and interconnecting
mainly.
2.3.6. Piping system blowing will be considered completed when air at the exit point
will appear clear. (The air has not to be orange dust color).

2.4. Steam Blowing


Cleaning by steam blowing is carried out essentially for steam circuits. Due to
problems of expansion or draining of condensate, this type of cleaning has to be
used with the utmost care.
Steam blowing will be carried out as follows:
2.4.1. Before putting steam into the system, control valves, turbine meters,
instruments, vacuum ejector, and strainers should be removed or blinded off.
The steam headers should be slowly warned up, one header at a time, while
expansion of the line is observed. Special attention should be given to pipe
support shoes.
2.4.2. Condensate must be drained manually to prevent steam hammering. The
headers should now be blown using a low pressure, high-velocity sweep as
explained hereafter.
2.4.3. When the headers are warm, the drain valves should be opened, blown
vigorously for a few moments before reclosing. Each lateral to header,
exchangers, or service lines should be blown in the same manner, usually not
more than one at a time. Condensate lines may be cleaned in the same
manner as steam lines, but close.observation of the pressure on the
condensate line is necessary since the working pressure and temperature of
the condensate lines are generally lower than of the steam headers. A
temporary movable silencer could be used to avoid exceeding noise level
limitations during the steam blowing operation, if necessary. Nevertheless, this
minimizes the efficiency of the steam blowing and steam blowing without
silencer is preferable. (Coordination with people working in the vicinity is
required).
2.4.4. When blowdown of the steam system is completed, equipment that were
removed prior to the blowdown can be reconnected. The system can then be
preheated and placed in service, after it has passed the steam test.

2.4.5. Completion and effectiveness of steam blowing will be determined as follows:


Steam piping at inlet of turbine, desuperheater and outlet of boiler.
 An aluminum target located at the vent point will be observed.
 Blowing of this piping system will be considered completed and cleaned
when on two consecutive targets, collected after blowing is carried out as
above described, are present less than two pits per square cm with a
maximum diameter of 0.3 mm.
 This is given as a guideline, and digression can be admitted for boilers
outlet.

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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

 Targets made from aluminum sheet will be inserted, on temporary vent only
after that three-four blowings (depending on the experience on site) have
been carried out and the steam appears to be clean.
Other steam piping and steam piping to turbine less than 4"
 Piping system blowing will be considered completed when steam at the exit
of vent point will appear clean. (The steam has not to be orange dust color).
 When blow down of the steam system is completed, traps and other
equipment that were removed prior to the blowdown may be reconnected.
The system can then be reheated and placed in service, after it has passed
the steam test.

2.5. Chemical Cleaning


2.5.1. Chemical cleaning of piping is required when either the product can react with
oil left inside of the piping or in case even very small parts of debris inside the
piping can lead to adverse effect.
2.5.2. This is normally limited to machinery lube oil pipework, before final installation,
and only in case some weldings are done on site.
2.5.3. Other pipework spools (as compressors suction spools), are mechanically
brushed/cleaned before installation.
2.5.4. Proper neutralizing and flushing of these systems after the chemical attack are
of utmost importance.
2.5.5. Typical chemical cleaning procedure is described here below. In case
specialized companies are used for chemical cleaning, their procedures shall
apply.

2.6. Cleaning And Pickling Of Piping


2.6.1. Solution Preparation, Handling and Use
All solutions shall be prepared, handled and used in strict accordance with the
manufacturer's instructions and this specification.
Chemical solutions shall not be introduced into piping systems or equipment
unless high point vents and low point drains are available to ensure proper
filling and complete removal of solutions.
2.6.2. Detergent Cleaning
 All oil, grease, soil, drawing compounds and foreign matter other than
rust, scale, and oxides shall be removed by detergent cleaning as
follows:
 The piping system shall be force flushed with water to remove non
adherent foreign matter and reduce the load on the detergent. Flushing
shall be continued until all such foreign matter is removed.
 Detergent cleaning shall include the removal of oil, grease, soil, drawing
compounds, and foreign matter other than rust and scale. Detergent
solution shall be circulated through the pipe at the temperature,
concentration, and flow rate recommended by the detergent
manufacturer.
 When detergent flow rate has not been recommended by the
manufacturer, the flow rate shall be 1.5 meter per second.

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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

 Surfaces cleaned with detergent must be thoroughly rinsed by warm,


fresh water to remove residues of detergent. To test the effectiveness of
rinse, universal pH test paper shall be placed against the wet steel. The
pH of the rinsed surface should be no greater than the pH of the rinse
water.
2.6.3. Acid Cleaning
 All oil, grease, and soils shall be removed by detergent cleaning. All rust,
scale and oxides shall be removed (to leave bare metal) by citric acid
cleaning as follows:
 Citric acid solution shall be circulated at the temperature, concentration
and flow rate recommended by manufacturer.
 Unless otherwise recommended by manufacturer, solution temperature
shall be maintained between 80°C and 95°C throughout the system
during this operation by injecting steam into the acid solution.
 The concentration of citric acid in the cleaning solution shall be
monitored and replenished in accordance with the manufacturer's
instructions. Samples shall be taken periodically and titrated to test for
acid and iron content. Cleaning shall be considered complete when acid
concentration and iron content are constant for one hour.
 When chemical tests indicate a constant ferric and ferrous ion
concentration, the used citric acid solution shall be displaced by rinse
water containing 0.05 percent to 0.10 percent citric acid solution to
ensure all traces of soluble ion are removed. This method of displacing
spent cleaning solution with rinse water shall be used in lieu of draining
the spent acid solution and refilling with rinse water. Circulation of rinse
water shall be maintained at least 10 minutes.
 Immediately following rinse water circulation, 1.0 percent soda ash
solution shall be circulated at 80°C for at least 10 minutes to neutralize
the cleaned surfaces. The pH of used soda ash solution shall be at least
9.5, in order to stop circulation.
 After the surfaces are clean and dry, the pipe shall be filled with nitrogen
and sealed. The nitrogen pressure shall be 0.1 to 0.2 kg/cm2g.
2.6.4. Chemical Solution and Rinse Disposal
All spent chemical solutions and rinses will be disposed to sewer, using water
for dilution.

2.7. Inspection Of Cleaned Surfaces


2.7.1. Cleaned surfaces shall be visually examined. Visual examination shall be
supplemented with borescopes, mirrors, and other aids as necessary, to
properly examine inaccessible or difficult-to-see surfaces. Lights shall be
positioned to prevent glare on the surfaces being examined.
2.7.2. Where visual examination is not practical, a clean, lint free, white cotton cloth or
filter paper moistened (but not saturated) with high purity isopropyl alcohol
(rubbing alcohol) may be rubbed against the surfaces at all openings. The
presence of a smudge on the cloth or filter paper is evidence of incomplete
cleaning and the cleaning shall be repeated.

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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

2.8. Inspection Of Other Surfaces


The internal surfaces of all piping systems shall be visually inspected to verify that all
surfaces are entirely free of weld slag, flux, soil, debris, grease, oil and any foreign
matter.

2.9. Identification Of Cleaned Pipe (Typical)


Cleaned pipe shall be metal tagged to avoid subsequent contamination. Tag shall
read similar to this: 'KEEP SEALED UNTIL USE. INTERNALLY CLEANED (AND
PRESSURIZED)ON (Date)
Pipe shall not be marked with paint or ink, in lieu of metal tagging, unless the pipe is
finish painted or insulated.

2.10. Storage or Installation of Chemically Cleaned Pipework


2.10.1. Usually, chemical cleaning is implemented just before installation.
2.10.2. The following good sense advice shall be followed to avoid corrosion that may
inhibit the work done.
 The piping should preferably be installed immediately, but if this is
impracticable then immediate steps must be taken to prevent rusting.
Generally, a dip or spray coating of light mineral oil will suffice for
storage of less than one month, but if piping is to be placed in outdoor
storage for more than one month, a coating of rust preventive should be
used.
 Unless piping is going to be installed immediately, suitable closures must
be placed on the ends and all openings to prevent entrance of moisture
or dirt. Use of steel plate discs and thick gaskets is recommended for all
flanges. Before applying closures, the flange surfaces should be coated
with grease.
 Before installation, check that no dirt or foreign matter has entered piping
and that rusting has not occurred. If in good condition, then pull through
a swab saturated with carbon tetrachloride. The piping shall not be
bolted up until inspected for cleanliness.

2.11. Safety Consideration


2.11.1. All activities connected with chemical cleaning must be supervised by
qualified staff in order to assure attainment of the required pickling effect and
to prevent damage to materials and/or to health.
2.11.2. Protective gloves, protective boots and aprons in correspondingly acid-
resistant material and tightly sealing protective goggles must be worn for all
work involving acids. Acids must always be stirred carefully in a thin stream of
water, never the reverse.

2.12. Lubrication Systems Flushing


Necessary instructions for cleaning the lubricant and seal oil piping systems are
given in manufacturer's data books. They have to be strictly followed to proceed with
the cleaning of such piping systems.
Typically, lubricant oil piping system for machinery can be cleaned as follows.

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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

2.12.1. Preliminary Air Blowing


The piping system will be blown with air in order to remove all dirt, debris.
Blowing will be accomplished with hammering of piping for removal of mill
scales. Air blowing will also remove water or moisture present into the piping
system.
2.12.2. Chemical Cleaning
Oil lines installed in the factory that have been flushed and sealed before
shipment, do not require any additional chemical cleaning before the final oil
flushing. Some other oil interconnecting piping, which have been fabricated at
the erection site, may require chemical cleaning before installation as
specified here below

Cleaning (Or Degreasing) Procedure


Procedure for Carbon Steel
 Immerse the piping in a caustic bath at a temperature of abo t 80/90°
for a period of at least 30 minutes, depending on the condition of the
material to remove all grease, dirt, oil or paint.
 Piping and/or solution are agitated to ensure the flow of solution
through the piping. The batch may be a solution of 6%wt of sodium
hydroxide in water with detergent.
 Remove piping from caustic bath and immediately rinse with cold
water.

Procedure for stainless steel


 Mechanically clean all welds as required and suitably wash with clean
demineralized water to remove dirt.

Pickling Procedure
Pickling is not required for Stainless Steel Piping. The pickling (or chemical
cleaning) of the carbon steel piping which follows cleaning or degreasing may
be carried out by the following recommended procedure.
Procedure for Carbon Steel
 Immerse the piping in an acid pickling bath containing a 10 % wt
solution of hydrochloric (muriatic) acid in water. Rodine, Pyridine or
other suitable inhibitors should be added to the solution in accordance
with the Supplier's instructions to prevent the piping from rusting
quickly when removed from the acid bath.
 Piping and/or solution is agitated to ensure the flow of solution through
the piping.
 The bath temperature should be between 60 and 70°C and the time of
immersion required to remove all scale and rust will depend on the
strength of the solution and condition of the pipe. Normally, 12 to 14
hours are required and 6 hours should be taken as a minimum.
 Remove piping from acid bath, drain it and immediate wash with cold
water to remove all traces of acid.

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KRC REFORMING SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71200.04 REV.0

Neutralizing Procedure
 Without allowing the piping to dry, immerse in a hot neutral solution of
0.75 to 1,5%wt of soda ash in water maintained at a pH value of 9 or
above. The temperature of the bath should be about 70/80°C.
 Piping and/or solution is agitated to ensure the flow of solution through
the piping.
 pH paper may be used to check the wet surface of the piping to
determine than an acidic condition does not exist. If the check shows
acidity then the neutralizing treatment must be repeated.
 Rinse piping with cold water, drain thoroughly and blowout with service
air until dry.

Flushing with Lubricant Oil


 The whole lubrication system for machinery will be assembled as per
design.
 Bearing house, seal, etc., will be by-passed by temporary connections
(i.e. rubber hoses) between inlet and outlet piping.
 Screen mesh will be installed on all flanges between lines (screen with
100 mesh will be used). When such screen will show to be clean (no
presence of dirt, debris or mill scales), a white cotton cloth will be
inserted to finally check the cleanliness of the system. Lubricant oil will
be circulated into the system by using its own lube oil pump and heated
up to 50-70DC, by means of console heater or by a temporary steam
connection to the oil coolers.

2.13. Blinds List


2.13.1. A blind list of permanent spectacle blinds and temporary blinds on the
pipework and/or equipment must always be current during the
precommissioning and commissioning. It is good practice to double check not
only that the list is accurate but that all blinds necessary for the safety of the
unit are in place. Marking the blinds with brightly colored paint or ribbons also
helps to locate installed blinds. .
2.13.2. When commissioning one unit, all blinds on process, fuel gas, closed drain
and flare lines at battery limit should remain closed on other units not in
operation or ready to be placed into operation.
2.13.3. Until the unit to be started-up is inerted, the following lines must remain
positively isolated from the rest of the unit .
2.13.4. Flare lines at battery limit must be blinded and the internal headers open to
atmosphere until nitrogen introduction for inerting, to prevent overpressure of
these headers.
2.13.5. Closed drain system and fuel gas must be blinded at battery limit.
2.13.6. All process lines in and out must be blinded at battery limit.

ISSUE DATE: 20/03/06 - 66 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

Contents: This instruction outlines the procedure for the start-up of the CCR
reforming unit up to the stage where the catalyst is being loaded. The
text includes:

1. Start-Up Requirement
2. Unit Purging
3. Initial Leak Test
4. Unit Dryout
5. Catalyst Loading
6. Second Leak Test And Partial Inerting
7. Supplements

1. Start-Up Requirement
1.1. All overhaul activities and technical modifications influencing Start-up are completed.
All units, removal of equipment and pipeline blinds conform to process requirements.
1.2. Pressure gauges and safety valves are checked. Replacement work and installation
is completed.
1.3. All chemical raw materials are ready and sufficient.
1.4. All process lines and equipment has been purged, qualified in pressure test and
undergone final inspection according to the following procedures.
1.5. Disassembled or replaced equipment flanges are padded and screwed uniformly.
1.6. Safety valves in good condition and its set pressure meet the requirement.
1.7. Close all atmospheric relief valves and drain.
1.8. Verify all instruments are in good condition.
1.9. Utilities services are working normal.
1.10.Ensure complete fire appliances, place inflammables and explosives in fixed area,
clean sundries on site.
1.11.Contact dispatch, maintenance department, fitters, electrical maintenance and lab.
Complete corresponding support work.
1.12.Complete and examine all Start-up schemes, planning diagrams, all related
procedures sheet and work permits.
1.13.All maintained and revamped equipment has acceptance qualification sheet.
1.14.Inspection of the unit is done according to “Plant Inspection” procedure in (KRCIM
71200.04)

2. Unit purging
2.1. Purging Objective
2.1.1. Eliminate welds rods and slags, abrasive dusts, oxides and in general other
substances which might impede the normal unit operation or damage the
equipment (valves, pumps, compressors, turbines, etc.)
2.1.2. Timely find existing problems through process line. Ensure system operability.
2.1.3. Make operators further understand field flow path.

2.2. Preparation Work Before Purging


2.2.1. All equipment and pipelines belonging to this unit should be inspected carefully
according to purging route before purging; any reassembled or newly installed
ISSUE DATE: 20/03/06 - 67 -
KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

equipment should be repositioned completely; any problem found should be


handled in time.
2.2.2. Contact with dispatch to prepare steam and water supply.

2.3. Notices For Purging


2.3.1. Proceed with purging and flushing of the unit according to instructions in
“Cleaning of Equipment and Pipeline” in (KRCIM 71200.04).
2.3.2. Media used for flushing and purging
 Pipeline for handling liquid should be flushed with water; except that
condensed water system uses condensed water for flushing, others use
fire water for flushing.
 Pipeline for handling gas should be flushed with air or nitrogen;
instrument’s pneumatic line should use purified air for purging.
 Steam pipeline should use steam of corresponding pressure level for
purging according to different pressure levels.

2.4. Purging Scheme


2.4.1. C-71201 system purging
The continuous reforming unit uses 1.0MPa steam as purging media. Firstly,
remove the blind plate on 50-LS-712003 line, and purge it to clean, then,
introduce steam into tower system and purge according to following flow:

ISSUE DATE: 20/03/06 - 68 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

→top tower vent


→PG-712101
→PSV-71216A/B uptream flange and downstream bypass valve
→150-P-712063→A-71202→100-P-712065→D-71204→Top Vent and PG2095 discharge steam
→50-P-712066→50-P-712067→PV-2096 bypass→50-P-712068 line 8-shaped blind plate discharges steam
→50-P-712069 line 8-shaped blind plate discharges steam
→150-P-712051→D-71205→ Top vent and PG-2091discharge steam
→PSV-71215A/B downstream flange and upstream bypass valve
→40-P-712057→PV2092 bypass →40-P-712058 line 8-shaped blind plate
discharges steam
→40-P-712059 line 8-shaped blind plate discharges steam
→Bottom drain and slop line 8-shaped blind plate discharges steam
→liquid level gauge discharge steam
→200-P-712052→P-71204A/B inlet drain and filter upstream flange discharge
steam
→50-P-712100 line 8-shaped blind plate discharges steam
→150-P-712044→LV2008 discharges steam
→SN-71207 sampler purging
→25-GN-712010 line 8-shaped blind plate discharges steam
→25-NF-712041→P-71203A/B outlet non-return valves and drain discharge steam
→All liquid level gauges discharge steam
→Bottom drain and slop line8-shaped blind plate discharges steam
→150-P-712070→P-71203A/B inlet drain and filter upstream flange discharge steam
→100-P-712080→FV2020 bypass →100-P-712074→P-71203A/B outlet non-return valves and drain discharge steam
→FT2018→50-P-712078→FV2019 bypass→LPG battery limit line 8-shaped blind plate discharges steam
→SN-71209 sampler purging
→150-P-712060→E-71208D/C shell side drain and slop line8-shaped blind plate discharge steam →E-71208B/A shell side drain and slop line8-shaped blind plate discharge
steam
→ 150-P-712056→FV-2015 bypass →150-P-712054→P-71204A/B outlet non-return valves and drain discharge steam
→50-P-712100 8-shaped blind plate discharges steam
→100-P-712099 →150-P-712020 line 8-shaped blind plate discharges steam
→P-71201A/B outlet non-return valves and drain discharge steam
→SN-71208 sampler discharge steam
→Tower bottom liquid level gauge and PG2108 discharge steam
→ Underground drain and slop line 8-shaped blind plate discharge steam
→300-P-712081→300-P-712082→P-71202A/B inlet filters upstream and drain discharges steam
→100-P-712136→P-71202A/B outlet non-return valves and drain discharge steam →150-P-712084→FV-2022, FV-2023 discharge steam
→E-71208D/C tube side drain and slop line8-shaped blind plate discharge steam →E-71208B/A tube side drain and slop line8-shaped blind plate discharge
steam →150-P-712094 → E-71208A/B shell side drain and slop line8-shaped blind plate discharge steam →
FT-2021 bypass→SN-71210 sampler discharge steam
→FV-2026 bypass→150-P-712096→Reformate battery limit line 8-shaped blind plate discharges steam
→100-P-712096/3 8-shaped blind plate discharges steam
→25-P-712096/1→D-71105→D-71105 top vent
→D-71105 bottom drain line

ISSUE DATE: 20/03/06 - 69 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0
→20-CL-711002→P-71107 inlet drain and filter downstream flange discharge
steam
→D-71105 top overflow line
→D-71105 nitrogen purging line and high-point vent
→25-P-712096/2→ D-71107 →D-71107 top vent and bottom discharge line
→20-CL-712010→P-71206A/B inlet drain and filter downstream flange discharge
steam
→25-CL-711001→P-71106 inlet drain and filter upstream flange discharge
steam
→D-71107 top overflow line
→D-71107 nitrogen purging line and high-point vent
→300-P712090→200-P-712089→F-71205→FV-2022 discharges steam
→200-P-712089/1→F-71205→FV-2023 discharges steam

 C-71201 steam purging blind plate table

No. Specifications Location Tube No. Qty. Status Remarks


1 Dg50 C-71201 bottom steam line LS-712003 1 Open 8-shaped blind plate
2 Dg25 D-71204 top nitrogen line GN-712010 1 Blind 8-shaped blind plate
3 Dg50 D-71204 top to flare header P-712069 1 Blind 8-shaped blind plate
4 Dg50 D-71204 top to fuel gas line P-712068 1 Blind 8-shaped blind plate
5 Dg50 LPG battery limit line P-712079 1 Blind 8-shaped blind plate
6 Dg40 D-71205 top to flare header P-712059 1 Blind 8-shaped blind plate
7 Dg40 D-71205 top to fuel gas line P-712058 1 Blind 8-shaped blind plate
8 Dg150 LV2008 downstream valve P-712044 2 Blind 8-shaped blind plate
and bypass valve
9 Dg150 Reformate battery limit line P-712096 1 Blind 8-shaped blind plate
10 Dg100 Reformate to D-71100 line P-712096/3 1 Blind 8-shaped blind plate
11 Dg50 D-71205 start-up inlet line P-712100 1 Blind 8-shaped blind plate
12 Dg100 P-71204 outlet start-up line P-712099 1 Blind 8-shaped blind plate

ISSUE DATE: 20/03/06 - 70 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

2.4.2. Purging scheme of recontacting system


During purging of recontact system, the media used is 2.5MPa nitrogen; purging is done after blowing-up purging of K-71202A/B
outlets pipeline; first, install the non-return valve before the hydrogen mixing point well, close K-71202A/B 2nd stage outlets valve,
then, introduce 2.5MPa nitrogen into K-71202A/B 2nd stage outlet line and purge according to following flow:

Nitrogen from 25-GN-712007→25-GN-712007/1→200-P-712039→150-P-712022→LV2002 bypass→150-P-712020 8-shaped blind plate discharges steam


Nitrogen from 25-GN-712007→25-GN-712007/1→200-P-712039→250-P-712042→A-71204→250-P-712043→
D-71203→D-71203 top vent
→80-NF-712026→PSV-71212A/B upstream flange and bypass valve downstream discharge steam
→150-P-712046→150-P-712049/1→150-P-712049→FT2014→PV2085bypass →100-P-712050/1 8-shaped blind plate discharges steam
→100-P-712050/2 8-shaped blind plate discharges steam
→50-P-712101 8-shaped blind plate discharges steam
→25-NF-712032→PSV-71217 upstream flange and bypass valve downstream discharge
steam
→150-P-712050 boundary 8-shaped blind plate discharges steam
→150-GH-72101 boundary 8-shaped blind plate discharges steam
→40-P-712050/4 boundary 8-shaped blind plate discharges steam
→80-GH-713001 8-shaped blind plate discharges steam
→50-P-712050/3 →non-return valve downstream FV1005 bypass discharge steam
→40-P-711089→PV1001A discharges steam
→SN-71203 sampler discharge steam
→150-P-712047→D-71206B→8-shaped blind plate at bottom flare line discharges steam
→SN-71205 sampler discharge steam
→8-shaped blind plate between double valves of 150-P-712049 line discharges steam
→80-NF-712024→PSV-71214 upstream flange and bypass valve downstream discharge steam
→25-GN-712009 8-shaped blind plate discharges steam
→150-P-712048/1 8-shaped blind plate discharges steam
→D-71206A →8-shaped blind plate at bottom flare line discharges steam
→SN-71204 sampler discharge steam
→8-shaped blind plate between double valves of 150-P-712048 line discharge steam
→80-NF-712022→PSV-71213 upstream flange and bypass valve downstream discharge steam
→25-GN-712008 8-shaped blind plate discharges steam
→D-71203 liquid level gauge discharge steam
→150-P-712044→LV-2008 discharges steam
→40-SLO-712004→underground drain and slop line 8-shaped blind plate discharges steam

ISSUE DATE: 20/03/06 - 71 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

2.4.3. Blowing-Up Purging Scheme


Use nitrogen to blow-up and purge system. Pipelines above DN150 should
undergo blowing-up purging. Blowing-up plate pressure is 0.3MPa.
 Close all instruments’ primary valves; instruments easily damaged with
vibration must be disconnected from purged pipeline.
 Remove all orifice plates on pipelines
 Announce the blowing-up area as a hazardous area and isolate it with a guard
tape.
 Use 0.8MPa nitrogen as a blowing-up purging media.

2.4.3.1. Reforming Section Blowing-Up Scheme


2.4.3.1.1. Introduce 0.8MPa nitrogen from outlet and inlet pipelines of K-71201
(close K-71201 outlet valve, install blind plate at K-71201 inlet filter
upstream flange, blowing-up purging media should not contact
compressor body)
2.4.3.1.2. At D-71201 top, turn the inlet elbow to atmosphere and install
temporary nozzle; the blowing-up flow is: 0.8MPa nitrogen to 50-GN-
712001→25-GN-71202→450-P-712015→600-P-712014→D-
71201top. Close other connected pipelines valves for isolation;
2.4.3.1.3. At E-71201 tube side, remove inlet hydrogen line’s non-return valve
and install temporary nozzle; the blowing-up flow is: 0.8MPa nitrogen
to 50-GN-712001→350-P-712016→E-71201 tube side inlet non-
return valve. Close other connected pipelines valves for isolation;
2.4.3.1.4. Blowing-up purging of reforming reaction system uses R-71202 inlet
as discharge nozzle. Remove R-71202 top inlet elbow pipe and
install blind plate on it together with E-71201 shell side inlet to isolate
the exchanger completely; purging will be done in two stages:
2.4.3.1.5. Install temporary nozzle at R-71202 top inlet, find a drain at E-71201
tube side outlet line, to connect a temporary line to introduce 0.8MPa
nitrogen; the blowing-up flow is: 0.8MPa nitrogen →500-P-
712002→F-71201→500-P-712003→R-71201→500-P-712004→F-
71202→500-P-712005→R-71202 top inlet. Close other connected
pipelines valves for isolation;
2.4.3.1.6. After system pipeline is purged to clean, install a temporary nozzle at
R-71202 top inlet. Find a drain on the shell side inlet of E-71201 to
connect a temporary line to introduce 0.8MPa nitrogen; the blowing-
up flow is: 0.8MPa nitrogen →500-P-712008→R-71203→500-P-
712007→F-71203→500-P-712006→R-71202 (enters from bottom
and flows upward) →R-71202 top nozzle. Close other connected
pipelines valves for isolation;
2.4.3.1.7. Insert a metal plate into E-71201 shell side outlet flange. Install blind
plate at A-71201 inlet to isolate completely. Find a drain near inlet of
A-71201 to connect a temporary line to introduce 0.8MPa nitrogen.
The purging flow is: 0.8MPa nitrogen →600-P-712011→E-71201
shell side outlet flange; Next, install a blind plate at E-71201 shell
side outlet flange to isolate completely,

ISSUE DATE: 20/03/06 - 72 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

2.4.3.2. Booster System Blowing-Up Scheme


2.4.3.2.1. Introduce 2.5MPa nitrogen from outlet and inlet pipelines of K-
71202A/B (close K-71202A/B outlets valve, install blind plate at K-
71202A/B inlets filter upstream flange, blowing-up purging media
should not contact compressor body)
2.4.3.2.2. At D-71207 top, turn the inlet elbow to atmosphere and install
temporary nozzle; the blowing-up flow is: 2.5MPa nitrogen enters
from K-71202A/B inlets respectively→25-GN-712004(25-GN-
712005)→400-P-712028→400-P-712027→D-71207 top outlet
flange. Close other connected pipelines valves for isolation;
2.4.3.2.3. Introduce 2.5MPa nitrogen from 1st stage outlet of K-71202A/B (close
K-71202A/B 1st stage outlet valve, blowing-up purging media should
not contact compressor body)
2.4.3.2.4. Install temporary nozzle at second valve of K-71202A 1st stage outlet
(remove valve); the blowing-up flow is: 2.5MPa nitrogen to 25-GN-
712007→300-P-712030→200-P-712029&300-P-712029/1→K-
71202A/B 1st stage outlet. Close other connected pipelines valves for
isolation;
2.4.3.2.5. After the pipeline from K-71202A/B 1st stage outlet to A-71203 is
blown-up to clean, connect K-71202A 1st outlet valve well, remove A-
71203 inlet blind plate and enter the next purging step: remove D-
71202 inlet flange and install temporary nozzle (if location is too
small to install temporary nozzle, insert metal plate at D-71202 inlet
flange for purging), the blowing-up (purging) flow is: 2.5MPa nitrogen
to 25-GN-712007→300-P-712030→A-71203→300-P-712031→D-
71202 inlet. Close other connected pipelines valves for isolation;
2.4.3.2.6. Introduce 2.5MPa nitrogen from outlet and inlet pipelines of K-
71202A/B 2nd stage (install blind plate at K-71202A/B inlets 2nd stage
filter upstream flange, close K-71202 A/B 2nd stage outlet valve,
blowing-up purging media should not conatct compressor body); at
D-71202 top, turn the inlet elbow to atmosphere and install temporary
nozzle; the blowing-up flow is: 2.5MPa nitrogen enters K-71202A/B
2nd stage inlets respectively→25-GN-712004/1 (25-GN-
712005/1)→300-P-712033→300-P-712032→D-71202 top. Close
other connected pipelines valves for isolation;
2.4.3.2.7. After pipeline is purged to clean, install temporary nozzle at the non-
return valve from K-71202A/B 2nd stage outlet to recontact system
(remove non-return valve); the blowing-up flow is: 2.5MPa nitrogen to
25-GN-712007→25-GN-712007/1→200-P-712039→the nozzle at
non-return valve. Close other connected pipelines valves for
isolation; remove A-71201 inlet blind plate, remove D-71207 inlet
flange and insert a metal plate.
2.4.3.2.8. Still use the drain at A-71201 inlet to connect a temporary line to
introduce 0.8MPa nitrogen.The purging flow is: 0.8MPa nitrogen
→600-P-712011→A-71201→700-P-712012→700-P-712013→D-
71207 inlet flange

ISSUE DATE: 20/03/06 - 73 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

 Blind plate table for blowing-up purging

No. Specifications Location Qty. Tube No. Status Remarks


5. Dg500 E-71201 shell side inlet 1 P-712008 Blind Temporary blind plate
6. Dg600 E-71201 shell side outlet 1 P-712011 Blind Temporary blind plate
7. Dg500 E-71201 tube side outlet 1 P-712002 Blind Temporary blind plate
8. Dg150 Downstream FV2006 1 P-712001 Blind 8-shaped blind plate
9. Dg80 R-71202 top leg pipes 8 CA-713012 Blind Temporary blind plate
10. Dg450 K-71201 inlet filter 1 P-712015 Blind Temporary blind plate
11. Dg450 K-71201 inlet line 1 P-712015 Open 8-shaped blind plate
12. Dg50 K-71201 outlet nitrogen line 1 GH-712001 Open 8-shaped blind plate
13. Dg25 K-71201 inlet nitrogen line 1 GH-712002 Open 8-shaped blind plate
14. Dg300 K-71201 outlet line 1 P-712016 Open 8-shaped blind plate
15. Dg200 D-71201 bottom pipeline 1 P-712018 Blind 8-shaped blind plate
16. Dg400 K-71202A/B 1st stage inlet filters 2 P-712028 Blind Temporary blind plate
st
17. Dg400 K-71202A/B 1 stage inlet lines 2 P-712028 Open 8-shaped blind plate
st
18. Dg25 K-71202A/B 1 stage inlet 2 GH-712004 Open 8-shaped blind plate
nitrogen lines
19. Dg300 K-71202A/B 1st stage outlet lines 2 P-712029 Blind 8-shaped blind plate
20. Dg25 K-71202A/B 1st stage outlet 1 GN-712007 Open 8-shaped blind plate
nitrogen lines
21. Dg300 K-71202A/B 2nd stage inlets 2 P-712033 Blind Temporary blind plate
filters
22. Dg300 K-71202A/B 2nd stage inlet lines 2 P-712033 Open 8-shaped blind plate
nd
23. Dg25 K-71202A/B 2 stage inlet 2 GH-712004/1 Open 8-shaped blind plate
nitrogen lines
24. Dg200 K-71202A/B 2nd stage outlet line 2 P-712038 Open 8-shaped blind plate
25. Dg25 K-71202A/B 2nd stage outlet 1 GN-712007/1 Open 8-shaped blind plate
nitrogen lines

ISSUE DATE: 20/03/06 - 74 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

2.4.4. Purging Of Utility Systems

2.4.4.1. Purging of 2.5MPa nitrogen line

2.4.4.1.1. Firstly, inspect to confirm that all branched lines of 2.5MPa nitrogen of CCR unit and the boundary valve of
GDHT unit are fully closed.
2.4.4.1.2. Introduce 2.5MPa nitrogen into the system, then, introduce nitrogen into the end of the CCR unit pipeline and
disconnect the blind flange at the end for blowing-up purging until the discharge is clear and the purging
requirements are met. Reinstall the blind flange.
2.4.4.1.3. Then, use nitrogen for purging and blowing-up purging to all branch lines respectively.
2.5MPa nitrogen →80-GN-714001→20-GN-711007 →purge at the disconnected location (disconnect D-71107 nitrogen inlet orifice plate) (remove top cover of D-71107 for water
washing)
→after D-71107 is washed to be up-to-standard →25-CL-711001→remove inlet filter of M-71101 to empty water flushing →after washing, re-
connect pipeline well → pump P-71106→25-CL-711004→to the location hand valve downstream
flange disconnects where pipeline 200-P-711003 is connected, flush with water
→25-CL-711001→20-CL-712010→flush P-71206A/B inlet pipelines with water (firstly, remove
pump inlet filter screen and flush with water, when it is up-to-standard, re-connect filter screen
well) → pump inlet drain discharges
→25-CL-711001→20-CL-712010→20-CL-712009→flush water in the location where 20-CL-
712007 line disconnects with 150-P-711044 line (simultaneously, flush water into pump outlet
line, discharge at pump outlet drain)
→after D-71107 is washed to be up-to-standard, re-connect D-71107 inlet pipeline to purge tank D-71107 with nitrogen, discharge from low
point on tank bottom outlet line→25-CL-711001→remove M-71101inlet filter for purging re-connect D-71107→ pump P-71206A/B line, purge,
discharge from the location where pump outlet line disconnects and low points on pump outlet and inlet lines

2.5MPa nitrogen →80-GN-714001→40-GN-711001→25-GN-71100→flange downstream first valve to K-71101A/B inlet nitrogen lines disconnects
→flange downstream first valve to K-71101A/B outlet nitrogen lines disconnects
→to the location where K-71101A/B instrument air blind plate disconnects
→40-GN-711003→ 8-shaped blind plate disconnects on D-71103 nitrogen line
→25-GN-712010→ 8-shaped blind plate disconnects on D-71204 nitrogen line
→25-GN-712008→ 8-shaped blind plate disconnects on D-71206A nitrogen line
→25-GN-712009→ 8-shaped blind plate disconnects on D-71206B nitrogen line
→25-GN-712007→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202A/B 1st outlet line (300-P-712030)
→25-GN-712007→25-GN-712007/1→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202A/B 2nd outlet line 200-
P-712039
→25-GN-712004/1→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202A 2nd inlet line (300-P-712033)
→25-GN-712005/1→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202B 2nd inlet line (300-P-712033/1)
2.5MPa nitrogen →80-GN-714001/1→80-GN-711001→25-GN-713028→GN-713067→Inlet of M-71302
→GN-713068→Inlet of M-71303

ISSUE DATE: 20/03/06 - 75 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

2.4.4.2. Purging Of 0.8mpa Nitrogen Line

2.4.4.2.1. Firstly, inspect to confirm that all branched lines of 0.8MPa nitrogen of CCR unit and the boundary valve to GDHT
unit are fully closed
2.4.4.2.2. Introduce 0.8MPa nitrogen from the system, then, introduce nitrogen to the end of reforming unit pipeline,
disconnect the blind flange at the end for blowing-up purging until the discharge is clear and the standard is met.
Reinstall the blind flange.
2.4.4.2.3. Then, use nitrogen for purging and blowing-up purging to all branch lines respectively
0.8MPa nitrogen →100-GN-714001/2→50-GN-712001→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71201 outlet and inlet lines.
→25-GN-712004→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71202A 1st inlet line.
→25-GN-712005→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71202B 1st inlet line.
→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71202B inlet line.
→25-GN-712103→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71201 outlet and inlet lines.
→25-GN-713064→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71302A outlet and inlet lines.
→25-GN-713064/1→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71302B outlet and inlet lines.
→25-GN-713063→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71301A outlet and inlet lines.
→25-GN-713063/1→ 8-shaped blind plate disconnects on nitrogen line that connects with K-71301B outlet and inlet lines.
→15-GN-719001→ 8-shaped blind plate disconnects on the nitrogen line that connects with K-71303 outlet and inlet lines.
→25-GN-714002→ flange downstream first valve of D-71405 disconnects.
→25-GN-714003→ flange downstream first valve of D-71404 disconnects.
→40-GN-713004→ 8-shaped blind plate disconnects at the joint of T-71303 oxychlorination zone line 40-GN-713005.
→to all hose stations

2.4.4.3. Purging Of Plant Air Pipeline


Firstly, inspect to confirm that all plant air branched lines and boundary valve of CCR unit are fully closed
Introduce plant air from system, then, introduce plant air to unit pipeline terminal, disconnect the blind flange at the end
for blowing-up purging until the discharge is clear and the standard is met. Reinstall the blind flange.
Then, use plant air to purge all branched lines respectively

Introduce plant air into →100-PA-714001→80-PA-711001→to hose stations in pretreatment part


→50-PA-713001→to hose stations in catalyst regeneration part
→50-PA-714002→to hose stations in utilities part
→80-PA-711002→to prehydrotreatment catalyst regeneration burning part
→80-PA-712001→to hose stations in reforming part

ISSUE DATE: 20/03/06 - 76 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

2.4.4.4. Purging Of Instrument Air Pipeline


2.4.4.4.1. Introduce instrument air to D-71402 inlet where uptream flange disconnects (disconnects pipeline flange before
air drum inlet) for blowing-up purging until the discharge is clear and the standard is met. Reinstall the blind
flange. Introduce instrument air into air drum D-71402. (Confirm that all instrument air branched lines to reforming
unit and hand valve to hydrogenation unit boundary valve have been fully closed) To purge air drum, i.e., make
discharge from air drum bottom until there is no emissions, then, close low-point hand valve.
2.4.4.4.2. Then, introduce instrument air into reforming unit pipeline terminal, disconnect the blind flange at the end for
blowing-up purging until the discharge is clear and the standard is met. Reinstall the blind flange.
2.4.4.4.3. Then, purge all instrument air branch lines respectively
Instrument air →150-IA-714001→D-71402→150-IA-714002→15-IA-714004→K-71201 steam solenoid valve UV-2002 where air line disconnects
→40-IA-711002→compressor room
→40-IA-711001→all instrument air using points in pretreatment part
→50-IA-712001→all instrument air using points in reforming part
→50-IA-71300/1→all instrument air using points in catalyst regeneration part
→40-IA-714003→all instrument air using points in hose stations part
→100-IA-713018→air using points in regeneration part

2.4.4.5. Purging Of 1.0mpa Steam Pipeline Reforming Unit


2.4.4.5.1. Firstly close hand valves from 1.0MPa steam header to all branch pipelines in the reforming unit
2.4.4.5.2. Then, introduce 1.0MPa steam from hydrogenation unit into reforming unit pipeline terminal; then, disconnect the
blind flange at the end for blowing-up purging until the discharge is clear and the standard is met. Reinstall the
blind flange.
2.4.4.5.3. Then, make blowing-up purging to following position pipeline respectively (make blowing-up purging respectively
one by one),
1.0MPa steam →200-LS-714002→20-LS-714005→to D-71401 inlet steam hand valve where upstream flange disconnects. (purge to clean and then re-connect flange) →to the
location where D-71401 outlet condensated water trap disconnects
→80-LS-714004→to E-71401 inlet steam hand valve where upstream flange disconnects (purge to clean and then re-connect flange) →to the
location where E-71401 outlet condensated water trap disconnects
→to hose stations
→50-LS-711001→to C-71101 purging where 8-shaped blind plate disconnects
→50-LS-711001/1→to all drain points on C-71101 fire protection line
→50-LS-712003→to C-71201 purging where 8-shaped blind plate disconnects
→50-LS-712004→to all drain points on C-71201 fire protection line
→ to K-71201 steam line where flange disconnects
→to hose stations in compressor area
→100-LS-71501→to the location where hot working part disconnects (blowing-up purging)
→80-LS-713001→to the location where DR-71301 steam inlet hand valve disconnects

ISSUE DATE: 20/03/06 - 77 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0
→80-LS-712002→to unit ejector J-71201 low-point condensate discharge
→to F-71201, F-71202, F-71203 fire protection steam and fire fighting steam where flange disconnects
→50-LS-714012→the location connecting with fuel gas line 50-GF-714001 from system where 8-shaped blind plate disconnects
→50-LS-714013→the location connecting with D-71401 discharging line 300-GF-714004 where 8-shaped blind plate disconnects
→to F-71101, F-71102, F-71205 fire protection steam and fire fighting steam where flange disconnects
→to the location where furnace fire protection steam flange disconnects

2.4.4.6. Flushing And Purging Of Water For Demineralized Water Pipeline

2.4.4.6.1. Firstly, inspect to confirm that all demineralized water branched lines of the reforming unit and hand valve to
hydrogenation unit boundary valve are fully closed
2.4.4.6.2. Introduce demineralized water from the system into reforming unit pipeline terminal; then, disconnect the blind
flange at the end for blowing-up purging until the discharge is clear and the standard is met. Reinstall the blind
flange. Then, use demineralized water to flush all branched lines respectively. Introduce demineralized water into
following positions respectively to flush:

Introduce demineralized water →150-SW-714001→40-SW-711006→to A-71101 water tank, then, empty from water tank for discharging.
→40-SW-711008→to A-71102 water tank, then, empty from water tank for discharging.
→50-SW-712006→to A-71201 water tank, then, empty from water tank for discharging.
→40-SW-712011→to A-71202 water tank, then, empty from water tank for discharging.
→40-SW-712009→to A-71203 water tank, then, empty from water tank for discharging.
→40-SW-712013→to A-71204 water tank, then, empty from water tank for discharging.
→100-SW-71501→to WHB
→40-SW-713008→to regeneration part oxychlorination water injection tank T-71302, empty from water tank for discharging.
→50-PW-713003→to P-713044 where flange disconnects
→40-SW-711001→to prehydrogenation water injection tank D-71106, then, empty from water tank for discharging.
→25-SW-712001→to reforming water injection tank D-71211, then, empty from water tank for discharging.
→50-SW-719010→to regeneration compressors house water station inlet where flange disconnects, after discharging to clean, re-connect flange.
Then, empty from water tank for discharging.
→to hydrogen compressor water station inlet where flange disconnects, after discharging to clean, re-connect flange. Then, empty from water tank
for discharging
→50-SW-713001→to P-71305A/B inlets where flange disconnects

ISSUE DATE: 20/03/06 - 78 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

2.4.4.7. Flushing And Purging Of Circulating Water Pipeline

2.4.4.7.1. Introduce circulating water into unit, (only open one-side boundary area circulating water inlet and outlet valve)
open bypass valves of all equipment using circulating water, close hand valves of inlet and outlet equipment
2.4.4.7.2. Then, introduce circulating water into all branched lines in turn to flush until the gas discharged from where all
branched lines disconnect is clear and meets the requirements. Then open another-side boundary area
circulating water valve.

2.4.4.8. Purging Of Fuel Gas Pipeline

2.4.4.8.1. Firstly confirm that fuel gas boundary hand valve is closed. Confirm that E-71401 bypass valve is opened; inlet
and outlet E-71401 hand valves are closed. Confirm that PV4303 bypass valve is opened; inlet and outlet
PV4303 hand valves are closed.
Introduce steam into →50-LS-714012→PV4303 bypass →300-GF-714001
→E-71401 shell side inlet where flange disconnects
→E-71401 tube side outlet where flange disconnects
→D-71401 fuel gas inlet where flange disconnects→purge to clean and then, re-connect flange
→D-71401 fuel gas tank bottom outlet and top flange downstream hand valve disconnects for discharging.
→50-LS-714013→D-71401 fuel gas top hand valve downstream flange disconnects for discharging.
→300-GF-714004→50-GF-711001→solenoid valve UV1001/B disconnects for purging →purge to be up-to-standard and then re-connect→PV1006 bypass →
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→50-GF-711001→25-GF-711002→solenoid valve UV1001/A disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV1001 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→80-GF-711005→solenoid valve UV1002/B disconnects for purging →purge to be up-to-standard and then re-connect→PV1007 bypass →
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→80-GF-711005→25-GF-711006→solenoid valve UV1002/A disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV1002 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→50-GF-712017→solenoid valve UV2004 disconnects for purging →purge to be up-to-standard and then re-connect→PV2110 bypass →
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→50-GF-712017→25-GF-712018→solenoid valve HV2004 disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV2112 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→100-GF-712001→solenoid valve UV2001/1 disconnects for purging →purge to be up-to-standard and then re-connect→PV2007 bypass →
burner flame arrester upstream flange disconnect for purging
→purge to be up-to-standard and then re-connect→purge to burner

ISSUE DATE: 20/03/06 - 79 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0
→300-GF-714004→100-GF-712001→25-GF-712002→solenoid valve HV2001/1 disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV2009 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→100-GF-712005→solenoid valve UV2001/2 disconnects for purging →purge to be up-to-standard and then re-connect→PV2019 bypass →
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→100-GF-712005→25-GF-712006→solenoid valve HV2001/2 disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV2021 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→80-GF-712009→solenoid valve UV2001/3 disconnects for purging →purge to be up-to-standard and then re-connect→PV2031 bypass →
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner
→300-GF-714004→80-GF-712009→25-GF-712010→solenoid valve HV2001/3 disconnects for purging →purge to be up-to-standard and then re-connect→filter
disconnects for purging →purge to be up-to-standard and then re-connect→PCV2033 disconnects for purging →purge to be up-to-standard and then re-connect→
burner flame arrester upstream flange disconnect for purging →purge to be up-to-standard and then re-connect→purge to burner

2.4.4.9. Purging Of Flare System Pipeline

2.4.4.9.1. Close reforming unit and confirm that all hand valves into D-71403 pipeline have been closed.
Introduce 1.0MPa steam into →500-NF-714001 (purge the main pipeline into D-71403) and discharge from bottom
1.0MPa Steam →500-NF-714001→D-71403→500-NF-714002 unit boundary 8-shaped blind plate disconnects
→80-SLO-714006 downstream valve flange disconnects
→150-NF-711003→Upstream D-71100 safety valves A/B and downstream bypass valve where flange disconnects
→80-NF-711006→Upstream D-71101 safety valves A/B and downstream bypass valve where flange disconnects
→50-NF-714008→the location where flame arrester FA-71402 disconnects (remove flame arrester)
→50-NF-714007→the location where flame arrester FA-71401 disconnects (remove flame arrester)
→150-NF-711017→Upstream C-71101 safety valves A/B and downstream bypass valve where flange disconnects
→80-NF-711011→Upstream K-71101A safety valve and downstream bypass valve where flange disconnects
→80-NF-711014→Upstream K-71101B safety valve and downstream bypass valve where flange disconnects
→450-NF-712005→Upstream D-71201 safety valve and downstream bypass valve where flange disconnects
→300-P-712025→D-71201 top where 8-shaped blind plate disconnects
→200-NF-712007→Upstream K-71201 safety valve and downstream bypass valve where flange disconnects
→150-NF-712009→Upstream D-71202 safety valve and downstream bypass valve where flange disconnects
→150-NF-712011→Upstream K-71202A 1st safety valve and downstream bypass valve where flange disconnects
→150-NF-712017→Upstream K-71202A 2nd safety valve and downstream bypass valve where flange disconnects
→150-NF-712016→Upstream K-202B 1st safety valve and downstream bypass valve where flange disconnects
→100-NF-712021→Upstream K-202B 2nd safety valve and downstream bypass valve where flange disconnects
→100-NF-712027→Upstream D-71203 safety valve and downstream bypass valve where flange disconnects
→80-NF-712029→Upstream D-71205 safety valve and downstream bypass valve where flange disconnects
→50-P-712069→the location connecting with line 50-P-712068 from D-71204 to fuel gas tank where 8-shaped blind plate disconnects
→100-NF-712023→Upstream D-71206A safety valve and downstream bypass valve where flange disconnects
→100-NF-712025→Upstream D-71206B safety valve and downstream bypass valve where flange disconnects
→40-P-712059→the location connecting with line 40-P-712058 from D-71205 to fuel gas tank where 8-shaped blind plate disconnects
→40-P-713057→ to T-71303 where flange downstream first valve disconnects
→100-NF-712031→Upstream C-71201 safety valve and downstream bypass valve where flange disconnects
→50-NF-711007→Upstream D-71101 safety valve and downstream bypass valve where flange disconnects

ISSUE DATE: 20/03/06 - 80 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

→40-NF-714009→ the location connecting with E-71401 steam inlet line where 8-shaped blind plate disconnects
→40-NF-714010→D-71401 bottom where 8-shaped blind plate disconnects
→100-NF-712040
→20-NF-712037→SN-71210 to first outlet valve where rear flange disconnects
→20-NF-712036→SN-71209 to first outlet valve where rear flange disconnects
→20-NF-712035→SN-71208 to first outlet valve where rear flange disconnects
→20-NF-712034→SN-71201 to first outlet valve where rear flange disconnects
→20-NF-711004→SN-71101 to first outlet valve where rear flange disconnects
→20-NF-711018→SN-71102 to first outlet valve where rear flange disconnects
→20-NF-711020→SN-71103 to first outlet valve where rear flange disconnects
→20-NF-711028→SN-71104 to first outlet valve where rear flange disconnects
→20-NF-711030→D-71105 to first outlet valve where rear flange disconnects
→50-NF-711021→D-71103 to first outlet valve where rear flange disconnects
→20-NF-711029→D-71107 to first outlet valve where rear flange disconnects
→100-P-712050/2→D-71206 reforming hydrogen exits where 8-shaped blind plate disconnects
→100-NF-714006→Upstream D-71401 safety valve and downstream bypass valve where flange disconnects

2.4.4.10. Purging Of Oil Collection Pipeline Of Drum D-71405


2.4.4.10.1. Introduce 0.8MPa nitrogen downstream inlet flange of underground oil collection drum D-71405 (disconnect
flange for purging until purge to be up-to-standard and then re-connect)
0.8MPa N2→25-GN-714002→D-71405→80-SLO-714005→100-SLO-714005 8-shaped blind plate disconnects
→100-SLO-711024 8-shaped blind plate disconnects
→50-SLO-714004→D-71404 upstream non-return valve disconnect
→150-SLO-714001→80-SLO-714006→D-71403 outlet where flange in front of hand valve disconnects
→40-SLO-712005→D-71205 outlet where flange in front of hand valve disconnects
→40-SLO-712006→D-71204 boot outlet where flange in front of hand valve disconnects
→40-SLO-712008→C-71201 bottom outlet where flange in front of hand valve disconnects
→40-SLO-712004→D-71203 bottom outlet where flange in front of hand valve disconnects
→40-SLO-712021→drain line on E-71203A/B outlet line where flange in front of hand valve disconnects
→40-SLO-712019→drain on line E-71208C tube pass outlet line where flange in front of hand valve disconnects
→40-SLO-712011→drain on line E-71208A tube pass outlet line where flange in front of hand valve disconnects
→40-SLO-712020→drain line on E-71208C shell pass outlet line where flange in front of hand valve disconnects
→40-SLO-712010→drain line on E-71208A shell pass outlet line where flange in front of hand valve disconnects
→40-SLO-712012→drain line on E-71201 tube pass outlet line where flange in front of hand valve disconnects
→40-SLO-711015→D-71103 boot outlet where flange in front of hand valve disconnects
→40-SLO-711008→D-71101 boot outlet where flange in front of hand valve disconnects
→50-SLO-711014→C-71101 bottom outlet where flange in front of hand valve disconnects
→40-SLO-711023→drain line between E-71103A and E-71103B/C shell pass where flange in front of hand valve
disconnects
→40-SLO-711022→drain line on E-71103A tube pass inlet line where flange in front of hand valve disconnects
→40-SLO-711011→drain line on E-71103C shell pass outlet where flange in front of hand valve disconnects
→40-SLO-711012→drain line on E-71103C tube pass inlet where flange in front of hand valve disconnects

ISSUE DATE: 20/03/06 - 81 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0
→40-SLO-711013→drain line on E-71109A/B outlet where flange in front of hand valve disconnects
→40-SLO-711007→drain line on E-71101B shell pass inlet line where flange in front of hand valve disconnects
→40-SLO-711006→drain line on E-71101B tube pass outlet line where flange in front of hand valve disconnects
→40-SLO-711003→hand valve of drain line on shell pass pipeline between E-71101A and E-71101B
→40-SLO-711002→ hand valve of drain line on tube pass between E-71101A and E-71101B
→40-SLO-711001→D71100 boot outlet where flange in front of hand valve disconnects

2.4.4.11. Purging Of Oil Collection Pipeline Of Drum D-71404

2.4.4.11.1. Introduce 0.8MPa nitrogen downstream inlet flange of underground oil collection drum D-71404 (disconnect
flange for purging until purge to be up-to-standard and then re-connect). Inject nitrogen into D-71404. If bottom
discharge is up-to-standard; then purge pipeline 80-SLO-714003 through its end flange. Disconnect the flange
for purging until up-to-standard and re-connect. Then, purge all branched lines respectively.
0.8MPa N2→25-GN-714003→D-71404→80-SLO-714003→40-SLO-712001→D-71201 bottom drain
→40-SLO-712003→D-71202 bottom drain
→40-SLO-712002→D-71207 bottom drain

2.4.4.12. Flushing Of Caustic Soda Pipeline


Introduce demineralized water from GDHT unit →40-KL-714001→
→40-SSW-713003→T-71301 inlet where flange disconnects for flushing (after flushing to clean, re-connect) →T-71301 low-point for discharging (close discharging
after being clean) →40-SSW-713004→P-71302A/B inlet drain for discharging and flushing (close after being discharged to clean) →40-SSW-713006→hand valve
connecting with P-71301 inlet line disconnects
→25-KL-711001→LV-1012 bypass →to D-71106 where inlet disconnects

ISSUE DATE: 20/03/06 - 82 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

3. Initial Leak (Air Tightness) Tests

3.1. Air Tightness Objective


Air tightness objective is to further inspect the quality of valve, flange, pipeline,
equipment, and welding seam using gas media (This unit uses nitrogen) to inspect
the leak sources in the system with field observation soap test method under the
regulated pressure.

3.2. Air-Tight Preparation


3.2.1. Air tightness test must be done after unit finishes purging, the pipe fittings such
as reassembled flanges, blind plates, and orifice plates etc. repositioned, the
existing problems have been rectified and improved and all flows reset.
3.2.2. Inspect the unit’s equipment, process pipelines, flanges, washer blind plates,
valves, safety valves, instruments, motors and pumps, etc. any problem should
be solved before air tightness test begin.
3.2.3. Contact with dispatcher to put the nitrogen source for air tightness into effect so
as to guarantee there is enough nitrogen supply.
3.2.4. Contact with dispatch to make preparation for transportation assurance of air
tightness gases
3.2.5. Contact with instrument to make air tightness to instruments related equipment
simultaneously with process system.
3.2.6. Prepare air tightness tools such as precision pressure gauge, spanner, soapy
water, brush, ear syringe, big and small barrels, etc. and organize personnel to
inspect and record by areas; workshop appoints special persons responsible
for handling of leakage points.
3.2.7. Inspect whether the air tightness points leak; use brush to brush soapy water or
use ear syringe to spray soapy water on air tightness points to observe whether
there is bubbles; if any, it means that the point is leakage point; then, mark it
with chalk or slate pencil and contact personnel to handle it in time.
3.2.8. For small space air tightness points, adhesive paper can be used to block the
flange, then, open a small hole on the adhesive paper, and then, inspect
whether the small hole leaks gas.
3.2.9. For the air tightness for drain points, their joints can be inserted into soapy
water for inspection.

3.3. Locations For Air Tightness Inspection


Air tightness inspection should be made to the system’s pipelines, equipment,
valves, flanges, pipe plugs, pressure gauges, instrument connecting positions,
pipeline welding seams, etc. They can be divided into reactor upper cap, lower outlet
flange, furnace inlet and outlet tubes, flanges in combined heat exchanger, high-
pressure separating tank liquid level gauge, pressure instrument flanges, etc.
according to locations.

ISSUE DATE: 20/03/06 - 83 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

3.4. Safety Considerations

3.4.1. Pressure boosting speed should be slow and air tightness test pressure should
comply with the regulations strictly without overpressure.
3.4.2. Any leak source found should be marked in time and the maintenance
personnel should be contacted for handling.
3.4.3. Pay attention to inspect whether there is interflow between systems and avoid
equipment overpressure strictly. Watch out for gas expansion in the system
and consequent equipment overpressure because of ambient air temperature
change.
3.4.4. During air tightness test, commands should be given uniformly and personnel
in all areas should contact with each other.
3.4.5. During air tightness test of each system, at least two pressure gauges should
be used to observe pressure with required pressure gauge precision of
magnitude 0.4, 1.5-2 times of the highest air tightness pressure.
3.4.6. Handling of leak sources under pressure is not allowed.

3.5. General Instructions

3.5.1. Initial leak tests will be performed under KRC or Engineering company
responsibility and the general instructions hereunder shall only be used as a
reminder.
3.5.2. The initial leak tests can be performed using air or nitrogen depending upon
local facilities. The test pressure will be the air or nitrogen system pressure or
the unit (or section of unit) design pressure, whichever is the lower.
3.5.3. The unit is isolated with blinds from adjacent sections containing hydrocarbons
(liquid or gaseous), and from utilities systems where pressure is lower than air
(or nitrogen) pressure.
3.5.4. The pressure rise must be checked on several manometers and possibly
checked on a pressure recorder. Leaks must be carefully located and
tightened. Their location must be recorded.
3.5.5. The leak test is satisfactory when the pressure decrease is lower than
0.005 MPa/hour over a period of 4 consecutive hours.
3.5.6. The air (nitrogen) used for leak tests should be purged out of the unit using low
points drains to remove free water, if any.
3.5.7. For the purpose of leak tests the unit will be divided into sections of
approximatively the same design pressure, as defined hereunder. Air (nitrogen)
will be injected at different locations depending upon check valves.
3.5.8. For the reaction sections the tests can be followed by a vacuum test at
maximum vacuum. Loss of vacuum shall not exceed 25 mm Hg/hour.

ISSUE DATE: 20/03/06 - 84 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

3.6. Recommended Sections For Leak Tests


For the purpose of leak testing reforming unit 71200 & Catalyst regeneration and
circulation unit 71300 are divided into the following sections.

A Reaction section (DWG. ReactionLEAK)


The following vessels with their connections are included:
 The reactors, R-71201/202/203
 The upper hoppers except the first upper hopper, D-71312 & D-71313
 The balance drums, D-71352 & D-71353
 The lower hoppers, except the first, D-71321 & D-71322 & D-71323
 The reduction chamber, D-71311
 The heaters, E-71301/302/303/304
 The feed/effluent exchanger E-71201 (welded plate type, special care must be
taken),
 The reactors effluent air cooler, A-71201
 The separator drum, D-71201
 The lift pots, except the first and last ones, D-71331 & D-71332
 H2 lift lines, heat exchangers, E-71304/305
 H2 rich gas compressors KO drum. D-71207

In addition, all utilities lines, especially the ones connected to the flare and fuel gas
networks (including safety valves) will be fitted with blind flanges.
The reaction section is isolated as described on the following attached scheme.
The points of isolation are indicative only and must be reviewed on-site, to take into
account actual piping arrangement.

B Recontacting section (DWGS. RecontactLEAK1/RecontactLEAK2)


The following vessels with their connections are included:
 The recontactor feed air cooler, A-71204
 The chloride absorber, D-71206A/B
 The recontacting drum. D-71203

In addition all utilities will be fitted with blind flanges.


The absorber section is isolated as shown on the following attached schemes.
Note: The interstage aircooler and the interstage drum of the booster compressors
are to be tested separately.

C Stabilization section (DWG. StabilizationLEAK)


The following vessels with their connections are included:
 The stabilizer absorber, D-71205
 The stabilizer feed / bottom exchanger, E-71208 A/B/C/D
 The stabilizer, C-71201
 The stabilizer reboiler, F-71205
 The reformate trim cooler, E-71203 A/B
 The stabilizer overhead air cooler, A-71202
 The stabilizer reflux drum, D-71204
ISSUE DATE: 20/03/06 - 85 -
KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

In addition all utilities will be fitted with blind flanges.


The stabilization section is isolated as shown on the following attached scheme.

D Nitrogen section (DWG. NitrogenLEAK)


The following vessels with their connections are included:
 The nitrogen lift gas lines,
 The first upper hopper, D-71310
 The first and last lift pots, D-71305 & D-71333
 The first and last catalyst lift pipes,
 The nitrogen loop trim cooler E-71306, storage cooler E-71307 and storage
drum, D-71341
 The upper surge drum, D-71301
 The catalyst fines filters, M-71302/303
 The nitrogen compressors KO. drum. D-71307

In addition all utilities will be fitted with blind flanges.


The nitrogen section is isolated as shown on the following attached scheme.

E Regeneration loop (DWG. RegenerationLEAK)


The following vessels with their connections are included:
 The lock hopper, D-71302
 The burning, oxychlorination and calcination heaters, H-71301/302/303
 The regenerator and first lower hopper, R-71301 & D-71304
 The burning feed/effluent exchanger, E-71301
 The calcination feed/effluent exchanger, E-71302
 The regeneration loop trim cooler, E-71303
 The washing drum, D-71306
 The regeneration gas dryer package, DR-71301
 The air trim cooler E-71308, dryer drum D-71342 and dryer DR-71302.

In addition all utilities will be fitted with blind flanges.


The regeneration loop section is isolated as shown on the following attached
scheme.

ISSUE DATE: 20/03/06 - 86 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

3.7. Reforming Unit Leak Test Procedure

Reaction Section
 The airtightness media is N2. Introduce nitrogen from hydrogen recycle
compressor K-71201 outlet to boost pressure. The pressure tapping point
uses pressure at separating drum D-71201 as reference. The highest work
pressure of D-71201 namely 0.4MPa is for reference.

 Air tightness standard


Air tightness Air tightness Pressure Constant Allowed
section pressure boosting pressure static
MPag speed time pressure
MPa/5min h drop
MPa/h
reaction 0.40 0.05 8 0.005

 Airtightness steps
1) Use the reforming ejector J-71201 after checking the airtightness flow
(The end lines of all pressure gauge pressure introduction lines should
be isolated before producing vaccuum) to evacuate the reforming
system. If vaccuum can’t reach 600mmHg after evacuuation for 2h, it
means that the system has obvious leak sources and further pressure
boosting is needed for inspection.
2) After vacuum test finishes, install 8-shaped blind plate in D-71201
vacuum line
3) Introduce nitrogen (circulation compressor K-71201 outlet) to break the
vacuum slowly. Pressurize the system to 0.4MPa (boost pressure
according to D-71201 regulations strictly). Make leakage test
inspection to system’s all air tightness points. Air tightness is up-to-
standard if pressure drop is lower than 0.005MPa/h continuously for
4h.

Recontacting Section
 The air tightness media is N2. Introduce nitrogen from hydrogen booster
compressor K-71202 outlet to boost pressure. The pressure tapping point
uses pressure at recontacting drum D-71203 as reference. The highest work
pressure of D-71203 namely 2.3MPa is for reference.

 Air tightness standard


Air tightness Air tightness Pressure Constant Allowed
section phase boosting pressure static
MPa g speed time pressure
MPa/5min h drop
MPa/h
recontacting 2.3 0.05 8 0.005

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KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

Stabilization Section
 Air tightness test of steady section uses 2.5MPa nitrogen as media. Introduce
nitrogen from nitrogen line 25-GN-712010 at D-71204 top to pressurize with
pressure tapping point at D-71205 as reference and highest operation
pressure of 1.6MPa. The leakage test is up-to-standard when pressure drop
is smaller than 0.005MPa/h for 4h continuously.

 Air tightness standard


Pressure Constant Allowed
Airtightness Airtightness
boosting pressure pressure
section phase
MPa speed time drop
MPa/5min h MPa/h
0.5 0.1 4 0.005
C-71201 1.0 0.1 4 0.005
1.6 0.1 4 0.005

 Air tightness steps


(1) Line-up the air tightness flow and then use N2 to boost pressure.
(2) Make air tightness inspection to all air tightness points in the system with
soapy water according to air tightness standard by phases. Any leak source
found should be recorded, labeled, rectified and treated subsequently.
(3) According to the air tightness requirements, the system’s leakage test is up-
to-standard when the final 1.6MPa air tightness is up-to-standard.

Chronologically, once the initial leak tests are over, the drying out of the unit
takes place, prior to catalyst loading.

ISSUE DATE: 20/03/06 - 88 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

4. Unit Drying
4.1. Drying Objective:
Reaction, catalyst circulation and regeneration sections must be dried out prior to
catalyst loading, firstly to avoid damaging the catalyst with water, secondly to
shorten the duration of the low severity operation after first oil in.

4.2. Drying Procedure Outlines


4.2.1. Unit dry out is conducted simultaneously with the heater refractory drying.
4.2.2. The dry out operation is carried out using hot nitrogen circulating in two loops,
physically separated. Temperature profile should strictly follow up the following
two diagrams:
 Furnaces F-71201/202/203 drying curve
 Reaction section drying curve (DWG. Dryingcurve1)
4.2.3. The first loop uses the recycle compressor, the hydrogen rich gas compressor
and the nitrogen lift gas compressor and includes the reaction section,
absorber section and nitrogen section as defined above in chapter 3.6
"Recommended sections for leak tests". The fired heaters are used for warming
up.
4.2.4. The second loop is the regeneration section (regeneration section as defined in
3.6 "Recommended sections for leak tests") and uses the regeneration loop
compressor to circulate nitrogen which is heated in the electrical heaters
(burning, oxychlorination and calcination heaters). The regeneration drying loop
is isolated from the previous one by the special gas tight valves between the
lock hopper and the upper surge drum and the valve on the seal leg between
the first lower hopper and its lift pot.

4.3. Preparation Work Before Unit Drying:


4.3.1. All TIs and TRs (in the firing box, in the process fluid, tube skin) have been
checked. The burners, dampers, control and safety systems have been
checked. All safety measures and control normally involved in the firing of
heaters must be followed in agreement with KRC or heaters manufacturer
procedures.
4.3.2. Make a list of required instruments and check that they are connected and in
service.
4.3.3. Check that orifices plates are installed where required and correctly calibrated
(coefficient adjusted for nitrogen) check that all safety valves are installed and
connected to atmosphere.
4.3.4. Make sure that all blinds between reaction section and Recontacting section
are removed.
4.3.5. The following compressors must be commissioned prior to start (blinds will be
removed and left in open position):
 Recycle compressor K-71201
 H2 rich gas compressors K-71202 A/B
 Nitrogen compressors K-71302 A/B
 Regeneration loop compressors K-71301 A/B
Note: To initiate the dry out of the reaction section, the recycle compressor
only is required.
ISSUE DATE: 20/03/06 - 89 -
KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

4.3.6. Commission cooling water to and start:


 Reactor effluent air cooler A-71201 A/B/C
 Recontacting air cooler A-71204
 Interstage air cooler A-71203
 Reduction gas trim cooler E-71304
 Nitrogen loop trim cooler E-71306

4.4. Drying of reaction and recontacting sections:


4.4.1. All blind plates have been installed to or removed from the specified locations
according to blind plates table.
4.4.2. Reaction section pressurization (reaction section as defined in 3.6
“Recommended sections for leak tests")
4.4.2.1. Check that:
 The reaction section is blocked in at the feed inlet
 The separator drum bottom pumps P-71201A/B are isolated.
 The off gas line to flare is blinded.
4.4.2.2. Nitrogen is introduced at recycle compressor K-71201 and the reaction
section is pressurized to 0.2 MPa gauge. The pressure controller on
separator drum D-71201 is commissioned and set to 0.2MPa gauge. Off
gas is discharged to atmosphere.
4.4.2.3. Special precautions must be followed concerning the feed/effluent
exchanger in, case of the choice of a welded plates heat exchanger (see
note 4.5.2).

4.4.3. Recontacting section pressurization


4.4.3.1. This section is pressurized simultaneously with the reaction section,
provided the following blinds have been removed in due time.
 On H2 rich gas kick back line 300-P-712035 to H2 compressor KO
drum D-71207.
 On H2 rich gas line to catalyst reduction 80-GH-713001

4.4.4. Nitrogen section pressurization


4.4.4.1. The equipment of the nitrogen section are lined up (refer to 6.4.3.6
"Recommended sections for leak tests" for definition of this equipment).
4.4.4.2. The section is pressurized to 0.2 MPa gauge.
4.4.4.3. Then reactor and absorber sections on one hand, nitrogen section on the
other hand, are connected while the following isolating valves are opened:
 On first upper hopper to reduction chamber UV3011
 On last reactor lower hopper to its lift pot UV3013
 On start up line 100-GN-712003 between separator drum (reaction
section) and nitrogen loop trim cooler.

4.4.5. Establish nitrogen circulation


4.4.5.1. Open suction and discharge valve of recycle compressor K-71201 and
start the machine according to manufacturer's instructions. This initiates
nitrogen circulation through the reaction section. Once the section is on
line, start draining free water from all low points.
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PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

K-71201→E-71201→F-71201→R-71201→F-71202→R-71202→F-
71203→R-71203→E-71201→A-71201→D-71201→K-71201

4.4.5.2. Light small fires in the preheater F-71201 and heaters F-71202 & F-71203
according to ignition instructions in KRCIM 71200.07 and increase reactor
inlet temperature at a rate of 40°C per hour up to 200°C.

4.4.5.3. The following steps must now take place to circulate nitrogen in the
recontacting section and nitrogen section:
 Line up the H2 rich gas circuit to reductor D-71311 and to 1st and
2nd reactors lift pots D-71331 & D-71332. Note that hydrogen
purification unit M-71301 is isolated and by passed.
 Start the H2 rich gas compressor K-71202A/B at 25% capacity, all
the compressed gas being recycled to H2 rich gas compressor KO
drum D-71207, the spill back PV2068C is full open in manual. KO
drums PIC2079 & PIC2080 are set in auto mode.
 Establish flow of gas (up to normal flow taking into account you
are handling nitrogen) to the 1st and 2nd reactors lift pots and to
the reduction chamber.
 Line up the N2 lift gas circuit to the regenerator and last lift pot,
upper surge drum and first upper hopper, fines filters. Set
PIC3014 on N2 lift gas compressor discharge at 0.3 MPa g.
 Start up K-71303 to establish flow to first upper hopper D-71310.
This will assure the smooth operability of elutriation system.
 Start N2 lift gas compressor K-71302 and load the valves to
circulate the gas at 100% capacity.
 Establish flow of gas to the regenerator and last lift pot up to the
normal flow.
4.4.5.4. When the above steps are completed, the nitrogen circulation for drying
purpose is fully established, as shown on the attached drawings (DWGS.
ReactionDRY, RecontactDRY & NitrogenDRY).

4.4.6. The reduction electrical heater H-71304 is then switched on and reduction
chamber inlet temperature is progressively increased at a rate of 20°C per hour
up to 200°C. H-71304 flow is 1900Nm3/h.

4.4.7. Follow-up and end of drying (DWG.Dryingcurve1)


4.4.7.1. Purge water from separator drain and all low points (air cooler and trim
cooler outlets, separators, compressors KO. drums etc.). Keep record of
all the water drained to follow the drying rate, showing total amount of
water drained at regular intervals.
4.4.7.2. The system is considered dry, at this temperature (200°C), when the water
draw-off is less than 10 liters per hour.
4.4.7.3. Then the temperatures are increased to 400°C at a rate of 20°C per hour.
When the amount of water drained is lower than 5.0 liter per hour the

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PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

temperature is increased to 500°C and maintained until the total water


draw-off is less than 1.0 liter per hour.
4.4.7.4. Note that the reduction heater outlet temperature is increased to 450°C
only.
4.4.7.5. The 500°C temperature must be reached in the reaction section in order
to check if any problem, due to the thermal expansion of the reactor
internals, occurs.
4.4.7.6. When the system is dry, lower the temperature to 200°C (50°C/h). Then
stop firing or stop electrical heaters and circulate nitrogen until the
reactors are cooled down to 40°C. The doors of the heater boxes could be
opened in order to speed-up the cooling process.
4.4.7.7. Stop then the recycle and H2 rich gas compressors and close the block
valves at suction and discharge. Depressurize and repressurize the unit
with air, to remove nitrogen. Check that the atmosphere is suitable for
entry into the vessels.

4.5. Notes
4.5.1. During the temperature rise, watch the skin temperatures of the heater tubes
and flue-gas temperature to avoid any overheating of the tubes. Check also the
temperature of each equipment in order not to exceed the design figures.
4.5.2. Welded plates heat exchanger (feed/effluent) E-71201
The following precautions must be carefully observed:
 Owing to the narrow space (2.5 mm) between plates, the upstream
piping must be thoroughly flushed prior to flow through the exchanger.
 During shell or bundle flushing (to remove air or process fluids) the
differential temperature between the feed stream and the effluent stream
must not exceed 50°C.
 The plate are stainless steel. Presence of chloride and liquid water for
an extended period must be avoided.
 Ensure that the feed side pressure always exceeds the effluent side
pressure. Consequently:
o the exchanger must be pressurized only from the feed inlet
(recycle compressor discharge).
o the exchanger must be depressurized only from the effluent outlet
(separator drum).
 When introducing the naphtha feed (Oil-in stage) at a linear rate in order
to reach 60% of the design within ten minutes. Ensure that both inlet
flows are balanced.

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KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

5. Catalyst Loading

5.1. Preliminary
5.1.1. When the reaction section drying out is complete and nitrogen has been
replaced by air, the CCR reactors and the regenerator can be opened for
inspection of the internals, cover plates and grids, to make sure that thermal
expansion has not caused any damage.
5.1.2. If needed, the reactors and regenerator will be brushed and vacuum cleaned
before catalyst loading starts.
5.1.3. The catalyst loading period must be as short as possible to minimize the risk of
moisture entering the reaction system. If necessary, the job will be done in
shifts.
5.1.4. Catalyst loading will preferably be interrupted in case of rain or snow, or
efficient protection must be in place.
5.1.5. The catalyst must be handled with care to avoid breakage of the catalyst
spheres. During the loading, the loading sleeves will be adjusted to allow a free
fall no higher than 2 meters above the catalyst level.
5.1.6. A representative of the Gamma Ray Level manufacturer is required for level
calibration.

5.2. Equipment And Personnel


The list below is based on the following assumption: catalyst loading will be carried
out with 2 cranes at the same time. One crane will be dedicated to load the first
reactor and regenerator. This crane must be able to handle a mobile hopper full of
catalyst, above the structure. For the 2nd and 3rd reactors, a second crane will be
used.
 2 telescopic cranes capable of lifting approximatively 3 tons, 5 meters
above the reactor upper manhole (See appendix 1).
 1 forklift to handle the catalyst drum pallets.
 2 stationary hoppers equipped with Ø 8 to 10" nozzles to be installed on the
reactor upper manhole (See appendix 2 and 4).
 4 mobile hoppers, each with a capacity of about 5 to 6 catalyst drums (See
appendix 3 and 4).
 1 structure (scaffolding and timbers) to unload the drums into the mobile
hoppers (See appendix 5).
 1 safety harness, portable oxygen analyzer, dust masks, goggles, plastic
sheets to protect drums and reactor in case of rain.
 2 empty half drums (for lift pots) and plastic sheets to install underneath.
 2 Ø 600 mm funnels (for upper hoppers) (See appendix 6).

To serve the above mentioned equipment the following personnel is necessary:


 1 foreman,
 2 crane operators,
 1 fork lift operator,
 1 team of 6 riggers at ground level for catalyst handling and loading into the
mobile hoppers,

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KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

 1 gamma ray level specialist, assisted by one instrument technician during


the loading of the vessels located above reactors and regenerator.
 1 team of 6 fitters for vessels opening and closing (inlet elbows,
manholes,...).

Note:This personnel shall be permanently present during the loading operation. The
total number of personnel will be obtained by multiplying by the number of shifts.

5.3. Manholes, Piping And Internals To Be Removed


(See Appendix 7)
For internal inspection and catalyst loading, some equipment must be removed:
5.3.1. For each reactor:
 4 inlet catalyst pipes
 1 inlet elbow
 8 cover plates
 3 conical sectors
 For each lift pot:
 1 primary injection nozzle
 For each balance drum
 3 x 3" flanges
5.3.2. For the 1st upper hopper and upper surge drum:
 1 elutriator (2 flanges each)
 1 manhole
5.3.3. For the lock hopper:
 1 manhole
5.3.4. For the reduction chamber:
 1 manhole
5.3.5. For the regenerator:
 5 manholes
 2 valves (ROVs between hopper and regenerator).
5.3.6. For each upper hopper, except the first:
 1 catalyst loading nozzle
 1 shell removal (MH flange untied)
 1 liaison pipe flanges untied.

5.4. Catalyst Drums Location


(See Appendix 8)
5.4.1. Most of catalyst is loaded by mean of the stationary hopper.
5.4.2. For the X-ray levels calibration the loading will be carried out with drums. These
drums will be located above the following equipment. The number of drums
hereunder will be determined on site by startup representative.

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KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

Reactor 1 : drums *
Reactor 2 : drums *
Reactor 3 : drums *
First upper hopper : drums
2d upper hopper : drums
3d upper hopper : drums
Regenerator manhole 5 : drums *
Regenerator manhole 1 : drums
Lock hopper : drums
Upper surge drum elutriator : drums
*: Check of the outlet catalyst pipes

5.5. Estimated Catalyst Inventory


The figures shown hereunder are determined at the process design stage. The
actual amount loaded may differ slightly and must be carefully recorded.

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KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

Approximated number of drums for the initial loading


(approx. 105 kg for each drum).
m3 DRUMS
1st Reactor Upper hopper 0.63
Reduction chamber 1.46
Reduction chamber legs 0.17
Other legs 0.13
Reactor 8.15
1st Reactor lower hopper and lift pot 0.13
TOTAL 1st REACTOR SECTION 10.68 66

m3 DRUMS
2nd Reactor Upper hopper 0.32
Upper hopper legs 0.17
Other legs 0.13
Reactor 12.15
2nd Reactor lower hopper and lift pot 0.13
TOTAL 2nd REACTOR SECTION 12.90 80

m3 DRUMS
3rd Reactor Upper hopper 0.32
Upper hopper legs 0.17
Other legs 0.13
Reactor 20.31
3rd Reactor lower hopper and lift pot 0.13
TOTAL 3rd REACTOR SECTION 21.06 130

m3 DRUMS
Legs 0.07
Lock hopper 0.63
Regenerator 4.07
First lower hopper and first lift pot 0.13
TOTAL REGENERATOR SECTION 4.90 30
TOTAL CATALYST TO BE LOADED
Reactors 44.64
: m3
Regenerator 4.90: m3
TOTAL 49.54
: m3 (307 Drums)

Note: Four additional drums to be stored nearby the catalyst loading device for
future loading and to be protected against rain.

ISSUE DATE: 20/03/06 - 96 -


KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

5.6. Reactors Loading


REMARK:
From this point, the detail of the number of drums to be loaded, at each step of the
procedure, has been left in blank (xxx) in the text, as well as in the drawings
(appendix 7 to 12).
The recommended number of drums will be determined, on site, and it is suggested
that the number of drums actually loaded be filled in during the loading process, in
place of the blanks.

5.6.1. Loading preparation


5.6.1.1. For each reactor, dismantle the four inlet catalyst pipes to permit the
removal of the inlet elbow. Protect the flanges against shocks.
5.6.1.2. Remove the reactor inlet elbows.
5.6.1.3. Pull out the reactors inlet distributors to permit entering into the reactors
and protect the manhole flanges against shocks.
5.6.1.4. Check that the atmosphere is suitable to enter the reactors (the previous
operation was drying with nitrogen).
5.6.1.5. As during reaction section dry out, high temperatures have been reached
(about 500 degrees C), the reactors internals must be inspected to
detect any problems caused by thermal expansion.
5.6.1.6. Some of the cover plates and sector pieces have to be dismantled to allow
internal inspection, cleaning and catalyst loading.
5.6.1.7. Before catalyst loading starts, make sure that the 4 catalyst nozzles at the
top of the reactors are free of any foreign material and covered with plastic
bags. A good house keeping around the reactor top manholes must be
maintained.
5.6.1.8. Remove the primary gas injection from the bottom of each lift pot.
5.6.1.9. Check each lift pot again for primary injection nozzle location.
5.6.1.10. Open the special tight manual valves on the catalyst lines under the
lower hoppers .
5.6.1.11. Remove the first reactor upper hopper manhole and elutriator tube to
permit lift piping checking.
5.6.1.12. Catalyst loading nozzles are opened on the 2nd and 3rd upper hoppers.
5.6.1.13. Close special tight manual valves on the lift pipes.
5.6.1.14. Catalyst outlet pipes and lower hoppers must be checked to make sure
that no foreign material remains inside. Air flush from inside the reactors
each of the 12 catalyst pipes.
5.6.1.15. When the flow from the lift pot bottom is dust free, close the special tight
manual valve on the catalyst line under the lower hoppers of each
reactor.

5.6.2. Reactors and lower hoppers loading

CATALYST FLOW TEST


5.6.2.1. The beginning of catalyst loading operation will be the same for each
reactor (see appendix 1 "Reactor and lower hopper loading").
5.6.2.2. Load two drums of catalyst into the reactor, in order to fill up the outlet
catalyst pipes, lower hopper and seal leg.
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PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

5.6.2.3. Knock on the pipe wall to check whether catalyst pipes are full.
5.6.2.4. Open the special tight manual valves under each lower hopper and unload
the catalyst in a clean drum installed under the lift pot.
5.6.2.5. When catalyst flow stops, check again by knocking that the catalyst pipes
are empty.
5.6.2.6. Close special tight manual valves under the lower hoppers and reinstall
the primary hydrogen gas nozzle on the lift pots.
5.6.2.7. When the test is completed, catalyst loading can start.

CATALYST LOADING
5.6.2.8. When the catalyst level reaches the upper part of the reactor centerpipe,
the catalyst loading is stopped.
5.6.2.9. Reinstall the sectors pieces and the removed cover plates, except 4 of
them located at 90° kept dismantled to control the end of catalyst
loading.
5.6.2.10. Fill up the conical parts of the catalyst bed.
5.6.2.11. Fit in the last 4 cover plates.
5.6.2.12. Install the reactor inlet distributors.
5.6.2.13. Install the reactor inlet elbows.
5.6.2.14. Install the four upper inlet catalyst pipes.

Note: For the end of catalyst loading, the procedure for the first reactor is different
from the other reactors (go to first reactor end of loading).

5.6.3. 2nd and 3rd reactors end of loading

CATALYST LOADING AND CALIBRATION (See appendix 1 and 10)


5.6.3.1. Through the catalyst feed nozzle, fill up the catalyst inlet pipes of the
reactor. Stop catalyst loading when they are full (checking by knocking).
5.6.3.2. Fill up 2nd and 3rd upper hoppers, calibrate the levels LIC with the
manufacturer. Note also at which level % the LSLL are activated.
5.6.3.3. Open the special tight manual valves under the lower hoppers. The lift
pots will be filled. Check in parallel the deviation of the 2 nd and 3rd upper
hoppers levels at the DCS.
5.6.3.4. Close the 2nd and 3rd upper hoppers catalyst loading nozzles.

5.6.4. First reactor end of loading

5.6.4.1. Check the 1st upper hopper catalyst sampling device.


5.6.4.2. Open the manual and auto special tight valves between the 1st reactor
upper hopper and the reduction chamber.

CATALYST LOADING AND CALIBRATION (See appendix 11)


5.6.4.3. Fill up the inlet catalyst pipes by loading catalyst through the 1st upper
hopper top hand hole.
5.6.4.4. Stop catalyst loading when they are full (checking by knocking).
5.6.4.5. Close the special tight manual valve under the 1st upper hopper.
5.6.4.6. Fill up the 1st upper hopper, with only xxx drums, about 40%.
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PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

5.6.4.7. Open the special tight manual valve under the 1st upper hopper, the
reduction chamber will be filled up partially.
5.6.4.8. Fill the 1st upper hopper, with 1 additional drum.
5.6.4.9. Close the special tight manual valve under the 1st upper hopper.
5.6.4.10. Fill up the 1st upper hopper, calibrate its level, in coordination with the
level manufacturer:
 xx drums and xx liters are loaded, this is 0% of the LI
 xx drums are loaded, to fill completely the cone: xx% of the LI
 xx drums are loaded: xx% of the LI per drum.
A total of xx drums will be loaded.
Note that the low level alarm LALL of the 1st upper hopper should be
switched off before reaching 20% at the LI.
5.6.4.11. Open the special tight manual valve under the 1st upper hopper and
finish filling the reduction chamber. Check the deviation of the 1st upper
hopper level LI on the DCS.
5.6.4.12. Check that the primary hydrogen nozzle of the first lift pot is reinstalled
and open the special tight manual valves under the 1st reactor lower
hopper. The lift pot will be filled up. Check again the deviation of the 1st
upper hopper level LI indication on the DCS.
5.6.4.13. Install the 1st upper hopper elutriator pipe and connect the piping. This
finishes the initial loading of the reactors.

5.6.5. Regenerator loading

Operation schedule
5.6.1. Open manholes MH1, MH2, MH3, MH4 and MH5 of the regenerator and the
MH of the upper surge drum.
5.6.2. Check if the atmosphere in the regenerator is breathable, for entry.
5.6.3. After inspection, and tack welding of the bolt pins, close the top manhole MH1
and reinstall the catalyst line from the lock hopper bottom to the regenerator.
After setting the internal plug, close the MH of the upper surge drum.
5.6.4. A good house keeping around the regenerator top manhole MH1 must be
maintained.
5.6.5. Remove the primary gas injection nozzle from the bottom of the lift pot.
5.6.6. The lift pot under the regenerator must be checked again (primary injection
nozzle location).
5.6.7. Remove the upper surge drum elutriator to permit lift pipe checking.
5.6.8. After lift pipe checking close the special tight manual valve on the lift pipe.
5.6.9. The catalyst pipes of the first lower hopper must be checked to make sure
that no foreign material remains inside.
5.6.10. Air flush from the regenerator each of the 6 catalyst pipes one by one.
5.6.11. Then, when the flow from the lift pot bottom is dust free, close the special tight
manual valve under the first lower hopper.
5.6.12. The catalyst flow test can now be carried out.

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5.6.13. One drum of catalyst will be loaded into the calcination zone of the
regenerator through the lower manhole MH5, in order to fill the first lower
hopper and the catalyst outlet pipes.
5.6.14. Check that the hopper pipes are full of catalyst (knock on the pipe wall).
5.6.15. Open the special tight manual valve under the first lower hopper and unload
the catalyst into a clean drum installed under the lift pot.
5.6.16. When catalyst flow stops, check that the first lower hopper pipes are empty.
5.6.17. Close the special tight manual valve under the first lower hopper and reinstall
the primary gas nozzle on the lift pot.
5.6.18. When the test is complete close the lower manholes MH4 and MH5 after
having set the internal plug.
5.6.19. Catalyst loading can now start.
5.6.20. At the beginning of the operation catalyst will be loaded from the upper surge
drum using the elutriator nozzle.
5.6.21. Open the automatic special catalyst tight valve UV between the upper surge
drum and the lock hopper.
5.6.22. Open the automatic special gas tight valve UV between the lock hopper and
the regenerator.
5.6.23. Open the automatic special gas tight valve UV between the upper surge drum
and the lock hopper.
5.6.24. Close the automatic special catalyst tight valve UV between the lock hopper
and the regenerator.
5.6.25. Check the lock hopper catalyst sampling device.

Lock hopper level alarm test (71 to 78).


5.6.26. Add catalyst in ten liter quantities until the low level alarm (LAL) is switched
OFF. The quantity to be added is xxx liters.
5.6.27. Open the automatic special catalyst tight valve UV between the lock hopper
and the regenerator. The lock hopper low level alarm LAL will be switched
ON.
5.6.28. Close the automatic special catalyst tight valve UV between the lock hopper
and the regenerator.
5.6.29. Add xxx drums in the upper surge drum. The lock hopper low level alarm LAL
will be switched OFF and the high level alarm LAH must stay OFF.
5.6.30. Add catalyst in ten liter quantities until the lock hopper high level alarm LAH is
switched ON. The quantity to be added is xxx liters.
5.6.31. Open the automatic special catalyst tight valve UV between the lock hopper
and the regenerator. The high level alarm LAH will be switched OFF, and the
low level alarm LAL will be switched ON, as the catalyst loads the
regenerator.
5.6.32. Close then automatic special catalyst tight valve UV between the upper surge
drum and lock hopper. Close the automatic special catalyst tight valve UV
between the lock hopper and the regenerator.

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Upper surge drum level indicator LI tests (80 to 86).


5.6.33. Load one drum into the upper surge drum The level must show 0%.
5.6.34. Add catalyst in ten liter quantities until the level indicator show 10%. The
quantity to be added is xxx liters.
5.6.35. Open the automatic special catalyst tight valve between the upper surge drum
and the lock hopper. The level indicator must show 0% again.
5.6.36. Close the automatic special catalyst tight valve UV between the upper surge
drum and the lock hopper.
5.6.37. Add xxx drums into the upper surge drum . The LI should indicate 100% but
high level alarm LAH must stay OFF.
5.6.38. Add one catalyst drum first and then in ten liter quantities until the high high
level alarm LAHH is switched ON. The quantity to be added is xxx liters.
5.6.39. Open the automatic special catalyst tight valve between the upper surge drum
and the lock hopper. LAHH will be switched OFF. The low level alarm LAL will
be switched ON.
5.6.40. Open the automatic special catalyst tight valve UV between the lock hopper
and the regenerator.
5.6.41. Check that the system is catalyst tight at the manholes MH2 and MH3.
5.6.42. Open the top manhole MH1.
5.6.43. Fill the regenerator from the top manhole with catalyst until the low low level
alarm LALL is switched OFF (xxx drums).
5.6.44. Close manhole MH1 and connect the catalyst line.

The level indicator LI of the regenerator can now be calibrated. This must
be done, in coordination with the level manufacturer.
5.6.45. Catalyst will be loaded drum by drum from the top of the upper surge drum.
5.6.46. All the automatic special catalyst tight valves are opened. The low low level
alarm LALL is switched OFF while the level indicator LI shows 0%.
5.6.47. Load xxx drum. The level indicator LI must show 10%.
5.6.48. Load drum after drum to perform level calibration including DCS low level and
high level alarms of this vessel.
5.6.49. Total number of drums added: xxx).
5.6.50. Check that the primary gas nozzle of the lift pot is reinstalled and open the
special tight manual valve between the first lower hopper and the regenerator
lift pot.
5.6.51. The lift pot will be filled. Check in parallel the deviation of the upper surge
drum level indicator LI on the DCS.
5.6.52. Close the automatic special catalyst tight valve UV between the upper surge
drum and the regenerator, and load the lock hopper with xxx drums, from the
top of the upper surge drum.
5.6.53. Reinstall then the elutriator and the related piping on top of the upper surge
drum.
5.6.54. Close manholes MH2, MH3 of the regenerator. This finishes the initial
loading of the regeneration section.

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6. Second Leak Test And Partial Inerting


6.1. After the catalyst loading, the reaction section and the regeneration section must be
leak tested again to inspect the removed positions for catalyst loading.
6.2. Leak test is combined with partial inerting: the objective is to reach an oxygen content
between 2 and 5% for the purpose of catalyst circulation. This is achieved by
successive pressurizations and depressurizations with nitrogen. Since catalyst
circulation will require the running of the H2 rich gas compressor, the absorber
section is also subject to partial inerting.
6.3. Leak test (using nitrogen):
 Reaction section, regeneration section and absorber section are isolated from
the rest of the unit. All pumps and compressors (suction / discharge valves) are
isolated.
 All connections to the flare are blinded.
 All safety valves are connected to atmosphere, if not possible, the collector to the
flare is blind to battery limit.
 Blind the hydrogen lines from the HP absorber to fuel gas system, to
downstream users and all lines going out to battery limits.
 A temporary blind is installed on liquid feed line to the LPG absorber.
6.4. All sections are pressurized with nitrogen up to 0.35 MPa gage.
6.5. The test is considered satisfactory when the average pressure decrease is lower than
0.005 MPa per hour during 4 hours.

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7. Supplements

 StartupScheme

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CCR UNIT KRCIM 71200.05 REV.0

 DWG.ReactionLEAK

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 DWG.RecontactLEAK1

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CCR UNIT KRCIM 71200.05 REV.0

 DWG.RecontactLEAK2

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CCR UNIT KRCIM 71200.05 REV.0

 DWG.StabilizationLEAK

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CCR UNIT KRCIM 71200.05 REV.0

 DWG.NitrogenLEAK

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PRODUCTION & OPERATION START-UP OPERATIONS (1)
CCR UNIT KRCIM 71200.05 REV.0

 DWG.RegenerationLEAK

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 Dryingcurve1

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 DWG.ReactionDRY

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 DWG.RecontactDRY

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 DWG.NitrogenDRY

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CCR UNIT KRCIM 71200.05 REV.0

 Appendix 1

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 Appendix 2

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 Appendix 3

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 Appendix 4

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 Appendix 5

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 Appendix 6

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 Appendix 7

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 Appendix 8

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 Appendix 9

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 Appendix 10

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 Appendix 11

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 Appendix 12

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 Appendix 13

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KRC REFORMING SECTION
PRODUCTION & OPERATION START-UP OPERATIONS (2)
CCR UNIT KRCIM 71200.06 REV.0

Contents: This instruction outlines the procedure for the start-up of the CCR reforming
Unit from the stage where the catalyst is being loaded. The text includes:

1. First Startup Of The Unit


2. Catalyst Circulation, Heating and Drying Procedures
3. Final Inerting
4. Reforming Section Startup
5. Oil In
6. Regeneration Startup
7. Unit Restart
8. Supplements

1. First Startup Of The Unit


1.1. Objective
The following describes the very first startup of a newly built unit. Any subsequent
startup of the same unit will very likely not include all the following steps but part of
them only, depending upon the status of the unit after the shutdown. For instance
the catalyst reduction procedure needs not be performed again, except in the case
of catalyst renewal.

1.2. Status
The status of the unit prior to its initial startup is a follows:
1.2.1. Each section as defined in chapter (3.6/ KRCIM 71200.05) “Recommended
sections for leak tests" has been leak tested (initial leak tests).
1.2.2. All the sections (except the stabilization section) have been dried.
1.2.3. Catalyst has been loaded in the reactors and the regenerator and the relevant
sections leak tested again and partially inerted (residual content of 0 2
between 2 and 5% volume).
1.2.4. The stabilization section has not been inerted
1.2.5. The unit is isolated with blinds at the battery limits:
 on the feed and products lines.
 on the flare and fuel gas headers.
1.2.6. Pressure relief valves in the reaction and HP absorber sections are blanked
off, except those to atmosphere.
1.2.7. The PCV on the separator drum discharges to atmosphere.
1.2.8. Pressure relief valves in the regeneration and nitrogen sections are directed
to atmosphere (normal status).

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1.3. Chronology
The sequence of first startup is as follows:
1.3.1. Circulation of catalyst and drying of catalyst under an atmosphere with a
residual O2 content.
1.3.2. Complete inerting of the sections involved in the circulation (i.e. all sections
except stabilization) O2 content is reduced to less than 0.2% volume.
1.3.3. Complete inerting of the stabilization section.
1.3.4. Stabilization section startup on total reflux.
1.3.5. Pressurization with hydrogen of the reaction section and the HP absorber
section.
1.3.6. Heating up and reduction of catalyst.
1.3.7. Oil in.
1.3.8. Operation of the unit at low capacity and low severity.
1.3.9. Operation of the unit at low capacity and high severity.
1.3.10. Operation of the unit at nominal capacity and high severity.
1.3.11. Start of the catalyst circulation.
1.3.12. Start of catalyst regeneration.

2. Catalyst Circulation, Heating and Drying Procedures


2.1. Objective of Heating and Drying
2.1.1. This operations must take place prior to oil in, in order to:
 Test the catalyst circulation and let the beds expand (the catalyst gets
closer to its density in operation).
 Dry the catalyst.
2.1.2. The catalyst is dried by a mixture of air and nitrogen. Air is used to prevent
sintering of the metals of the catalyst. The oxygen content in the sections
concerned must be kept between 3 and 5% volume.

Note: When pre-reduced catalyst is used heating and drying of the catalyst cannot
be performed. After recycle gas compressor startup reaction section heaters pilots
are lighted-on and the temperature of the circulating gas shall not be higher than
100°C.

2.2. Objective of Catalyst Circulation


2.2.1. To perform the drying-out of the catalyst located outside the reaction section
and into the regenerator section.
2.2.2. To perform the first catalyst circulation to check the correct catalyst flow
through the entire circulation loop.
2.2.3. To check and adjust the automatic regenerator catalyst transfer sequence.
2.2.4. And finally to perform the operator training of the catalyst circulation operation
without any hazard risk from the Hydrogen lift gas.
2.2.5. Key points to get catalyst circulation under nitrogen:
 Always get the correct pressure balance around the lift pot.
 The FV primary gas setting for the lift which normally operates under
Hydrogen has to be adjusted due to the gas molecular weight difference
between H2 and N2.
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Always start by the FCV to set the primary flow to empty the small catalyst
quantity which is already engaged on the lift area and, then have a smooth
action on the DPCV lift valve to get catalyst lift smooth start-up.
2.2.6. As the catalyst circulation may not be stable due to low pressure drop across
the reactors, it may not be easy to keep running the catalyst circulation
continuously.

2.3. Outline of Circulation Procedure and Principle of Catalyst Transportation


2.3.1. The sections concerned are the reaction section and the recontacting section,
the nitrogen section and the regeneration section. These sections have
normally been left under a pressure of air and nitrogen, at the end of the
second leak test and partial inerting chapter (6/ KRCIM 71200.05) “Second
leak test and partial inerting”.
2.3.2. Nitrogen circulation is then started in the reaction and absorber section
through the recycle and the hydrogen rich gas compressors, in the nitrogen
section by means of the nitrogen lift compressors. In the regeneration section
which is isolated from the latter ones, nitrogen is circulated through the
regeneration compressor.
2.3.3. N2 seal gas is established first. Although this is not strictly mandatory at this
moment (there is no H2 nor HC yet in the unit), it is advised to do so, to train
operators to use the right sequence and to test the interlocks associated with
N2 seal.
2.3.4. Catalyst circulation is started from reactor R3 lift pot to the upper surge drum,
then from reactor R2 lift pot to reactor R3 upper hopper ... from reactor R1 lift
pot to reactor R2 upper hopper and ultimately from regenerator lift pot to
reactor R1 upper hopper. (Fig. 8) For memory Fig. 9 and 10 show how the
catalyst flows in the reactors and the regenerator.
In order to understand how catalyst flow is started and controlled, the
principles of catalyst transport and catalyst flow control are shown in
Fig. 11.
2.3.5. The total lift gas (primary plus secondary gas) must be kept constant to
ensure a constant catalyst particles velocity. The secondary lift gas controls
the amount of catalyst which is introduced in the primary lift gas. Within the
design operating range, the catalyst flow is proportional to the secondary flow
of gas. Moreover the differential pressure in the lift pipe is proportional to the
catalyst flow, hence lift catalyst flow is measured and controlled by the
differential pressure.
2.3.6. The differential pressure controller of the catalyst lift pipe is reset by the level
of its destination upper hopper. This applies to the lift pipes A to C (Fig. 8). It
does not apply to lift pipe D because the upper surge drum level works on an
ON/OFF basis. The PDC set point of lift pipe D is fixed by the operator and
actually governs the catalyst flow in the whole unit.
2.3.7. A paramount criteria in catalyst circulation is safety. During normal
operation, when hydrocarbons are present in the reaction section, they
must be prevented from entering the regeneration section, and air from
entering the reaction section. Hence, the lifts from the last reactor lift pot to

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CCR UNIT KRCIM 71200.06 REV.0

the upper surge drum and from the regenerator lift pot to the 1st upper hopper use
nitrogen. Moreover an independent source of nitrogen referred to as " N 2 seal gas" is
used (refer Fig. 12):
 to maintain a controlled nitrogen over pressure between the first
reactor upper hopper and the reduction chamber.
 to maintain an overpressure in the last reactor lower hopper against
the lift pot pressure on one side and the reactor pressure on the other
side (refer to Fig. 13).
 to maintain an overpressure in the first lower hopper against the lift pot
pressure and the regenerator pressure (refer to Fig. 13).

Note: Seal gas using hydrogen is also injected in the lower hoppers of reactors 1
and 2 to prevent hydrocarbons from entering into the lift pipes.
In normal operation (hydrocarbons in the reaction section) nitrogen seals and
hydrogen seals must always be established prior to starting catalyst
circulation.
The details of the catalyst circulation and drying procedure are covered in the
following paragraphs.

2.4. Preparation

2.4.1. Unit status check


Prior to start, confirm the status of the unit:

2.4.1.1. Reaction section and recontacting section are interconnected and


isolated from the rest of the unit as follows:

 8 blind plate is blinded after reforming feed filters (150-P-712001)


 All samplers outlet lines to flare is blinded
 Install a blind after valve on makeup hydrogen line to prehydrotreatment
(50-P-712050/3)
 8 blind plate at hydrogen line to fuel gas system blind is blinded (100-P-
712050/1)
 8 blind plate at hydrogen line to flare header is blinded (100-P-712050/2)
 Install a blind after check valve at hydrogen line to hydrogen network
(150-P-712050)
 8 blind plate at secondary valve of hydrogen line from GDHT unit (40-P-
712050/4)
 8 blind plate at D-71201 hydrogen gas to flare header is blinded (300-P-
712025)
 Install a blind after LV2006 at D-71203 outlet (150-P-712044)
 Install a blind after LV2006 bypass at D-71203 outlet (150-P-712044)
 8 blind plate at line (100-P-712097)from D-71201 to ejector J-71201 is
blinded
 8 blind at D-71201 bottom line to slop oil system is blinded
 8 blind at D-71207 bottom line to slop oil system is blinded
 8 blind at D-71202 bottom line to slop oil system is blinded
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 8 blind plate at line (50-P-712032/1)from D-71202 to ejector J-71201 is


blinded
 8 blind plate at start-up hydrogen line to K-71201 (50-P-712101)
 8 blind plate at bottom of D-71206A to flare is blinded.
 8 blind plate at bottom of D-71206B to flare is blinded.
 8 blind at D-71203 bottom line to slop oil system is blinded
 8 blind plate at E-71201 tube side inlet to slop oil system is blinded.
 Must close P-71201A / B pump outlet, inlet valve. 8 blind plate at line
200-P-712018 is blinded
 Put all of cooling plants in this part into operation.
 Catalyst level indicators and alarms have been commissioned

2.4.1.2. Nitrogen section isolated (see DWG. Initial Status) as follows: -

Special catalyst tight manual valves:


 on seal legs at bottom of reactors 1 and 2 : closed
 on seal legs at bottom of last reactor and regenerator : open
 on lift lines : open
 from first upper hopper D-71310 to reduction chamber : open

Lock hopper D-71302 is isolated by remote operated ON/OFF valves:


 from upper surge drum UV3001 and 3002 : closed
 from regenerator UV3003 and 3004 : closed
 from N2 seal gas UV3010 : closed
 N2 seal gas to upper surge drum UV3006 : closed

First upper hopper D-71310 isolated (by ROV, ON/OFF):


 from reduction chamber UV3011 : closed
 from N2 seal gas UV3012 : closed

First lower hopper D-71304 isolated (by ROV, ON/OFF):


 from first lift pot UV3005 : closed
 from N2 seal gas UV3007 : closed

Last lower hopper D-71323 isolated (by ROV, ON/OFF):


 from lift pot UV3013 : closed
 from N2 seal gas UV3014 : closed

2.4.1.3. Regeneration section already isolated from nitrogen section:


 On top of regenerator UV3003 and 3004 : closed
 On bottom line of lower hopper UV3005 : closed

 Commission the oxygen analyzer AE3004 to the


oxychlorination/calcination zone at the shell inlet of the exchanger E-
71302.

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 Commission the oxygen analyzer AE 3105 at the suction of the N2


compressor K-71302 and set the scale on 0-10% vol.
 Temporarily connect the oxygen analyzer AE3001 located on shell
side inlet of burning feed / effluent exchanger E-71301 to any point of
the reaction section, (scale 0-10%), in order to follow the O2
concentration in the reaction section.
Note that the information from the 02 analyzers to the interlock and
sequence systems must be inhibited.

2.5. Establishing Circulation Procedure

2.5.1. Establish nitrogen cycle

2.5.1.1. Recycle compressor and H2 rich gas compressor


The circulation involves the reaction section and recontacting section as
shown in the DRY OUT process flow schemes
2.5.1.1.1. Start the recycle compressor K-71201 as per manufacturer's
instructions and adjust flow to the maximum acceptable with nitrogen.
2.5.1.1.2. Start the H2 rich gas compressor K-71202A/B, as per manufacturer's
instructions, at minimum capacity. As the duty of this machine will
only be to supply gas sent to the reduction chamber and gas to the
2nd and 3rd lift pots, the main part of the available flow will be recycled
to the suction KO drum through the spill back PV2068C & PV2079.
This valve is controlled in manual. Set ~ 1.0 MPa g at compressor
discharge pressure.
2.5.1.1.3. The pressure in the separator drum D-71201 is set at 0.35 MPa g,
and monitored by the pressure controller. The PV2068A/B is directed
to atmosphere.

2.5.1.2. Nitrogen lift compressor K-71302


The circulation involves the nitrogen section (Refer to DRY OUT process
flow scheme).
2.5.1.2.1. Start the nitrogen lift gas compressor K-71302, at 100% capacity.
2.5.1.2.2. Pressure set point for PI3016: 0.35 MPa g at the suction.
2.5.1.2.3. Pressure set point for PI 3060: 0.60 MPa g at the discharge (check
the temperature at compressor discharge. Prevent over high
temperature).

2.5.1.3. Regeneration loop compressor K-71301


2.5.1.3.1. Start-up the regeneration recycle gas compressor and increase
capacity to 100% (compressor by-pass FV3004 is progressively
closed)
2.5.1.3.2. Set burning, oxychlorination and calcination flows at 80% of design
value.
2.5.1.3.3. Pressure set point for regeneration loop pressure PIC3002: 1st
reactor inlet pressure (PI3123) + 0.070 MPa
2.5.1.3.4. Commission the regeneration loop dryer DR-71301

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2.5.1.3.5. Put in service PDIC3005 between regenerator top and first burning
zone.
2.5.1.3.6. Put in service PDT3003 (Differential Pressure between second
burning zone and oxychlorination/calcination zone in regenerator) but
keep corresponding control valves PDV3003A and PDV3003 B in
manual.

2.5.2. Initiate gas seal system


Supply seal nitrogen for nitrogen sealing system. Concrete procedures as
follows:

2.5.2.1. Establish N2 seal gas to the first reactor upper hopper D-71310
2.5.2.1.1. Override interlocks IS3019 and IS3025 to allow proceeding with next
steps.
2.5.2.1.2. Open ON /OFF valve UV3012 (N2 seal gas to upper hopper).
2.5.2.1.3. Open FIC3011 (before UV3012) manually: adjust flow to the design
figure. Switch into auto. Set corresponding FSLL 3114 at design
value.
2.5.2.1.4. Put PDIC3019 and PDALL3122 in service (Differential Pressure First
upper hopper / reduction chamber).
2.5.2.1.5. Open ON/OFF valve UV3011 manually between D-71310 and D-
71311.
2.5.2.1.6. Wait a few minutes to allow pressure and flow to stabilize.
2.5.2.1.7. Reset interlock IS3019. UV3012 and UV3011 must remain open
2.5.2.1.8. Correct flow coefficient of orifice for use of nitrogen
Since the first upper hopper is now sealed from the reduction chamber,
reduction gas circulation can be established to the reduction heater, reduction
chamber and coolers (refer to Fig 14). Line up the equipment involved and put
in service PDIC3012 at tube side outlet of reduction exchanger, FIC3017 at
shell side inlet of reduction exchanger and PIC3004 at shell side inlet of
hydrogen lift gas exchanger

2.5.2.2. Establish N2 seal gas to the third reactor


2.5.2.2.1. Override interlock IS3022.
2.5.2.2.2. Open in manual, ON/OFF valve UV3013 (between last lower hopper
and lift pot).
2.5.2.2.3. Open in manual, ON/OFF valve UV3014 (N2 seal gas to last lower
hopper).
2.5.2.2.4. Open FIC3016 (before UV3014) manually: adjust flow to the design
figure. Switch into auto.
2.5.2.2.5. Put PDIC3018 in service (Diff. Pressure between N2 seal gas and
primary lift gas)
2.5.2.2.6. Put PDI3137, PDALL3137 in service (Diff. pressure between last
reactor and N2 seal gas).
2.5.2.2.7. Reset interlocks IS3022, IS3025. ON/OFF valves UV3013 and
UV3014 must remain open.

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2.5.2.3.Establish N2 seal gas to regenerator seal leg


1. Override interlock IS3016.
2. Open ON/OFF valve UV3005 manually.
3. Put PDIC3007 in service (Diff. Pressure between N2 seal gas and
regenerator bottom).
4. Put PDI3114, PDALL3114 in service (Diff. Pressure between N 2 seal gas
and primary lift gas).
5. Reset interlock IS3016, UV3005 must remain open.

2.5.2.4. Establish H2 seal gas to 1st and 2nd reactors bottoms


Note: at this stage nitrogen is used instead of hydrogen
Adjust seal gas with globe valve to the 1st and 2nd reactors, in order to
meet design value for the two corresponding PDIs. PDI3119 & PDI3127

2.5.3. Establish catalyst circulation


2.5.3.1. The following valve should be already opened
 UV3011 top of reduction chamber
 UV3013 on last reactor seal leg
 UV3005 on regenerator seal leg

2.5.3.2. Operators must now open the other valves on catalyst (manual local
catalyst tight valves): on seal legs between lower hoppers and lift pots of
1st and 2nd reactors.
2.5.3.3. For each of the four lift pots, first adjust total gas flow manually through
the four corresponding FICs to the recommended figure as indicated in
"Lift gas flow". For the FICs through second and third lift pots, correct
coefficient for nitrogen. Then switch to auto mode
2.5.3.4. Open slowly PDV3011 (last reactor lift pot) in order to lift catalyst to the
upper surge drum until the level in the 3 rd upper hopper decreases to
40%.
2.5.3.5. Then open slowly PDV3009 (second reactor lift pot) in order to lift
catalyst to the 3rd upper hopper until the level in the 3rd upper hopper
decreases to 40%.
2.5.3.6. Then open slowly PDV3008 (second reactor lift pot) in order to lift
catalyst to 3rd upper hopper until the level in the second upper hopper
decreases to 40%.
2.5.3.7. Then open slowly PDV3006 (first reactor lift pot) in order to lift catalyst to
the 2nd upper hopper until the level in the 1st upper hopper has been
decreased by about 30%.
2.5.3.8. Make Adjustments to keep the levels constant
2.5.3.9. The PDIs of the lift pipes will be set at a value between 0.010 and 0.020
MPa as to obtain equal catalyst flows
2.5.3.10. Stabilize the circulation, in manual mode, until the levels in the upper
hoppers are steady. Set the catalyst circulation at about 25% of the
design flow. Then set the control in auto-cascade from level controllers
to differential pressure controllers

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2.5.4. Catalyst transfer sequence


At the beginning of the catalyst circulation, it is recommended to carry out the
first transfers from the upper surge drum to the lock hopper and from the lock
hopper to the regenerator in manual mode.
After a few manual transfer sequences to solve the teething problems, if any,
the catalyst transfer is switched to full auto mode.

2.5.4.1. Catalyst handling from surge drum D-71301 to lock hopper D-71302:
2.5.4.1.1. The level of catalyst increases in the upper surge drum while it
decreases in the regenerator. When these levels reach the transfer
conditions, open the pressure equalizing valve UV3006 between the
lock hopper and the surge drum: the pressures will equalize.
2.5.4.1.2. Open then the two ON/OFF valves UV3001 & UV3002 below the
upper surge drum, allowing the catalyst transfer into the lock hopper.
2.5.4.1.3. Then close the pressure equalizing valve UV3006 and the two
ON/OFF valves UV3001 & UV3002.

2.5.4.2. Catalyst handling from lock hopper D-71302 to regenerator R-71301:


2.5.4.2.1. After the transfer from the upper surge drum to the lock hopper the
situation is as follows:
 The four automatic ON/OFF valves between upper surge drum
and lock hopper and between lock hopper and regenerator are
closed. UV3001, UV3002, UV3003 & UV3004
 The two pressure equalizing valves are closed UV3006 &
UV3009.
 The upper surge drum D-71301 is empty but the catalyst coming
from the bottom of the last reactor R3 is filling up the lower part of
the vessel.
 The high level alarm LAH3108 of the lock hopper indicates full .
 The level in the upper part of the regenerator is still going down
as catalyst is withdrawn. Regenerator level is in the middle of the
range.
2.5.4.2.2. Open the pressure equalizing valve between the lock hopper and the
regenerator UV3009.
2.5.4.2.3. When the pressures between the two vessels are equalized, open
the ON/OFF valves under the lock hopper UV3003 & UV3004. The
catalyst is transferred to the regenerator.
2.5.4.2.4. When LAL3109 of the lock hopper is activated, close the ON/OFF
valves to regenerator and pressure equalizing valves UV3003,
UV3004 & UV3009.The sequence is in stand-by conditions

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CCR UNIT KRCIM 71200.06 REV.0

2.6. Catalyst Heating Up and Drying


2.6.1. Preparation
2.6.1.1. Make sure the O2 content in reaction section and regeneration section is
between 3 to 5% by volume until the end of the heating.

2.6.1.2. If required, inject air in reaction section at the recycle compressor K-71201
suction and in regeneration section at suction of loop compressor K-
71301.
2.6.1.3. To test the make up air compressor K-71304, if possible, operate this
machine to introduce air in the regeneration section.

2.6.2. Heating up, drying procedure


2.6.2.1. When oxygen content is confirmed and catalyst circulation in automatic
steady conditions light small fires in the reforming heaters F-
71201,202,203 according to instructions in KRCIM 71200.07.
2.6.2.2. Start electrical heaters on the regeneration loop H-71301,302,303 and on
H2 gas to the reduction chamber H-71304.
2.6.2.3. Increase the temperatures in the reactors and regenerator beds at a rate
of 20°C per hour. Start to perform hot bolting around 250°C.
2.6.2.4. When temperatures in the reactors and regenerator are above 300°C,
start to drain water at all low points of the sections and keep a record of
the amount drained.
2.6.2.5. Increase the temperatures up to 480°C in the reaction section and to
420°C in the regeneration section and reduction section. Keep theses
values for at least 8 hours or more if the amount of drained water stays
above 0.05% of the catalyst weight per hour
2.6.2.6. When the total amount of water drained at the low points is lower than
0.05% of the catalyst weight per hour, decrease the bed temperatures to
300°C at a rate of 40°C per hour.
2.6.2.7. Stop the fired and electrical heaters but keep pilot burners on for fired
heaters.
2.6.2.8. Stop catalyst circulation while closing the four FVs on lift pots streams and
the four PDV's measuring the lift pots P. Close block valves related to the
control valves. The closure of the catalyst tight manual valves under the
lower hoppers, under the first upper hopper and the closure of UV3005
(bottom of regenerator) is optional
2.6.2.9. Stop the compressors when the heaters are shut down.

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CCR UNIT KRCIM 71200.06 REV.0

2.7. Instruments Set Points


The recommended set points for nitrogen circulation and catalyst circulation are
listed below: the figure shown must be confirmed by AXENS start up representative.

Parameter Parameter point name Unit (MPa)


PIC2068 Recycle compressor K-71201 suction 0.220
PIC2079 H2 rich gas compressor K-71202A/B suction 0.210
PIC2085 Hydrogen rich gas to reduction delivery pressure 2.080
PIC3016 Nitrogen lift gas compressor K-71302 suction 0.225
PI3160 Nitrogen lift gas compressor discharge 0.870
PDIC3019 Differential Pressure N2 seal gas/reduction 0.015
chamber
PDALL3122 Differential Pressure N2 seal gas/reduction 0.005(min)
chamber
PDIC3012 Differential pressure reduction chamber / 1st 0.010
reactor
PDIC3018 Differential Pressure N2 seal gas/last reactor lift 0.015
pot.
PDIC3007 Differential Pressure N2 seal gas/regenerator 0.005
bottom
PDIC3118 Primary lift gas / 1st reactor 0.010
PDIC3126 Primary lift gas / 2nd reactor 0.010
PDIC3018 Primary lift gas / 3rd reactor 0.015
PDI3135 Differential Pressure N2 seal gas/3rd reactor 0.005
outlet
PDALL3137 Differential Pressure N2 seal gas/3rd reactor 0.002(min)
outlet
PDI3114 Differential Pressure N2 seal gas/regenerator lift 0.015
pot
PDAL3114 Differential Pressure N2 seal gas/regenerator lift 0.003(min)
pot
PDI3119 Differential Pressure H2 seal gas/1st reactor 0.005
outlet
PDI3127 Differential Pressure H2 seal gas/2nd reactor 0.005
outlet

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Parameter Parameter position Unit (Kg/h)


FIC3011 N2 seal gas to 1st reactor upper hopper 12
FALL3114 N2 seal gas to 1st reactor upper hopper 6(min)
FIC3016 N2 seal gas to 3rd reactor lower hopper 55
FALL3117 N2 seal gas to 3rd reactor lower hopper 22(min)
FIC3017 Hydrogen rich gas to reduction 216
FIC3010 Total lift gas to regenerator lift pot 354
FIC3012 Total lift gas to 1st reactor lift pot 108
FIC3013 Total lift gas to 2nd reactor lift pot 102
FIC3015 Total lift gas to 3rd reactor lift pot 296

Note: During trial run, (according to the pressure of lift pot), recalculate N2 flow rate.

3. Final Inerting
The purpose is to reduce the O2 content in all the sections below 0.2% volume prior
to hydrocarbons introduction. All the sections (with the exception of the stabilization
section) have been partially inerted (2 to 5% volume of residual O2). The stabilization
section has not been inerted at all.
3.1. All sections except stabilization
3.1.1. The catalyst beds have been left at approximately 300°C at the end of the
catalyst circulation .
3.1.2. Electrical and fired heaters are off. But fired heaters pilot burners are on.
3.1.3. All compressors are stopped. They must be isolated and purged with N 2 and
left under an atmosphere of pure N2.
3.1.4. Remove blinds on all process lines between the sections (if any remain) - with
the exception of the stabilization section - remove also blinds to/from the
battery limits (with the exception of the liquid feed).
3.1.5. Remove blinds on the safety valves to flare.
3.1.6. Install blinds on the safety valves which were previously routed to atmosphere.
(Reaction, Recontacting and stabilization sections only). Install also a blind on
PV2068 previously directed to atmosphere (suction of recycle compressor).
3.1.7. Close double block valves on start-up lines:
 Between recycle compressor suction and nitrogen lift gas compressor
suction 100-GN-712003
 Between hydrogen rich gas product and nitrogen lift gas compressor
discharge: 80-GN-713050
3.1.8. Depressurize the reaction section to 0.010 MPa gauge then introduce N 2 to
recycle compressor discharge and raise the pressure to 0.400 MPa g.
Depressurize again to 0.010 MPa gauge, through all the low points dead legs,
etc. Vent and drain the special heat exchanger (reactor feed/effluent) last.
Renew the operation until the O2 content is below 0.2% volume. Leave a
residual N2 pressure of 0.005 to 0.010 MPa gauge.
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3.1.9. Repeat same steps for the recontacting section. Residual pressure 0.005 to
0.010 MPa gauge.
3.1.10. Do the same for the regeneration section. Residual pressure 0.350 MPa
gauge.

Typically the required O2 content (0.2% volume) is achieved with 3 cycles


(pressurization/depressurization)

3.2. Stabilization Section


3.2.1. The stabilization section can be inerted either with nitrogen (preferable) or with
steam. The choice must take into consideration the effect of water on
downstream units (if any).
3.2.2. The initial status of the stabilization is: isolated from the reaction section and
blind flanges on safety valves to flare, on PV2096 & PV2092 to fuel gas, and on
products to battery limits.
3.2.3. If inerting is performed with nitrogen the same process of depressurization /
pressurization applies
3.2.4. Once the O2 content is lower than 0.2%, remove the blinds on:
 Safety valves to flare.
 Fuel gas from LPG absorber drum D-71205
 Flare header.
 Fuel gas header.
 Products to battery limits.
3.2.5. If inerting is performed with LP steam:
3.2.5.1. Vent air from the high points and drain condensate from the low points.
3.2.5.2. Steam the column from the feed lines and through the reboilers. The
reboiler heaters should have some pilots in service to keep steam from
condensing.
3.2.5.3. Steam each drum separately. Continue steaming for one hour minimum
after steam appeared at all vents.
3.2.5.4. Remove the blinds as above.
3.2.5.5. Shut-off the steam and immediately pressure the section with fuel
gas or hydrogen to prevent vacuum as steam condenses. A dedicated
line is provided for this purpose, connected to the upper section of the
stabilizer. As the fuel gas is admitted, the system will cool down, and
condensate can be drained off. The column is now ready for charging with
naphtha

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CCR UNIT KRCIM 71200.06 REV.0

4. Reforming Section Start-Up


For the first startup (or any subsequent startup), the following products are required:
 Pure hydrogen gas (electrolytic).
 Desulfurized naphtha (free of water)

4.1. Stabilizer Startup on Total Reflux


4.1.1. If the stabilization section was inerted with steam it has been subsequently
pressurized with fuel gas. If the stabilization section was inerted with nitrogen,
purge nitrogen to vent or to flare, then pressurize with fuel gas.
4.1.2. Fill-up the bottom of the stabilizer C-71201 with desulfurized naphtha from
storage through:
 The start-up line 100-P-712099 to the suction of the separator bottom
pumps
 Start the separator bottom pump P-71201A/B.
 Then through the startup line, to the discharge of LPG absorber bottom
pump P-71204A/B.
 Through the stabilizer feed/bottom exchangers E-71208A/B/C/D.
 To the stabilizer C-71201.
Oil flow as follows: Storage→D-71100→P-71101→E-71103→C-71101→P-
71201→P-71204 outlet→ E-71208→C-71201
4.1.3. When controller LIC2011 of the stabilizer bottom indicates 80%, stop the
naphtha make-up and:
4.1.3.1. Establish a close loop around the stabilizer reboiler F-71205 through the
stabilizer reboiler pump P-71202A/B.
4.1.3.2. Set the flow at design conditions.
4.1.3.3. Start the stabilizer air cooler A-71202 with the manual louvers fully
opened.
4.1.3.4. Light the stabilizer reboiler F-71205 burners according to ignition
instructions and slowly warm up the column with 15-20˚C / h.
4.1.3.5. Pressure should stay around 0.600 to 0.700 MPa gauge. When the level
of the reflux drum D-71203 indicates 50%, start pump P-71203A/B and
send reflux to the column.
4.1.3.6. Operate stabilizer on total reflux

Note: After reforming feed oil is cut, lift tower pressure to 1.56MPa according to
normal process conditions, control operating temperature at 57°C / 224°C ( top/
bottom).

4.2. Pressurization of The Unit


4.2.1. Unit Status
After catalyst drying, the unit has been purged with nitrogen to be oxygen free,
(less than 0,2% vol.) and is now under a slight positive pressure.
Inlet temperatures of the reforming reactors are now about 250°C.

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4.2.2. Preparation
4.2.2.1. Nitrogen lift gas circuit is pressurized with nitrogen up to 0.350 MPa at
nitrogen lift gas compressor KO drum D-71307.
4.2.2.2. Regeneration circuit is pressurized with N2 up to 0.450 MPa at the suction
of the regeneration loop compressors K-71301.
4.2.2.3. N2 seal gas lines are commissioned
4.2.2.4. Pressurize the reaction and recontacting sections with pure hydrogen
(electrolytic H2). The resulting nitrogen in these sections is about 25 vol. %
which is favorable for a steadier catalyst circulation.
4.2.2.5. Set pressure controller of the separator drum D-71201 at 0.030 MPag
above the start-up pressure (0.35MPa), Increase the pressure of the
separator drum via the recycle compressor discharge.
4.2.2.6. Commission the split range pressure control PV2068C on the H 2 rich gas
compressor K-71202A/B suction
4.2.2.7. Check again all the flanges for leaks using an explosimeter, and all
interlocks related to catalyst circulation are made operational

4.2.3. Operation
4.2.3.1. Start one nitrogen lift gas compressor at 100% capacity, PIC3014 at
nitrogen compressor discharge set at design pressure, send N 2 to the inlet
of regeneration loop compressor K-71301A/B.
4.2.3.2. Start one regeneration loop compressor and increase capacity to 100%
(BIAS not in service). FIC3004 of the Burning gas is set at 80% of design
capacity (944 m3/h)
4.2.3.3. FIC3019 and 3009 of calcinations and oxychlorination gases are set in
auto mode at 80% of design capacity (87 m3/h)
4.2.3.4. Commission all oxygen analyzers. Remember that certain ranges have
been changed during catalyst drying and information to DCS inhibited.
4.2.3.5. Commission the regeneration dryer DR-71301
4.2.3.6. Start the H2 recycle compressor K-71201. Increase the capacity up to the
maximum allowed by manufacturer.
4.2.3.7. Commission the hydrogen purity on line analyzer AI2001
4.2.3.8. Start K-71202A/B at 50% capacity and bring the recontacting drum D-
71203 pressure to about 0.120 MPa g, recycling all the gas to the H 2 rich
gas KO Drum D-71207
4.2.3.9. All H2 users and lines to fuel gas are isolated, only FV3017 on reduction
gas, PDV3012 at the tube side outlet of E-71304 and the HV3003 at the
tube side outlet of E-71305 are closed but block valves are open.

4.3. Catalyst Heating-Up and Reduction (See DWG.ReductionCurve)


4.3.1. Objective
4.3.1.1. The aim of the reduction of the catalyst is to switch the catalyst metals
from oxidized to reduced forms in presence of Hydrogen.
4.3.1.2. During this reduction step, additional leak tests can be made when the
reaction section temperature is increased.
Caution: Some leaks of H2 may appear and could catch fire.

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4.3.2. Procedure
4.3.2.1. The pressure must be maintained by make-up of hydrogen or nitrogen.
Nitrogen content in the circulating gas must not exceed 30% vol.
4.3.2.2. Some water will be released from the catalyst. This water will be
collected in D-71201.
4.3.2.3. Light the burners of F-71201/202/203 and increase the temperatures at
the inlet of reactors up to 300°C at the rate of 25°C/h.
4.3.2.4. Switch-on H-71301/302/303, then increase the temperature at the heater
outlet TIC3001/3005/3006, up to 300°C at the rate of 40°C/h.
4.3.2.5. Set the flow H2 FIC3017 to reduction chamber at 80% of design capacity
(294m3/h) and PDIC3012 between reduction chamber outlet and first
reactor at 0.010 MPa.
4.3.2.6. Switch on H-71304 and increase its TIC3007 outlet temperature to
400°C at the rate of 40°C/h
4.3.2.7. When the temperature of 400°C is reached in the reactors, start catalyst
circulation first from the 3rd reactor lift pot D-71333 to the upper surge
drum D-71301, etc. Note however that either nitrogen or hydrogen will
be used depending on the lift pot (nitrogen for the third reactor lift pot
and regenerator lift pot).
4.3.2.8. Set the catalyst circulation flow at the maximum compatible with the P
in the reaction section.
4.3.2.9. Increase the temperature to 480°C at the reactors inlets and at the
reduction chamber D-71311 inlet at a rate of 25°C/h.
4.3.2.10. Maintain this temperature for a minimum of 12 hours until the total water
drained at the low points is lower than 0.2L/h.
4.3.2.11. Owing to the difficulty of sustaining a steady catalyst circulation when the
reaction section is under hydrogen (low DP in reactors), this step shall
be maintained long enough to ensure that the catalyst contained in the
upper and lower hoppers has been reduced.
4.3.2.12. After reduction of the total inventory of catalyst contained in the
regeneration system, the catalyst circulation rate is increased to fill the
lock hopper in about 3 hours.
4.3.2.13. Whenever possible it is recommended to stop the catalyst circulation
after a transfer from the upper surge drum to the lock hopper. The
reason for leaving an empty surge drum is explained in regeneration
start up
4.3.2.14. Decrease then temperatures at reactors and reduction chamber inlets
down to 360°C at the rate of 40°C/hour.
4.3.2.15. Stop catalyst circulation: isolate the manual catalyst tight valves under
the lower hoppers.
4.3.2.16. Close the remote operated ON/OFF valves on the catalyst pipes:
4.3.2.17. Between first lower hopper and lift pot UV3005
4.3.2.18. Between third reactor lower hopper and lift pot UV3013
4.3.2.19. Reduce gas flow of reducing chamber to 40% of design flow (147m 3/h)
4.3.2.20. Keep in service the N2 lift loop and the regeneration loop compressor at
75% capacity to burning oxychlorination and calcination beds with the 3
electrical heaters in service (300°C outlet temperature).

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The unit is now ready for oil in.


Note: During the reduction period the pressure indicated in the procedure must
be maintained in the reaction section, by H2 make-up and in the regeneration
section or N2 lift section, by N2 make-up.

5. Oil in
5.1. Integrated Start-up Scenarios
The aim of this paragraph is to give an overview of a combined pretreatment plus
reforming startup.
 The ideal situation to start a reforming is when a source of hydrogen of adequate
purity, independent from the unit is available. In this case the pretreatment unit will
be started with this hydrogen gas, and once the pretreatment effluent is on
specifications (with respect to sulphur nitrogen and water mainly) it will be fed to
the reforming unit.
 Generally, however, this is not the case. A batch of desulfurized naphtha will then
be used as start up feed for the reforming unit.
One possible way of starting a reforming unit when no external H 2 is available is as
shown in Fig. 16 at the end of chapter 6.5 “First startup of the unit”. The
desulfurized naphtha batch from the storage is used to start the reforming unit. As
soon as a steady and reliable amount of hydrogen is produced, the pretreater can
be started with raw naphtha. The off-specifications product is sent back to the raw
naphtha tank, until the hydrotreater splitter effluent is on specifications. Then it is
switched to the reforming unit. All possible precautions must be taken to ensure
this naphtha batch is free of water. It is recommended to store it in a fixed roof
blanketed tank and to thoroughly drain the tank bottom and the feed line.
 An alternate hydrotreatment plus reforming startup sequence is sometimes used
when dryness of the desulfurized naphtha is questionable.It consists of feeding the
desulfurized naphtha from storage to the hydrotreater stripper - through the
hydrotreater startup by pass in order to remove the water, if any, at the stripper
reflux drum. The stripper bottom effluent is sent back to the desulfurized naphtha
tank. When operators are satisfied with the water content (10 ppm wt) then the
stripper bottom can be switched to the reforming unit and the reforming unit started
with desulfurized dry naphtha to produce hydrogen.
 During the whole period of pretreatment startup (approximately 12 hours) it is
strongly recommended to operate the unit at low severity (see later on) in order to
minimize the impact, of possible upsets (sulphur, water content) on the catalyst

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5.2. Preparation and Feed Introduction

The specifications of the feed acceptable for the reformer start-up are:
 Feed with similar ASTM distillation as design feed. Impurities are according to
the following:

Poisons Max. level (wt) Source

Arsenic 1 ppb max Cracked Naphthas

Lead 5 ppb max Recycled slops

Copper < detection limit Corrosion

Mercury 5 ppb max Naphtha - condensates

Iron < detection limit Corrosion

Silicon < detection limit Additives (foaming)

Nickel < detection limit Corrosion

Chromium < detection limit Corrosion

Organic nitrogen 0.5 ppm max

Total sulfur 0.5 ppm max

Halogens 1 ppm max

Water and lower than 10 ppm


oxygenated products (start up only)

5.3. Oil Cut Check List


5.3.1. C-71201 is operating on total reflux, its pressure being maintained by H 2
injection if required.
5.3.2. Check that blinds have been removed: at separator bottom pump P-71202
(suction and discharge) and at LPG absorber pump P-71204.
5.3.3. K-71201 is operating at full capacity.
5.3.4. K-71202A/B is operating at 50% capacity.
5.3.5. PV2068 split range valves on H2 compressor suction KO drum are in service,
connected to flare and atmosphere part is blinded.
5.3.6. Catalyst circulation is stopped
5.3.7. The regeneration loop is in stand-by: electrical heaters are in service (300°C
outlet temperature), K-71301 in service (75% capacity), air injection is
carefully closed.(Close UV3015, UV3006 and UV3007)
5.3.8. The N2 lift gas compressor K-71302 is in operation.
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5.3.9. UV3005 & UV3013 valves on catalyst are also closed


5.3.10. Manual valves on all seal legs are closed.
5.3.11. Bed temperatures of the reactors are steady at 360°C in auto mode.
5.3.12. Outlet temperature of the reduction heater H-71304 is maintained at 360°C,
and the flow is about 80% of design capacity(294 m3/h)
5.3.13. Separator bottom pump P-71202 is commissioned and ready to start.
5.3.14. Air coolers (A-71201, 202, 203 and 204) fans are in service.
5.3.15. Cooling water is in service on all users.
5.3.16. PDIC3012 is set at 0.010 MPa.
5.3.17. All instruments of the recontcting section are commissioned. A last check of
all other instruments in the reaction section and nitrogen section is made.
5.3.18. Commission the moisture analyzer AI2002 on the recycle gas.
5.3.19. Prepare a batch of chlorine solution (2% vol. of chloriding agent in
hydrotreated naphtha).
5.3.20. Set chlorine injecting liquid level of chlorine injection tank T-71303 at
70%.Commission chlorine pump for injection in the feed.
5.3.21. Remove blinds from the feed filters.
5.3.22. Drain water from the feed filter and from the feed line to the inlet FV2006.

Note: During the oil in, when the water content of the recycle is within the range of
the analyzer and until the reaction section operating conditions are stabilized, the
water content in the recycle gas must be recorded every hour.

5.4. Feed Introduction

5.4.1. Feed is introduced in 10 minutes at 60% capacity, quickly enough to insure a


minimum flow on the fresh catalyst.
5.4.2. Stop the H2 rich gas make-up, if any.
5.4.3. As soon as the PV2068A to flare on the separator drum start opening,
increase the pressure at K-71202A/B discharge and bring the pressure up to
design conditions in recontacting drum .
5.4.4. The export gas PV2085, in auto mode, will at the beginning of the operation
send part of the H2 rich gas to preatreatment unit 71100 and/or to the flare
system. When the spill back PV2079 tends to close increase the capacity of
K-71202A/B, first to 75% then to 100%.
5.4.5. When liquid appears in D-71201, and the level is above 50%, start P-71201
and send the product to the recontacting section (LIC2002 in manual mode).
5.4.6. When liquid appears in D-71203 and the level is above 50%, start to feed D-
71205
5.4.7. When liquid appears in D-71205 and the level is above 50%, start P-71204
and feed, as smoothly as possible, the stabilizer column (FIC2015 in manual
mode), Commission stabilizer bottom LIC2011 cascaded to FIC2026 and
route the reformate to slop. Route the LPG to off spec. LPG

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5.5. Low Severity Operation At Reduced Capacity

The low severity operation allows lowering the water and hydrogen sulfide content in
the recycle gas, without damage to the catalyst. It also enables a check of the
operation of the catalyst circulation and to carry out the reduction of any fraction of
the catalyst which was at the very beginning in the regenerator, and has not been
contacted by H2 gas.
The low severity operation is characterized by:
 A higher than design H2/HC ratio (feed at 60% and recycle compressor at full
capacity).
 A pressure higher than normal.
 Temperatures which will be increased step by step as the water content in the
recycle drops.
 The low severity operation yields a gasoline with a relatively low RON. This
product can be routed to the gasoline pool when found suitable.
 During the different steps the water content of the recycle will be determined
by lab analysis until it falls within the range of the on line moisture analyzer

400˚C(752˚F) stage
1. Raise temperature at reactor inlet to 400°C at a rate of 20°C/h.
2. Check water content in the recycle by lab analysis. Whenever possible put
the moisture analyzer on. Cross-check results of both measurements.
3. Drain water at low points and D-71201
4. Initiate chlorination agent injection: starting rate 5 ppm wt of pure
component related to feed rate
5. Stabilize the unit conditions at 400°C

Caution:
From the moment when feed is introduced do not stop K-71201 since this
would favor a quick build up of coke on the catalyst. In an emergency shut
down of the recycle compressor, shut-off heaters and feed immediately (refer to
“Emergency shutdown”).

Step at 450°C (842°F)


1. When the unit is stabilized, increase the reactors inlet temperature to 450°C
at a rate of 25°C/h..
2. Keep this temperature as long as the water content in the recycle is higher
than 200 ppm vol..
3. The excess of H2 rich gas can be sent to fuel gas or flare and later on, when
the production and quality are sufficient, to the other downstream users.
4. Increase the H2 rich gas to H-71304 up to 100 % of design flow (367m 3/h),
and bring the reduction chamber inlet temperature to 430°C. Set HV3003 at
tube side outlet of hydrogen lift gas exchanger opening and PDV3012 at
tube side outlet of reduction exchanger set point at design value. When
flows are stabilized commission hydrogen purification unit M-71301, then
increase reduction chamber D-71311 inlet temperature to design value.

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Step at 460°C (860°F)


When water content in the recycle gas is lower than 200 ppm, increase the
temperature at the reactors inlet to 460°C in one hour. Stabilize the unit and
keep this temperature as long as the water content in the recycle is higher than
100 ppm vol.

Step at 470°C (878°F)


1. When the water content in the recycle gas is lower than 100 ppm vol., then
the reactors inlet temperature is increased to 470°C in one hour.
2. Stabilize the unit and keep this temperature as long as the water content in
the recycle is higher than 50 ppm vol.

Step at 480°C (896°F)


1. When the water content in the recycle gas is less than 50 ppm vol., the
reactors inlet temperature is increased to 480°C in one hour and this
temperature kept until the water content in the recycle is lower than 30 ppm.
2. Reduce chlorine injection to 2 ppm related to the feed.
3. Decrease the pressure at D-71201 down to 0.300 MPa g over a two hours
period.
4. Check that the two bias are operational, and that pressure in both
regeneration section and nitrogen lift loop decreases in parallel.

5.6. High Severity Operation

High severity at 60% capacity


1. Until now the unit has been operated at 60% capacity, with maximum
recycle and separator drum pressure higher than the normal operating one.
Each reactor inlet temperature has been raised to 480°C. The water content
in the recycle is lower than 30 ppm vol. Stop the injection of chlorine in the
feed.
2. Inlet temperature are now progressively increased at a rate of 3°C/h until
the recommended temperature for the startup feed at reduced capacity is
reached.
3. After each step of temperature increase, wait until the unit has stabilized
and measure the RON of the product. When the required RON is met, the
temperature profile is kept.
4. Lower the pressure of the D-71201, slowly, to its design figure (0.23Mpa), in
approximately two hours.
5. The expected RON figures for the operation at reduced capacity will be
provided by startup representative.

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High severity at nominal capacity


1. Increase the feed rate in increments of 10%. After each increment, raise the
temperature (2°C/h step) in order to maintain gasoline RON.
2. Allow the unit to stabilize before measuring the octane. A flow increase must
always be achieved prior to temperature increase.
3. The expected final temperature profiles for the design feed at normal
capacity is as follows:
∆T
1st Reactor in °C 122
2nd Reactor in °C 84
3rd Reactor in °C 68

 Start the catalyst circulation in order to perform the coking of the catalyst
contained in the regeneration system (See paragraph 2.5.3 above).
 At the end of the catalyst reduction phase, the upper surge drum has been left
empty. Hence the catalyst we will recover in the upper surge drum is representative
of the catalyst from the bottom of the 3rd reactor. Take sample of catalyst every day
in order to analyze carbon and chlorine contents. The regeneration will be started
when the coke level of the circulating catalyst reaches 3%.

6. Regeneration Start-up
Regeneration is started when the coke content of catalyst is higher than 3% wt. For the
first startup, the catalyst circulation only is already on stream. During routine operation,
situations may occur when the regeneration (and the catalyst circulation subsequently)
have been stopped. The sequence below describes the catalyst circulation and
regeneration startup.

6.1. Overall Sequence


The overall sequence is as follows:
6.1.1. The regeneration loop is first started under an atmosphere of nitrogen. The
regeneration compressor is started and flows to the first burning zone and
oxychlorination/calcination zones are controlled in auto mode. Caustic washing
is started simultaneously (caustic circulation pump, water make-up, etc.). Air
injection is kept closed although the air compressor is started.
6.1.2. Inlet temperatures to the burning and oxychlorination/calcination zones are set
through the electrical heaters.
6.1.3. The catalyst circulation is started according to the relevant procedure.
6.1.4. When coke content is sufficient to start the regeneration, circulation should be
stopped:
 To prevent a temperature run away and to better control and adjust the
regeneration parameters
 As circulation is in low rate, attrition of catalyst might take place
6.1.5. Air is introduced into the burning zone and controlled through the relevant O 2
analyzer. Temperatures are adjusted in the different burning zones.

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6.1.6. Resume catalyst circulation in black burning mode as soon as excess O 2 at the
2nd bed outlet is satisfactory
6.1.7. Change to normal burning mode as soon as Oxychlorination/Calcination zone
is free of coke
The detailed procedure is given below.

6.2. Regeneration General Procedure


6.2.1. Establish regeneration gas circulation
6.2.1.1. Pressurize regeneration section upto 0.2MPa. Start regeneration loop
compressor K-71301. Control gas flow at 75% of design capacity and
keep FV3004 under autocontrol mode. Start regeneration gas dryer DR-
71301.
6.2.1.2. Switch-on the burning, calcination and oxychlorination electrical heaters
H-71301/302/303, then increase the temperature at the heater outlet
TV3001-TV3005-TV3004 up to 300°C at the rate of 40°C/h and keep
under auto control mode.
6.2.1.3. Start K-71302 with full load.
6.2.1.4. Set pressure difference PDIC3002 the bias between the 1st reactor inlet
and the regeneration loop pressures at about 0.080 MPa
6.2.1.5. Check all procedures and interlocks under normal use.
6.2.1.6. Confirm N2 seal gas of first lower hopper D-71304 and N2 seal gas on
lower hopper D-71323 of final reactor are enabled (automation mode).

6.2.2. Preliminary Operations


6.2.2.1. Set FIC3010/3015 of N2 lift in auto mode at the recommended calculated
value. The two corresponding lift PDV's PDIC3006/3011 are kept close
in manual.
6.2.2.2. Check that PDIC3019 between 1st upper hopper and reduction chamber
is set at 0.015 MPa.
6.2.2.3. Set seal gas at lower hoppers N°1 and 4 in automatic mode.
6.2.2.4. Set FIC3012/3013 of H2 lift in auto mode at the recommended calculated
value. The corresponding lift PDV's PDIC3008/3009 are kept close in
manual.
6.2.2.5. Increase H-71301 outlet temperature up to 450°C at a rate of 50°C/h.
The scope being to reach ~ 410/415°C in the first catalyst bed at the
inlet TIC3001. Increase the calcinations and oxychlorination heaters
outlet temperatures to 530°C.
6.2.2.6. Start the washing water injection to the top tray of D-71306 at 4993 kg/h
and commission the LIC3001 to caustic sewer.
6.2.2.7. Prepare a solution of water and caustic soda (3% wt concentration) in
the bottom of D-71306, then commission the LIC3002 to caustic sewer
and set the fresh caustic solution flow at 33 kg/h. Water make-up should
too be started.
6.2.2.8. Start the caustic solution circulation at 5557 kg/h. Check that the ∆P at
the caustic injector is ~0.150 MPa. Put in service the pH analyzer to
control the circulating caustic solution.

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6.2.2.9. Adjust the trim cooler E-71303 outlet temperature as near as possible to
design conditions (42°C).
6.2.2.10. Both air injection FV3007/3002 (oxychlorination/calcination and burning
air) are closed, including the block valves, start-up the air compressor K-
71304 and set the discharge pressure at design value (0.88 MPa).
6.2.2.11. Put in service the air dryer DR-71302
6.2.2.12. Line up piping to be ready for air injection to the burning zone only.

6.2.3. Catalyst circulation startup and stabilization


6.2.3.1. When the temperature at the 1st burning zone inlet reaches 410/415°C,
the catalyst circulation can be started-up.
6.2.3.2. Make sure H2 reduction (flow rate and temperature) is in operation.
6.2.3.3. Set the flow H2 FIC3017 to reduction chamber at 80% of design capacity
(294 m3/h) and PDIC3012 between reduction chamber outlet and first
reactor at 0.010 MPa.
6.2.3.4. Switch on the reduction chamber electrical heater and increase its
TIC3007 outlet temperature to 400°C at the rate of 40°C/h
6.2.3.5. Open the manual special tight valve between the 1st upper hopper and
the reduction chamber. Check that ON/OFF remote operated valve
UV3011 is open.
6.2.3.6. Check the PDI3114 between the first lower hopper and first lift pot. Open
UV3005 under the regenerator.
6.2.3.7. Open the manual special tight valve under the last reactor. Check that
UV3013 is well open.
6.2.3.8. Open the manual special tight valves under the reactors R1 and R2
lower hoppers.
6.2.3.9. Start then the catalyst circulation, lift by lift, according to the initial
catalyst level in the upper surge drum and upper hoppers, by manually
opening slowly the PDV's on N2 and H2 lift gas (Refer to“Catalyst
circulation”).
6.2.3.10. Stabilize the circulation in manual until the levels in the upper hoppers
are steady. Set the catalyst circulation at about 25% of the design
capacity (100 kg/h). Then set the control in AUTO-CASCADE from LC to
PDC.
6.2.3.11. The level of catalyst increases in the upper surge drum D-71301 while it
decreases in the regenerator R-71301. When these levels reach the
transfer conditions, the automatic sequence of catalyst transfer from the
surge drum to the lock hopper and to the regenerator will be energized.
If for any reason the automatic sequence fails, this transfer shall be
performed manually (Refer to “Catalyst circulation” above) and the
defect of the sequence shall be found and cleared.

6.2.4. Regeneration startup


(Refer DWG.Loopcontrol)
The catalyst circulation is stopped, the burning bed is at about 410/415°C at
TIC3001, the washing drum D-71306 is in service, the air compressor K-71304
is in operation with its spillback PV3010A/B full open.

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When the coke content of the circulated catalyst reaches 3.0% wt the coke
burning can be started.

CAUTION: as the catalyst contained in the calcination / oxychlorination zone


has a coke content similar to the catalyst of the burning zone, the air coming
from FV3007 (before UV3016) will be routed through the blackburning/startup
line entirely to the burning zone and isolated to the calcination zone (the reason
is to avoid too high temperature in the calcination zone).

6.2.4.1. UV3016 air to 1st bed is open while UV3017 air to oxychlorination /
calcination is closed.
6.2.4.2. The air is slowly introduced through FV3007 (before UV3016) in order to
reach 0.4 vol.% of O2 in the flow to the burning zone (check analyzer
AIC3001 at the shell side inlet of E-71301).
6.2.4.3. At 410/415°C in the burning zone the combustion will start immediately
and all the oxygen will be consumed. Check the first burning bed
TDI3122A/B/C read by difference of TI indication at inlet and outlet of the
bed, which must not exceed 40°C. Then begin to inject air through
FV3002 in the second burning bed in order to reach ~ 0.2% vol. O2 at
the outlet (check relevant analyzer AIC3002 on line to the second
burning bed ).
6.2.4.4. Stabilize the conditions and then set in auto cascade these AIC3001 and
FIC3007 through HS3124 selector and the AIC3002 to FIC3002.
6.2.4.5. Resume catalyst circulation with 50–75 % design flow rate
6.2.4.6. Air can be switched from the 1st burning zone to the
oxychlorination/calcination zone only when the catalyst contained in the
oxychlorination/calcination zone has been replaced by regenerated
catalyst. The safe way is to change the air injection only when the
catalyst sampled in the first upper hopper has a coke level lower than
0,2% wt. For such a purpose the catalyst circulation can be increased up
to 75% (310 kg/h). Air switch is made by opening UV3017 to
oxychlorination/calcination and closing UV3016 to 1 st burning bed. After
stabilization of FIC3017 air injection will be cascaded to analyzer
AIC3004 on oxychlorination/calcination gas which will receive its set
point from analyzer AIC3001 on first burning bed inlet.
Notes:
 This period of replacement of the coked catalyst with regenerated
catalyst will take place after 8 to 10 hours of burning. In case of
temperature increase after the switch of the air injection to the
oxychlorination/calcination zone, return immediately to the previous
situation and wait another couple of hours before switching again air to
the oxychlorination/calcination zone.
 Check carefully the operation of the regeneration loop trim cooler E-
71303
 Check the operation of D-71306, caustic solution circulation, caustic
soda and water make-up, water injection. The gas effluent temperature
shall be maintained as low as possible.
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 The circulating caustic solution shall be analyzed, twice a day, for total
sodium concentration (to be kept higher than 3%) and the pH analyzer
AI3101 at caustic recycle pump suction, it shall remain higher than 8.5
(9.5 max.).
 Check the operation of the regeneration gas dryer and air dryer DR-
71301/302 (once per shift during startup period).
 Check that O2 content to the calcination zone stays between 4 to 6
vol.%. When the temperature in oxychlorination zone reaches 470°C,
the chlorination agent injection can be started. The amount to be injected
is calculated as follows:

target value %wt Cl on catalyst


wt% Cl- on spent catalyst
estimated losses during burning
Kg/h

(1.1 - Actual) + 0.2 x Catalyst circulat ion


Cl C = CHCl injection =
2
l/h 100 X 0.85 X 0.810 X 1.465

Cl C = CHCl Sp. gr.


2
Cl C = CHCl, wt fract ion of chlorine
2
Chlorine fixation rate

 This formula applies to ethylene trichloride. For other chlorination agent


use the characteristics in table hereunder.
 This flow will be set by pump stroke adjustment and cross checked by
the level decrease in the calibration gauge.

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CHARACTERISTICS OF CHLORINATION AGENT

NAME Formula MW Density % wt Cl

Methane trichloride CHCl3 119.5 1.483 89

Ethylene dichloride C2H2Cl2 97 1.218 73

Ethylene trichloride C2HCl3 131.5 1.464 81

Ethylene C2Cl4 166 1.623 86


tetrachloride

Ethane trichloride C2H3Cl3 133.5 1.325 80

Propylene trichloride C3H3Cl3 144.5 1.382 73

Propylene C3H2Cl4 180 1.537 79


tetrachloride

6.2.5. Final adjustments


The regeneration and catalyst circulation loops are now set in auto mode on all
controllers.

6.2.5.1. By raising PDIC3006 of the master lift (from regenerator to first reactor),
increase slowly the catalyst circulation. Check that the lift flows are set at
the recommended value.
 Adjust TIC3001 between 470-480°C.
 Adjust TIC3003 between 470-480°C.
 Adjust TIC3006 between 510-520°C.
 Adjust TIC3005 between 500-510°C.

6.2.5.2. Then the catalyst circulation shall be increased until the following values
are obtained:

1st burning zone:


470 °C inlet
< T° 480°C
<
535 °C outlet
< T° 545°C
<

2nd burning zone:


470 °C intlet
< T° 480°C
<
500 °C outlet
< T° 510°C
<

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Oxychlorination zone:
500 °C outlet
< T° 510°C
<

Calcination zone:
510°C outlet
< T° 520°C
<

6.2.5.3. The oxygen analyzer controllers shall be in the following range:

O2 content at first burning zone inlet: 0.5 to 0.7 % vol.


O2 content at second burning zone outlet: approximately
0.25 % vol.
O2 content at calcination zone inlet: 4.0 to 6.0 % vol.

6.2.5.4. Take catalyst samples from the 1st upper hopper D-71310 to control coke
and chlorine content on the regenerated catalyst.
The chlorination agent injection is adjusted in proportion to the catalyst
circulation and to the chlorine level of the spent catalyst contained in the
upper surge drum D-71301 (refer to injection rate formula).

6.2.5.5. Check regularly the satisfactory operation of the dryers as well as all
washing drum parameters.

6.2.5.6. The field operators shall regularly perform the following operations:
 Drain the analyzer upstream KO pots. Check and if necessary correct the
sampling flow rates.
 Drain the dryers upstream KO pot.
 Drain the loop compressor K-71301 suction bottles.
 Check NaOH injection rate (pump strokes and tank level).
 Check chlorination agent injection rate (pump strokes and tank level).
 They must report to the shift foreman for any deviation.

During the increase of temperature, the thermal expansion of the reactor internals will
tend to increase the quantity of catalyst contained in the reactors and consequently
will tend to decrease the quantity of catalyst in the circulation loop. The level of the 1st
upper hopper D-71310 will have to be set at a lower value to compensate for this
"loss". Conversely when temperatures are reduced the upper hoppers will operate at a
higher catalyst level.

7. Unit Restart
7.1. Restart Of The Entire Unit
(including regeneration section)
7.1.1. Any unit restart procedure derives from the first startup procedure. The only
difference results from the unit status after the shutdown which dictates the
point where the general startup procedure can be resumed.

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7.1.2. For instance, assume a shutdown of the feed pump P-71102A/B of a short
duration: the unit will be kept on stand-by with the recycle compressor K-71201
running, the heater still on, the reactor temperature lowered, Recontacting
section blocked, the H2 rich gas compressor K-71202A/B stopped and possibly
(depending upon the expected duration) the regeneration loop and catalyst

circulation stopped. In this specific case operator will have to resume the first startup at
paragraph " Preparation and feed introduction ", including, if required, the restart of the
regeneration section.

7.1.3. More generally, in most cases of normal or emergency shutdowns of relatively


long duration, the stand-by conditions are as follows:
 Feed and heaters are shut down, catalyst circulation and regeneration
sections are stopped. The reaction section is isolated from the recontacting
section and cooled down under an atmosphere of hydrogen.
 Recycle compressor is stopped and isolated under nitrogen. The H2 rich gas
compressor is shut down and isolated.
 The stabilization section is isolated from the recontacting section. Both are
under an atmosphere of hydrogen or fuel gas.

Then, the restart procedure will be resumed at stabilizer total reflux (“Stabilizer
startup on total reflux”) or catalyst heating up and reduction (“Catalyst heating
up and reduction”). However the reduction step of 12 hours at 480°C for water
removal is not required.
Also the feed can be introduced again at a temperature of 425°C, no need for
steps at 360°C and 400°C (no or very little water is expected).

7.1.4. Note also that the unit shutdown results (in the general case where no
independent H2 supply is available) in the shutdown of pretreatment unit 71100.
The unit will be restarted with desulfurized dry naphtha.

7.1.5. An extreme case of unit restart is when the catalyst has been regenerated, or
the reaction section was aerated (for inspection), in this case the restart
procedure will start all over again from the beginning i.e. leak test and partial
inerting (“Second leak test and partial inerting”), catalyst circulation heating and
drying (“Catalyst circulation procedure and principle of catalyst transportation”)
until oil in (“Preparation and feed introduction”).

7.2. Restart Of The Regeneration Section Alone


7.2.1. After a partial shutdown
In some cases of operating problems which affect the regeneration section
only, and it is expected to be corrected in a couple of days, the regeneration
section alone plus the catalysts lifts may be partially shut down. This
means that the regeneration section is isolated from the reaction section, air to
burning zones cut off, but regeneration and air compressors may still be
running.

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Then the restart procedure is as follows:


7.2.1.1. Make sure that the shutdown sequence was correct i.e. the circulation of
catalyst has been stopped first and air to burning zone and
oxychlorination/calcination after. If yes, proceed with next steps.
7.2.1.2. Start the regeneration loop compressor K-71301 - if required - control
flow in manual mode through spillback FV3004, switch to auto.
7.2.1.3. Adjust flows to the burning beds, to oxychlorination and calcination
7.2.1.4. Adjust PDV3003 A and B respectively between 2nd burning bed and
oxychlorination outlet.
7.2.1.5. Set PDIC3002 bias between first reactor top and regeneration loop
pressure at 0.080 MPa - if required i.e. if compressor K-71301 has to be
restarted.
7.2.1.6. Start the air compressor K-71304 if required.
7.2.1.7. Check O2 analyzers are ready for use.
7.2.1.8. Set TIC3001 at burning gas heater outlet at 480°C.
7.2.1.9. Set TIC3006 at calcination heater outlet at 520°C.
7.2.1.10. Set TIC3003 at second bed inlet at 480°C.
7.2.1.11. Set TIC3005 at oxychlorination heater outlet at 510°C.
7.2.1.12. Check that first burning zone inlet temperature is approximately 520°C.
7.2.1.13. Make sure that the caustic recycle pump P-71302A/B, the water injection
pump P-71305A/B and the washing system operate satisfactorily.
7.2.1.14. Open the 2 FVs air valves 3002 and 3007 and adjust set points to the
previous ones.
7.2.1.15. Switch on cascades between oxygen analyzers and FVs when the
required O2 content has been reached (Refer to Fig. 19 : Principle of
regeneration loop control in paragraph “Regeneration startup”).
7.2.1.16. Open ON/OFF remote operated valve UV3005 on regenerator bottom
pipe.
7.2.1.17. Start the catalyst lifts. First from last reactor to regenerator, etc. (See
“Catalyst circulation”).
7.2.1.18. Set PDIC3011 on the lift from the last reactor to the regenerator at its
design figure.
7.2.1.19. When T in the first burning zone increases adjust burning heater outlet
temperature at 470°C.
7.2.1.20. When the oxychlorination zone reaches 450°C start water and chlorine
injection.
7.2.1.21. Adjust TIC3011 set point, at burning heater H-71301 outlet, to maintain
the inlet temperature to the first burning zone between 470 and 480°C.
2nd bed inlet temperature must be around 480°C.
If at the previous shutdown the air injection was stopped prior to
stopping the catalyst circulation, some coked catalyst has entered the
calcination zone. Special caution must be taken at restart: At the beginning
air must be directed exclusively to the burning zone and none to the calcination
zone, i.e. UV3016 is closed to oxychlorination / calcination zones and UV3017
is open to 1st burning bed. Only when the catalyst contained in the
calcination/oxychlorination zone has been replaced with catalyst from the
burning zone can air be directed to the calcination zone again (Refer
“Regeneration startup”).
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PRODUCTION & OPERATION START-UP OPERATIONS (2)
CCR UNIT KRCIM 71200.06 REV.0

7.2.2. Restart after a total shutdown of the regeneration section


If the regeneration section has been fully shut down: Either alone,
Or as a result of a shutdown of the entire unit .
Then operators must refer:
Either to Regeneration start up (paragraph “Regeneration startup”).
Or to Oil in (paragraph “Preparation and feed introduction”).

IMPORTANT:
Under normal steady conditions and design feeds the unit typically operates with a
coke content on the catalyst between 4 to 6% wt (Refer to “Regeneration”).
However, the reforming unit can be maintained on stream without the
regeneration section for some period of time.
In this case, the limiting factor being the coke deposit, the lower the severity, the
longer this period. It is then recommended to reduce reactors inlet temperatures to
approximately 480°C and flow to approximately 60% with maximum recycle rate, in
order not to significantly exceed the 6% wt coke deposit. The period without
regeneration might then last up to two weeks.
However, regeneration with coke deposit higher than 6% wt. have been carried out. In
this case, operators must bear in mind that the coke burning capacity (Kg/h) of the
unit is limited.

Consequently upon restart of the regeneration they must adjust the catalyst circulation
rate taking account of:
a) the maximum coke burning capacity
b) the actual wt% coke deposit
Moreover, they must carefully watch the temperature increase in the burning zones.

Example: Coke burning capacity 80 Kg/h


Actual coke deposit 10% wt
Maximum catalyst circulation. Qcata (Kg/h)
Qcata = 80 x 100
10 : 800 Kg/h

It is recommended to start with a lower circulation rate (say 80% of the maximum rate)
and increase progressively, according to the temperature increase in burning beds.

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8. Supplements

 Figure 8 (Catalyst Circulation – 3 Reactors)

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CCR UNIT KRCIM 71200.06 REV.0

 Figure 9 (Reactor- Gas Circulation)

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CCR UNIT KRCIM 71200.06 REV.0

 Figure 10 (Regenerator – Gas Circulation)

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CCR UNIT KRCIM 71200.06 REV.0

 Figure 11 (Catalyst Flow Control)

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CCR UNIT KRCIM 71200.06 REV.0

 Figure 12 (N2 Circulation & Seal Gas – 3 Reactors)

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CCR UNIT KRCIM 71200.06 REV.0

 Figure 13 (Seal Gas System)

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CCR UNIT KRCIM 71200.06 REV.0

 Figure 14 (Reduction – 3 Reactors)

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CCR UNIT KRCIM 71200.06 REV.0

 DWG.InitialStatus

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CCR UNIT KRCIM 71200.06 REV.0

 DWG.ReductionCurve

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CCR UNIT KRCIM 71200.06 REV.0

 DWG.LoopControl

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CCR UNIT KRCIM 71200.06 REV.0

 Oil In Scheme

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PRODUCTION & OPERATION FURNACES OPERATION
CCR UNIT KRCIM 71200.07 REV.0

Contents: This instruction outlines the operation of the CCR heating furnaces. The text
includes:

1. Dryout General Instructions


2. Start-up Procedure
3. Daily Operation Of Heating Furnaces
4. Troubleshooting
5. Shutdown

1. Dryout General Instructions


1.1. Activities For Drying Out
List the required instruments and inspect whether these instruments have been
connected and put into use. All thermocouples including field and DCS display
should be complete and available; orifice plates should be installed at the locations
needing normal checkout.
1.1.1. Inspect the burners, flue damper, safety interlock system, etc. of heating
furnace; all should be complete and on standby status. The drying gas should
have been introduced into the unit.
1.1.2. Inspect to be sure that all safety valves have been installed and lined up to
atmosphere.
1.1.3. Verify that all external and internal inspections have been completed.
1.1.4. Prepare ignition appliances.
1.1.5. Prepare the furnace drying and heating up curve of furnace
1.1.6. Prepare furnace drying record. During furnace drying, the primary
temperature should be recorded each hour, and the actual furnace drying
curve should be plotted in time.
1.1.7. Organize operation personnel to study this scheme and master it skillfully
before furnace drying.
1.1.8. The fire holes, flue dampers, and explosion doors of furnace should be
opened before furnace drying for natural ventilation.
1.1.9. Blow-down condense drains on atomizing and steam snuffing lines. Check
damper for open position and remove fuel blinds which protected the fuel
lines.
1.1.10. The flow of cooling fluid, especially through the convection section, should not
be too large or flue gas will be wet and so the furnace refractory.
1.1.11. Additional pilot burners and burners should be ignited according to furnace
drying temperature curve so that the ignited pilot burners and burners can be
distributed on the entire heating furnace uniformly as possible.
1.1.12. During furnace drying, it is unnecessary to ignite all burners, therefore, every
4h switch between burners to allow all burners attend furnace drying.
1.1.13. The burners should be operated with a large amount of excess air in order to
maintain low flame burst temperature and to carry the generated moisture
from the combustion chamber to the atmosphere.
1.1.14. Normally, drying out according to drying curve will turn the refractories dry
enough to be placed in operation. However, the most accurate indication of
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CCR UNIT KRCIM 71200.07 REV.0

readiness of a furnace for operation is the shell temperature. When the fires
are started in a new furnace the moisture of the outer surface of the refractory
evaporates into gases but much of the moisture held deeper in the refractory
is driven back into the insulation next to the shell. During this period the
furnace shell remains cold. Then, as heat density in the combustion chamber
is increased the lining heats through and the moisture from the insulation
begins to evaporate. This causes the furnace shell to heat up by the
generation of steam on the adjacent insulation. However when this moisture
has been throughly evaporated, the shell temperature will gall again. If the
operator keeps some progressive account of the shell temperature, he will
note this rise and fall during the drying out process and when the shell
temperature has decreased to the rated casing temperature the furnace can
be considered ready for operation.

1.2. Safety Considerations


1.2.1. Verfify that proper fire fighting equipment and fire extinguishers are present
and operational.
1.2.2. Clean up the ground in the furnace area and move the combustible and
explosive materials away
1.2.3. All personnel, not associated with the dry-out, should keep free of the heater
area. All hot work should be stopped in the heater area.
1.2.4. Before introducing gas into unit, isolation work should be done to prevent gas
from flowing into other positions. Burner gas valve should be closed tightly to
avoid gas from flowing into furnace hearth, which can cause explosion during
ignition.
1.2.5. After introducing gas, the condensed liquid in the gas knock-out drum is not
allowed to discharge into drain and disorderly discharging is strictly
prohibited.
1.2.6. Purge the heater of combustible gases before lighting burners during 15
minutes.If system has fans purge with fans.
1.2.7. During ignition, furnace hearth purging must be done according to
regulations, then, analyze the explosive gas to be up-to-standard, and then
ignite.
1.2.8. Any person is not allowed to stand on furnace top or platform during ignition.
1.2.9. Rise and reduce temperature according to heatingup and cooling curve for
furnace drying strictly.
1.2.10. Constant temperature time must be guaranteed; temperature must be
controlled steadily with fluctuation controlled within ±5℃.
1.2.11. Direct contact of flame directly to furnace tube should be avoided;
overtemperature of pipe wall and furnace tube outlet is strictly prohibited.
1.2.12. Burner air, and flue damper should be adjusted slowly. Too fast adjustment
will cause excessive fluctuation of negative pressure in furnace hearth.
1.2.13. During ignition, not to observe underneath the lightening hole; during
inspection, the body should deviate from the fire hole to avoid backfire hurting
persons.
1.2.14. Inspect the fuel gas often to see whether it takes liquid, and use fuel gas
heater if necessary.

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1.2.15. If temperature measurement instrument fails, not to continue in heating up,


instrument personnel should be contacted for inspection and treatment;
fluctuating operation should be controlled manually.
1.2.16. The fire apparatus and fire fighting steam rubber hose in the furnace area
must be arranged completely and can be used easily.

1.3. System Treatment After Drying Operation Of Furnace Drying


After furnace drying finishes, inspection should be made and repairing to the
positions with cracked linings or possible crack positions.
1.3.1. If lining crack width is smaller than 3mm and does not run through the fire-
proof coating, it is unnecessary to repair it. If the crack width is equal to or
bigger than 3mm and smaller than 1m in length, furthermore, there is no
possibility of further cracking. Prepare fiber mud with bauxite cement (500#)
and fiber cotton in proportion of 30:70 (wt) for filling.
1.3.2. When the crack depth on lining surface exceeds 15mm or cracking depth
reaches 1/5 of fire-proof coating thickness, it is necessary to repair.
1.3.3. Inspection of fiber lining.
1.3.3.1. Observe to see if there is damage or loosening and cracking positions.
1.3.3.2. Investigate whether the combined parts between fibers comply with
requirements.
1.3.4. During furnace drying, implement patrol inspection, monitor the thermal
expansion situation of furnace tubes, furnace body and furnace inlet and
outlet pipelines strictly; any abnormal deflections found should be recorded
and reported in time.
1.3.5. After system drying and dewatering, it should be guaranteed that the system
is under slight positive pressure status with system pressure kept at least
0.05MPa to avoid the outside wet air from entering the system.
1.3.6. After the unit has been dried-out it is important to prevent entrance of
excessive moisture into the furnace. Close tightly the stack damper access
and peep doors and all burner registers. If the heater is to be shut-down for
an extended period before initial start-up and the stack has no rainhood,
provide a canvas stack cover to eliminate rain water infiltration. The longer a
furnace is inoperative, the more moisture is taken up by the refractory and
insulation due to atmospheric exposure.
1.3.7. Handle other problems in furnace drying process

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CCR UNIT KRCIM 71200.07 REV.0

2. Start-up Procedure
2.1. System Purge, Pressure Test, Hearth Sweeping
2.1.1. Fuel system purge pressure test
After checking, conduct steam blowing downstream PV4303. Before purging,
disconnect flanges on every main and pilot burner gas line. Remove flame
arrester. Meanwhile, gas knock-out drum D-71401 pressure shall not exceed
0.4MPa controlled by PV4303. After purging is over, connect nitrogen at main
gas drain point to evacuate water in the system.
2.1.2. Hearth sweeping
F-71101.71102.71205 Use air blower to purge, open all main burner throttles.
Purge for 15 minutes above.
2.1.3. Flue gas duct test
Contact instrument to regulate and test F-71101, 71102, 71205, 71201, 71202,
71203 flue dampers and solenoid valves and ensure good condition (flexible
and not jamed).

2.2. Lead-In Fuel Gas


2.2.1. Close gas boundary gate valve, remove boundary blind plate, open E-71401
shell side inlet and outlet valves. Line-up system to D-71401.
2.2.2. Slowly open gas boundary valve, lead system gas into D-71401, enable
PV4303 to control drum pressure within process sheet range ( 0.27±0.03MPa).
2.2.3. Properly, enable E-71401 heating steam, control D-71401 gas temperature
within 70- 100˚C.
2.2.4. Discharge from D-71401 bottom oil to flare drum. Replace N2 with fuel gas,
control D-71401 pressure at 0.275MPa. (Ensure N2 less than 5%)
2.2.5. Perform furnace explosion gas analysis.
After gas component analysis at two points is qualified( oxygen content not to
exceed 0.2%), open D-71401 top and lead gas to every furnace valve waiting
for ignition.

2.3. Three In One Furnace (F-71201.F-71202.F-71203) Ignition Operation


2.3.1. Completely open burner baffle and flue damper, lead extinguishing steam for
hearth purging, open purging steam to purge hearth for 20 - 30 minutes.
2.3.2. Manually, open solenoid valve of main gas and pilot gas, slightly open
isolation valves of flame arresters, contact panel operator to open burner
control valve 15% - 20%, lead gas to two manual valves of main burner and
pilot burner. Check leakage at metal hose installed and in case of valve leak,
timely stop gas and replace valve. If no leakage, timely connect metal hose.
2.3.3. Close air damper, close flue damper to 1/3. Hearth negative pressure is
controlled at -0.035KPa to prevent extinguishment due to air. Close pilot
burner register.
2.3.4. Light a portable torch
2.3.5. Insert the torch through the ignition port on the first pilot burner and ensure
that the torch burner flame remains stable.
2.3.6. Fix the torch on the pilot burner and leave furnace bottom.
2.3.7. With the pilot burner register half-open, ignite pilot burner (slowly open pilot
gas valve)

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2.3.8. Ensure that a stable pilot flame has been established before removing the
torch burner.
2.3.9. Check pilot gas pressure downstream of the pressure regulator
2.3.10. If the burner fails to light within 10 seconds, promptly close the gas valve and
repeat the operation starting from steam purging
2.3.11. When checking flame through flame window, operator must stand beside
flame window. Looking to fire flame, must wear special fire glass.
2.3.12. Before lighting main fuel gas burners it is necessary to circulate a cooling
medium through the heater tubes to prevent local and general overheating.
2.3.13. With the primary and secondary air registers half open, slowly open (1/3) the
first fuel gas gate valve to the first main gas burner
2.3.14. Check main burner is ignited through fire window; regulate the flame through
the globe valve. Fully open manual valve and regulate burner air register.
2.3.15. If the gas burner fails to ignite with in 10 seconds, promptly close the gas
valve and repeat the operation starting from steam purging.
2.3.16. Symmetrically ignite another burner.
2.3.17. Main burner must be ignited by light pilot burner
2.3.18. After igniting all burners as above, conduct overall check on furnace.
2.3.19. Ensure heating furnace under normal burning, turn furnace solenoid valve to
automatic position and conduct stability test of pilot burner and main burner.
2.3.20. After ignition and heat up of heating furnace, when furnace outlet temperature
reaches and stabilize at normal operation value, can switch from manual
control to cascade control.

2.4. Cylindrical Furnace Ignition Operation


2.4.1. Start induced fan and ventilator, use air damper to regulate F-71101, 71205,
71102 furnace air quantity as maximum. Use flue damper regulating valve to
regulate F-71101, 71205 and 71102 flue damper opening as 1/2
2.4.2. Manually, open solenoid valve of main burner and pilot burner.
2.4.3. Slightly open flame arresters isolation valves
2.4.4. Contact panel operator to open burner control valve 15% - 20% and lead gas
to two manual valves of main burner and light pilot burner. Check leak at
metal hose installed. In case of valve leaking, timely stop gas and replace
valve. If no leakage, take out pilot burner gun.
2.4.4.1. Use air regulation valve to regulate F-71101, 71205 and 71102 furnace air
quantity opening at 20%.
2.4.5. Use flue damper regulating valve to regulate F-71101, 71205 and 71102
negative pressure as -0.15KPa.
2.4.6. Ignite pilot burner, then insert into furnace
2.4.7. Regulate air door and stabilize pilot burner flame.
2.4.8. If the burner fails to light within 10 seconds, promptly close the gas valve and
repeat the operation starting from steam purging
2.4.9. Confirm pilot burner is ignited and replace it back
2.4.10. Slowly open corresponding fuel gas valve and ignite main burner.
2.4.11. Stablize burning for 1 minute, then regulate air door and gas burner valve to
ensure normal burning.
2.4.12. Symmetrically ignite another burner.

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2.4.13. Ensure heating furnace under normal burning, turn furnace solenoid valve to
automatic position and conduct stability test of pilot burner and main burner.
2.4.14. After ignition and heat up of heating furnace, when furnace outlet temperature
reaches and stabilize at normal operation value, can switch from manual
control to cascade control.

3. Daily Operation Of Heating Furnaces


3.1. General
3.1.1. Three in one box heater shall adopt natural ventilation process. Inlet air is
regulated by air baffle and flue damper. Flue damper's function is to regulate
furnace pressure. It will widely open with the increase of furnace load. If air
baffle opening is small it will lead to small air suction, air quantity insufficient,
incomplete burning, hearth shading, and flame color become dark red. Too
small baffle opening will cause hearth positive pressure and flame turbulence.
Incase damper is opened widely, furnace air quantity will be in excess, leading
to a large thermal loss, low thermal efficiency low and a colorless hearth. Baffle
opening too large will cause burner extinguishing. Ensure frequent and careful
check, analysis, and regulation on heating furnace. Strictly control the
fluctuation of furnace outlet temperature at± 3˚C.
3.1.2. Cylindrical furnace is forced ventilation heating furnace realized through blower
and induced fan. One solenoid valve separately set at the inlet of two fans to
regulate air output of blower and negative pressure value from induced fan inlet
to the top of every furnace's convection chamber. A butterfly valve separately
set at air inlet of every furnace to individually control air quantity into every
furnace. The flue dampers on every furnace roof separately regulate hearth
pressure of every furnace.

3.2. Daily Inspection Of Heating Furnace


3.2.1. Check burners flame and gas leak,
3.2.2. Drain D-71401 bottom liquid
3.2.3. Local instrumentation display and DCS indication comparison,
3.2.4. Gas alarms operability
3.2.5. Appearance of furnace tubes, fans, fire fighting devices and hearth inner wall
3.2.6. Check whether fire equipment complete, ensure safekeeping
3.2.7. Person on duty shall indicate furnace status on log book. Furnace is considered
in normal operation if complete burning is taking place, hearth is bright, furnace
tubes or furnace wall are not directly exposed to flame (No overheat points and
deformations) and flue gas out of stack is colorless or slight blue.
3.2.8. During normal operation record data daily for the following:
 Inlet/outlet temperature and pressure of the process fluid
 Flow rates of the process fluid.
 Temperatures of the flue gas at the top of the radiant chamber.
 Tube skin temperatures
 Chamber pressure (draft) at the top of the radiant chamber (regulate
according to O2 content analysis).

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CCR UNIT KRCIM 71200.07 REV.0

4. Troubleshooting

Serial Trouble Possible Cause Remedial Action


no.
1 Flame Burner position not correct. Stop or temporarily extinguish burner and allign.
contact Combustion air insufficient, flame Regulate furnace air quantity, make burning
furnace tube weak. normal.
Burner air hole and nozzle erosion and Replace burner in case of break-down
deformation. maintenance.
2 Incomplete When heating furnace burns under the Firstly reduce gas rate.
combustion condition of insufficient air, stack gas Then slowly open burner throttle, lead-in more air.
will have higher CO, in this way, Once incomplete stops, and no CO inside heating
incomplete combustion may occur on furnace, can increase gas rate and regulate
the bottom even on top of stack. furnace air quantity so as to guarantee normal
combustion.
3 Media flow Feed pump evacuation Heating furnace tube internal flow reduction or
reduced Compressor trips interrupt will cause too high hearth temperature
inside Meter displays dummy flow and furnace tube superheated. Immediately reduce
furnace tube gas quantity or adopt emergency blowing out
measures according to actual situations
Check and fix flow meters readings
4 Fuel gas Fuel gas pressure reduction, and Contact dispatch immediately, clarify cause, if
interrupt burner hard to maintain normal pressure fails to be lifted, immediately blowout;
combustion
5 Fuel gas Heavy draft inside heating furnace. Firstly close burner gas, open flue damper and
burner Fuel gas pressure with acute change. blow steam into furnace for 20 minutes. Then ignite
extinguish Condensed fluid accumulated inside burner as per lighting up procedure, and according
fuel gas pipeline. to the cause of burner extinguish, regulate furnace
draft, Stabilize gas pressure, thoroughly preheat
gas line, purge to remove accumulated liquid.
6 Flame profile Oversize long and irregular flame. Properly reduce gas rate.
abnormal Burner nozzle choking Blowing out and burner treatment.
Ventilation quantity oversize, flame Regulate flue damper, reduce suction.
flickers, flash, even cause small Adjust air
explosion Adjust air
Too clear and bright (Too much air)
Red and Wavy (Lack of air)

7 Flame Excess furnace load, flue damper Reduce fuel gas quantity & Regulate air door or flue
pulsation opening small, suction small damper.
Fuel gas pressure unsteady or containCheck pipe network or unit generated gas, and
liquid conduct pressure stabilization regulation
accordingly.
8 Unstable Fuel gas pressure change or fuel gas Stabilize fuel gas pressure
furnace with oil According to furnace load, burning status,
outlet Burning influencing factors change determine the number of burners to be ignited, the
temperature (Ex: Climate, load etc..) height of whole flame shall not exceed two-third of
Instrument auto control failure hearth height, every part of hearth shall be heated
Hearth temperature change uniformly
Inspect and adjust auto control of furnace
Make adjustments according to feed flow rate when
feed temperature changes. In case of larger
change, can regulate outlet temperature as above-
mentioned 1-2 minute in advance

9 Tube coking Flame uneven, making temperature Retain uniform hearth temperature
inside hearth uneven, causing local Retain stable feed, timely burnout in case of feed
overheating interrupt and insure uniform feed rate in every loop
Feed rate changed too large or Regulate flame, ensure more burners, uniform
stopped suddenly flame, short burning flame, hearth bright, flame
Flame deflects to furnace tube, cause vertical, not burn furnace tube, not generate local
local overheating overheating area

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CCR UNIT KRCIM 71200.07 REV.0

4.1. Air Regulation

Heating furnace status Regulation method


High O2 and high negative Turn down flue damper
pressure
Low O2 and low negative Open wide flue damper
pressure
High O2 and low negative Turn down burner air register
pressure
Low O2 and high negative Open wide burner air register
pressure

5. Shutdown
5.1. Normal Shut-Down Of Heating Furnace
5.1.1. General Precautions
During controlled shutdown or in an emergency, the following dangerous
conditions must be avoided:
 Fuel gas entering the combustion chamber when all fires are off as,
explosions may occur.
 The presence of heavy hydrocarbons at low velocity in the coils. This can
lead to coke deposition.
 Thermal shock due to a rapid cool-down.
 Either a positive pressure in the combustion chamber or too high a vacuum.
Either condition can cause refractory cracking.

5.1.2. General Procedure


5.1.2.1. Deactivate the furnace interlock. Strictly control cooling rate according to
shutdown scheme; properly close flue damper according to flame status.
5.1.2.2. With reduction of heating furnace temperature, properly and gradually
extinguish partial burners, meanwhile ensure symmetry burner extinguish.
5.1.2.3. For dead burner, immediately close two manual valves, pilot burner
remains on.
5.1.2.4. Guarantee normal combustion of heating furnace.
5.1.2.5. When furnace outlet temperature less than 200˚C, can stop heating
furnace, meanwhile close solenoid valve of main burner and pilot burner,
isolation valves of flame arrester and control valve as well as two manual
valves of every burner; remove all metal hoses of main burners and pilot
burners.
5.1.2.6. In case the fuel gas system in the unit not shutdown, install blind plates at
fuel gas control valve and its bypass in addition to blinds before flame
arrestors in pilot gas line.
5.1.2.7. When all of heating furnaces burnout, close fuel gas boundary valve.
5.1.2.8. Add blind plate at fuel gas boundary valve in case of long-term blowing
out, and open wide flue dampers and air doors.

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CCR UNIT KRCIM 71200.07 REV.0

5.2. Emergency Shutdown operation


5.2.1. If process fluid interrupts, heating furnace main burner will interlock and
extinguish, after interlock, immediately close solenoid valve, control valve and
burner globe valve. Properly extinguish partial pilot burners according to
temperature inside hearth, guarantee at least one flame inside hearth.
5.2.2. When gas tank pressure is too low and reach interlock value, main burner and
pilot burner of heating furnace will extinguish, by this time, no naked flame
inside heating furnace. Urgently blow fire steam into box furnace, for not less
than 20 minutes. Fully open flue and air dampers
5.2.3. In case of emergency shutdown due to furnace tube rupture, immediately cut
off the source of flammable process fluid inside furnace tube, extinguish main
and auxiliary burner, blow extinguish steam into hearth

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

Contents: This instruction outlines the operating conditions and control of the reforming
section. The text includes:
1. Operation Influencing Parameters
2. Principles Of Key Parameters Control
3. Adjustment Of Operating Conditions
4. Troubleshooting
5. Operation Conventional Control
6. Analysis Control
7. Supplements

1. Operation Influencing Parameters


1.1. Reaction Temperature
Temperature, together with space velocity (see hereafter) is the most important and
most used operating parameter.
By simply raising or lowering reactor inlet temperatures, operators can raise or lower
the octane number of the product.
Since all reactor inlet temperatures are not necessarily identical, it is commonly
accepted to consider the weight average inlet temperature (WAIT) as representative
of the reactor temperatures.
The WAIT is defined as follows:

wt of catalyst R1 x Ti1 + wt Catalyst R2  x Ti2....+ wt Catalyst R4  x Ti4


WAIT =
Total wt of catalyst
Ti1, Ti2, ... Ti4 are inlet temperatures to reactors R1, R2...
(wt of catalyst R1) are the weight of catalyst in reactors R1, R2...

An increase of temperature (i.e. WAIT) have the following effects, assuming the
space velocity (i.e. the feed rate) and feed characteristics stay unchanged:
 Increases octane.
 Decreases the yield (of C5+ fraction).
 Decreases the H2 purity.
 Increases the coke deposit.

At constant WAIT, the ageing of the catalyst (caused by the numerous


regenerations, the possible metal deposit, the unavoidable upsets) results in a slight
but steady loss of activity (i.e. of octane). A slight increase of temperature (WAIT)
through the life of the catalyst makes up for this activity loss.
Larger and temporary changes in temperature are required:
 To change octane - at constant feed quality and quantity.
 To change feed quantity and still maintain octane (see space velocity
hereunder).
 To change feed quality and still maintain octane (see feed quality).

The set of curves given in (Figures 20 to 24) allows an estimate of the increment in
the WAIT which would result from increment in the selected parameter:
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 Space velocity (WHSV)


 Pressure
 RON clear
 Feed quality (A + 0.85N and MABP).

Example: one wants to increase RON from 96 to 100. Refer to Fig. 22

RON 96  WAIT -4.5=


RON 100  WAIT 5.5=
Result  WAIT 5.5=- (-4.5) = 10°C

WAIT must be raised by 10°C.

1.2. Reaction Pressure


Theoretically, the lower the pressure, the higher the reformate yield and hydrogen
purity - for a given space velocity - and feed characteristics. The pressure at the last
reactor inlet is generally considered as the most representative for the purpose of
this discussion However, there is little flexibility since the unit and the recycle
compressor are designed for a given pressure. Lowering the operating pressure
below the design pressure results in higher pressure drop and is limited by the
recycle compressor design power.

Not regulated normally, working control pressure is product separator pressure (i.e.
D-71201 pressure) instead of reactor pressure, reaction changes along with the
change of system pressure. D-71201 pressure normally controlled at 0.243MPa, D-
71201 pressure controller PIC-2068 output adopts two split-range control, normal
pressure regulation controlled by valve PV-2068A and valve PV- 2068C . Open PV-
2068 / B only in case of system overpressure.

The low pressure which favors high yields, favors also coke build up. During
transient conditions (startup, shutdown, upsets) it is recommended to increase the
pressure to 0.34MPa.

1.3. Space Velocity


Space velocity is the amount of liquid (expressed in weight or in volume), which is
processed per hour, divided by the amount of catalyst (in weight or in volume). The
inverse of the space velocity is linked to the residence time (or contact time) in the
reactors.

Knowing the liquid flow rate (or the space velocity), plus the recycle flow and the
reactors operating conditions enables to calculate the actual flow in the reactor,
hence the contact time.

The lower the space velocity (i.e. the higher the contact time), the higher the
severity, assuming all other conditions unchanged.
Lowering the space velocity has, then, the same effects as increasing the
temperature i.e., it:
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 Increases the octane.


 Decreases the product yields.
 Decreases H2 purity.
 Increases coke deposit.

If temperature increase is limited (by heater design duty or anything else) lowering
space velocity (i.e. decreasing flow rate) can give an additional boost to octane.

Operators must bear in mind that each time liquid feed rate is changed, a
temperature correction must be applied if octane is to be maintained. When feed is
increased, temperature must be raised and conversely, when feed is reduced
temperature must be lowered.

When changing feed rate, an important rule is:


For feed increase: Increase feed first, then adjust temperature increase to meet
octane.
For feed reduction: Lower temperature first, then adjust feed reduction to meet
octane.

Example of temperature adjustment with space velocity (see Fig. 20).

Original Increased
conditions feed
bbl/h 800 1000
Feed vol.
m3/h 127.19 158.99
(API) lb/bbl (55) 265.3 no change
Sp gr
Kg/m3 756.9 no change
lb/h 212,240. 265,300.
Feed wt
t/h 96.270 120.340
wt (lb) 117,910. no change
Catalyst
(t) 53.480 no change
WHSV 1.8 2.25
WAIT reading (°C) -2 + 2.5
WAIT change (°C) Base + 4.5

CONCLUSION: For an increase of WHSV from 1.8 to 2.25 the WAIT must be
increased by 4.5°C.
The unit's space velocity is 1.6, usually not less than half of design value.

1.4. Hydrogen-to-Oil Ratio


The H2/HC ratio is the ratio of pure H2 in the recycle (mole/h) to the feed flow rate
(mole/h)

The H2/HC ratio is calculated as follows:


R
H2 M xY
HC = F
m

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CCR UNIT KRCIM 71200.08 REV.0

Where R is the recycle flow in Kg/h (or lb/h)


M is the recycle gas molecular weight
F is the feed rate in Kg/h (or lb/h)
m is the feed molecular weight
Y vol. fraction of H2 in the recycle gas

The recycle gas MW is obtained by chromatographic analysis, as well as the H 2 vol.


fraction (Y).
The feed MW is obtained by chromatographic analysis or by correlation from its
distillation range and specific gravity.
Operators can change the H2/HC ratio by lowering or increasing the recycle
compressor flow.
The H2/HC ratio has no obvious impact on the product quality (octane) or yield. But a
high H2/HC ratio reduces the coke build up.
It is strictly recommended to operate with a H2/HC ratio equal to (or higher than) the
design figure.
The unit 's hydrogen oil ratio is 3.

1.5. Feed Quality


The feed has always been hydrotreated with the object of removing sulfur, nitrogen,
metals and, in case of cracked naphthas, olefins and diolefins. It is assumed that the
pretreated feed meets the specifications given in chapter 5 "Oil in" (KRCIM
71200.06).
The feed quality, once hydrotreated, is mainly expressed by its chemical analysis
and its distillation range.

1.5.1. Chemical analysis


The chemical analysis of the feed will give for each carbon number (C6, C7, ...
to C10) the breakdown into Paraffins, Naphthenes, Aromatics (or PNA).
As the fastest reaction is the dehydrogenation of naphthenes into aromatics,
the value of a specific feed can be characterized by its initial concentration in
naphthenes and aromatics.

An index (A + 0.85N) where N and A are the liquid volume percent of


naphthenes and aromatics in the feed, is used by AXENS to characterize the
process feed.
A feed with a high (A + 0.85N) will be easier to process than one with a lower
(A + 0.85N) i.e.:
 The same octane will be obtained at a lower severity (temperature) and
the product yield will be higher.
 Or for the same severity (temperature), the octane will be higher.

Typically, with a feed having a higher reforming index, the naphtenic


hydrocarbon content is generally higher, the endothermic reaction heat is
increased and the feed flow rate will be limited by the heater design duty. In the
opposite case, with a paraffinic feed the hydrogen purity of the recycle gas
decreases and operation will be limited by the recycle compressor capacity.

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Fig. 23 gives an estimate of the relationship between PNA and severity. As with
the other figures it is used by determining increments related to an existing
base case (see example).

1.5.2. Distillation range


One feed property that the Unit Owner can control is the distillation range. The
naphtha end point is controlled in the upstream unit distillation (crude unit
fractionator for straight run naphtha). The initial boiling point is controlled at the
naphtha hydrotreater splitter.

The feed distillation range is generally as follows:

(°C) (°F)
IBP (Initial Boiling Point) 70-100 158-212
EP (End Boiling Point) 150-180 302-356

This IBP enables to include in the feed components such as


methylcyclopentane (BP 72°C) and cyclohexane (BP 80.7°C) which are
benzene precursors.
In some cases, however, the benzene content in the gasoline is strictly limited.
In these cases, the IBP must be raised to 82°C (180°F) or above.
A feed with a low IBP generally contains more C6 and lighter paraffins and
requires a higher severity to obtain the same octane number than a feed with a
higher IBP.

One must also consider the distillation end boiling point (EP). High EP means
heavier fractions which are richer in aromatics and naphthenes and thus are
easier to process. However the high boiling point fractions are potential sources
of polynuclear aromatics which are coke precursors. EP higher than 180°C
(356°F) are generally not recommended.

Fig. 24 in Appendix gives an estimate of the change in severity associated with


a change in the distillation range. The distillation range is expressed by the
mean average boiling point (MABP).

Example based on Fig. 23 and 24


Base case Alternate
(A + 0.85 N) LV% 42 35
MABP (°C) 130 122
 WAIT Fig. 4 -4.8 + 0.7
 WAIT Fig. 5 - 1.2 + 0.8
 WAIT from Fig. 23 (A+0.85N) 5.5
 WAIT from Fig. 24 (MABP) +2

CONCLUSION: WAIT must be increased by 7.5°C.

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2. Principles Of Key Parameters Control


The principles of the control of the operating parameters are explained below.

2.1. Reaction Section And Recontacting Section Pressure


(See DWG. PressureControl)
2.1.1. The philosophy behind the pressure control is to maintain the reactor outlet
pressure within a narrow range. To do so the pressure is actually controlled at
the separator drum by delivering at the battery limit all the produced hydrogen.
In normal operation no hydrogen gas is purged at the separator drum.
2.1.2. A part of the hydrogen production flows through recycle compressor in order to
maintain the H2/HC ratio. The H2 rich gas compressor (reciprocating) exports
the rest of H2 production through two stages.
2.1.3. The pressure at reactor outlet is controlled by PIC2068. This PIC acts either on
the valve situated between the interstage KO drum (in case of low pressure) or
on the valve at the separator drum (in case of high pressure).
2.1.4. PIC2079 controls the interstage KO drum pressure by acting on the spill back
line from 2nd stage discharge to 1st stage discharge .
2.1.5. PIC2085 controls directly the pressure at the recontacting drum by acting on
the PV situated on battery limit line.

2.2. Reactor Temperature Control


The temperature control at each reactor inlet is straightforward: it acts on the amount
of fuel gas delivered to each heater.

2.3. H2 To Hydrocarbon Ratio


This ratio is adjusted by variation of the recycle compressor rotating speed.

2.4. Stabilization Section


C-71201Operation parameter analysis
2.4.1. Tower bottom temperature
Tower bottom temperature is a major parameter of stabilization gasoline
quality, when tower pressure unchanged, increasing tower bottom temperature,
which will lead to a heavier component in tower top. Tower bottom temperature
is cascaded with gas pressure for reboiler furnace F-71205
2.4.2. Pressure
In normal operation, the pressure of the tower is controlled by controller
PIC2092 in D-71205 overhead stream to fuel gas system. When reflux tank D-
71204 has more gas phases, D-71205 absorption is out of time or under start-
stop operation, use controller PIC2096 to control reflux tank D-71204 pressure.
2.4.3. Reflux ratio
Overhead reflux quantity is an important method to regulate fractionation effect.
Reflux ratio 7.47 (for product, when stabilization gasoline overlapped with
component of tower top), shall increase tower bottom temperature and reflux
rate for regulation to normal status.

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

3. Adjustment Of Operating Conditions

3.1. Water And Chlorine In The Recycle Gas


The impact of water and chlorine on catalyst activity has been discussed in 3.3
"Catalyst Activity Mechanism" of (KRCIM 71200.03).
3.1.2. Although too large amount of water in the recycle (over 30 ppm vol.) is
detrimental to the catalyst; it is also recognized that some water (15 to 25 ppm
vol.) is required to activate the acid function of the catalyst.
3.1.3. In a reforming unit, the amount of water produced in the reduction phase
normally results in 15-25 ppm vol. in the recycle. An on-line moisture analyzer
enables to check this figure.
3.1.4. Chlorine is injected in the oxychlorination phase and its flow is adjusted to meet
the recommended range of 0.9% wt to 1.1% wt of chlorine on catalyst.
3.1.5. In CCR, under normal conditions, there is no need for water or chlorine
injection into the feed. Chlorine injection into the feed may be required in a few
instances such as after a water upset in the feed, or if the regeneration unit is
shutdown. In this case, chlorine injection is a function of water content in the
recycle. The following figures are recommended.

Water content in recycle Chlorine injection


(ppm vol.) (ppm wt in feed)
25 to 35 1
35 to 50 2
50 to 100 2
(lower temperature to 480°C)
above 100 5
(lower temperature to 460°C)
The two last cases result obviously from operation upsets. Severity must be
lowered to protect catalyst against quick deactivation. Such water upsets must
be corrected: the operation of the hydrotreater stripper or the source of water
contamination in the storage must be investigated.
3.1.6. Water injection in the feed when regeneration is stopped is even more unlikely.
If water content in recycle is lower than 15 ppm vol. water injection must be started
to restore 15-25 ppm. One ppm wt of water in feed yields approximately 4 ppm vol.
in the recycle.

Note that some water analyzers drift, with time, towards lower readings. It is
wise to check the analyzer prior to start water injection.

3.2. H2S Content In The Recycle Gas


3.2.2. In normal operation, at high severity, the H2S content in the recycle gas will be
lower than 1 ppm vol. as the sulfur content of the feed is lower than 0.5 ppm.

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3.2.3. A higher H2S content in the recycle indicates a malfunction of the hydrotreater,
either a too low temperature in the reaction, a sudden increase of total sulfur in
the hydrotreater feedstock, or simply a poor operation of the stripper. The
cause must be found and corrected as to reduce the total sulfur of the feed
down to the design value.
3.2.4. If the H2S content of the recycle gas tends to increase, do not compensate with
a temperature increase. The reason for the sulfur content in the feed must be
found and corrected.
3.2.5. Anyway if this value reaches 5 ppm vol. the feed flowrate and severity must be
decreased to 480°C until the problem is solved and the H 2S content of the
recycle gas restored to its normal value.

4. Troubleshooting
4.1. General
The main causes of concern, related to process, are a possible:
 Unexpected decrease of octane number.
 Loss of reformate yield.
 Unexpected T reduction in the first catalytic bed.

 High hydrocracking rate and risk of a temperature runaway.


 High pressure drop in the reactor(s) or the regenerator.

Note that critical equipment or system failures (recycle compressor, H2 rich gas
compressor, instrument air, cooling water ...) which lead to an automatic emergency
shutdown are covered in “Emergency instructions manual”.

4.2. Unexpected Decrease Of The Octane Number


We are not considering here the cases where the octane number decrease is easily
related to:
 A change in feedstock quality (more paraffins).
 A lowering of the reactor inlet temperature.
 An increased feed flow rate.
An unexpected decrease of the octane number may be caused by one or several of
the following:
 Leak in the feed/effluent exchanger.
 Presence of nitrogen in the feed.
 Presence of sulfur in the feed.
 Presence of metals in the feed.
 Low chlorine content of the catalyst.
 Partial by-pass of the catalyst.

4.2.1. Leak in the feed/effluent heat exchanger


4.2.1.1. Since the feed is at higher pressure than the effluent, it may leak through
the exchanger. Relatively small leaks can lower the product octane
number.
4.2.1.2. Exchanger leaks can be detected by injecting tracers in the feed. An
easy tracer is methylcyclohexane which is present in the feed and not in
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the product. Another method is by measuring the octane number on the


product side, upstream and downstream the exchanger.

4.2.2. Presence of nitrogen in the feed


4.2.2.1. The maximum allowable nitrogen content in the feed is 0.5 ppm wt
expressed as NH3.
4.2.2.2. The effect to the catalyst, the causes and the remedies to apply have
been described in chapter 3.4 “Catalyst contaminants" of (KRCIM
71200.03).

4.2.3. Presence of sulfur in the feed


4.2.3.1. The maximum allowable sulfur content in the feed is 0.5 ppm wt
expressed as sulfur.
4.2.3.2. It is worth noting that sulfur affects primarily the reformate yield. The
octane number is also affected for high sulfur levels (up to 10 ppm wt).
4.2.3.3. The effect, the causes and remedies have been covered in chapter 3.4
"Catalyst contaminants" of (KRCIM 71200.03).

4.2.4. Presence of metals in the feed


4.2.4.1. The presence of metal induces a permanent catalyst poisoning which
results in a quick and noticeable drop in the octane number. It shows
mainly through a shift in the T across the reactors. This will be
discussed under that item.

4.2.5. Low chlorine content of the catalyst


4.2.5.1. If the chlorine content is too low, the catalyst activity is reduced and the
octane is lower than expected.
4.2.5.2. There are sampling points which enable to keep track of the chlorine
content. The optimum figure is between 0.9 to 1.1% wt. of pure chlorine
on the catalyst. This figure can be momentarily increased to make up for
excessive chlorine losses, due to ammonia, for instance. The injection
rate formula is given in 6.2.4. "Regeneration startup" of (KRCIM
71200.06).

4.2.6. Partial by-pass of the catalyst


4.2.6.1. If, for any reason, part of the catalyst is by-passed, the actual space
velocity is higher than expected and the octane will drop. A higher
temperature would be required to make-up for the octane loss.
4.2.6.2. The causes of by-passing can be multiple: damaged internals, build-up
of fines or scales at various places in the catalytic bed, etc.
4.2.6.3. It may develop into a hazardous situation because of the resulting
channeling and the risk of exothermic hydrocracking reactions taking
place in the area where space velocity is very low.
4.2.6.4. By-passing and channeling are generally identified by an increased
pressure drop and uneven, odd temperature profiles.

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4.3. Loss Of Product Yield


A loss of product yield may be caused by one or several of the following:
 Presence of sulfur in the feed.
 Presence of metals in the feed.
 Too high chlorine content of the catalyst.

4.3.1. Presence of sulfur in the feed


4.3.1.1. The sulfur affects primarily the product yield. Any increase in sulfur
above 0.5 ppm wt. reflects immediately in a lower product yield and a
reduced T across the reactor. Refer to 3.4 "Catalyst contaminants" of
(KRCIM 71200.03) for the causes, effects and remedies.

4.3.2. Presence of metals in the feed


4.3.2.1. This will be discussed in the item related to decreased T in the first
reactor.

4.3.3. Too high chlorine content of the catalyst


4.3.3.1. A too high chlorine content (above 1.1 wt% of pure chlorine) promotes
hydrocracking reactions which result in a lower products yield, a lower
hydrogen purity, a lower hydrogen yield, but a higher octane.
4.3.3.2. A too high chlorine content will be detected through an increased yield of
stabilizer overhead gas and lower hydrogen recycle purity.
4.3.3.3. To correct it, chlorine injection must be reduced.

4.4. Unexpected T Reduction


4.4.1.1. The temperature difference T (inlet - outlet) in the various reactors is a
very good indication of the catalyst condition.
4.4.1.2. Obvious reasons for a T decrease are:
 Feedstock quality: naphthene dehydrogenation is highly endothermic.
A lower naphthene content shows up immediately on the T in the
first reactor.
 H2/HC ratio increase (increased recycle). An increased recycle acts
as a larger heat sink for the heat of the reaction.
Other reasons of a T decrease are the consequence of upsets,
mentioned earlier, such as:
 Presence of sulfur in the feed.
 Presence of nitrogen in the feed.
 Too high chlorine content (which favors hydrocracking - exothermic
reaction).
4.4.1.3. A loss of T in the first reactor generally results from a sulfur upset in the
unit feed. Poor operation of the pretreatment reactor or of the stripper
can then be suspected. Severity must be reduced, according to the H2S
content in the recycle (for H2S > 5 ppm volume, reduce temperature to
480°C).

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4.4.1.4. In case of low T in reactors 2 and 3, hydrocracking can be suspected. If


such is the case, H2 purity drops and LPG production increases (refer
below to 2.5 “High hydrocracking rate and risk of temperature runaway”).
Generally hydrocracking does not occur in the first reactor because the
average temperature is lower.
4.4.1.5. But the most worrying aspect of a decreased T is when it cannot be
related to one of the above grounds and results from a permanent
poisoning with metals.
Lead, arsenic and other metals mentioned in 3.4 "Catalyst contaminants"
of (KRCIM 71200.03) are very severe catalyst poisons.
4.4.1.6. Due to the very high poisoning activity of the metals, the catalyst in the
first reactor is affected first, and the T through this reactor decreases.
The endothermic reactions (naphthenes dehydrogenation) move then to
the 2nd reactor which exhibits an unexpected high T.
4.4.1.7. Heavy metals generally result either from the crude processed or from a
poor operation of the upstream hydrotreating unit. Reprocessing leaded
gasoline (not a common occurrence today) can also cause catalyst
poisoning.
4.4.1.8. Metals poisoning requires the dumping of the catalyst load.

4.5. High Hydrocracking Rate And Risk Of Temperature Runaway


Hydrocracking will be suspected when H2 purity drops, the amount of LPG and
stabilization off-gas increases with a simultaneous decrease of product yield.
4.5.1. Hydrocracking can be caused by:
 A fresh catalyst (too active) or an excessive acid function of the catalyst (i.e.
high chlorine).
 A too high severity (either a too high temperature at the reactor inlet or a too
low space velocity).
 Poor distribution (channeling) in the reactor which results in local high severity
conditions.
4.5.2. The precautions to avoid hydrocracking are:
 Not to operate at capacity below the design turn-down ratio.
 Not to introduce feed for the first time on a fresh catalyst, at temperature
higher than 360°C. For a subsequent restart, the temperature limit can be
increased to 425°C.
 When raising throughput, to raise flow first and increase temperature
afterwards.
 When lowering throughput, to lower temperature first and throughput
afterwards.
 To raise temperature always cautiously: proceed by increment of 2°C/h.
 To monitor the differential pressure in the reactors. An increased differential
pressure is the sign of poor distribution.
4.5.3. If hydrocracking is suspected:
 Lower the reactor inlet temperature down to 400°C.
 Increase the feed rate to full capacity (to increase space velocity).
 Keep (or set) the recycle gas flow to the maximum.

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

4.6. High Pressure Drop In The Reactors


4.6.1. Reactors
4.6.1.1. This problem is linked to an excessive catalyst attrition (broken particles,
fines and dust). Excessive catalyst attrition is almost always associated
with a too high velocity in the catalyst lift pipes.
4.6.1.2. Operators attention is drawn to the fact that the increased pressure drop
will show days or weeks after operating conditions have deteriorated and
the situation cannot be improved. The best, one can expect, while
restoring the right operating conditions, is a pressure drop status quo.
4.6.1.3. Hence, it is advised to perform regular checks of the catalyst velocity :
once a week on a routine basis when there is no change in operating
conditions and each time operating conditions are changed (P, T,
hydrogen gas molecular weight).
4.6.1.4. The process of the increase of the pressure drop is the following :
broken catalyst particles are being trapped between the vertical wires of
the center pipe and obstruct the open area. Then fines and dust also
accumulate and dust starts building a cake around the center pipe. At
this, point the pressure drop starts to increase significantly. Depending
upon the amount of dust, the pressure drop increases more or less
quickly.
4.6.1.5. It can take between one to six months to reach about 0.100 MPa. The
maximum allowable pressure drop is dependant upon the required
severity of the operation and throughput, as the recycle gas rate will
decrease significantly.

Prevention
4.6.1.6. The best prevention is to record, on a periodic basis, the lift conditions
and the reactor pressure drop. The lift gas velocity must be adjusted to
the recommended velocity as calculated above in 4.3 "Lift gas flow". One
must keep in mind that when an excessive pressure drop occurs it is
already too late to correct the cause. This is why maintaining the
recommended catalyst velocity in the pipe is so important.

Reactor cleaning
4.6.1.7. The only way to reduce the pressure drop when it becomes
unacceptable is to shut down the unit, unload the affected reactor and
screen the catalyst with a 1.7 mm x 1.7 mm mesh with a screening
machine. The catalyst must be stored in drums under an atmosphere of
nitrogen.
4.6.1.8. Depending upon the time available for this unplanned shutdown and also
of the time to run until the next planned shutdown, the reactor may be
inspected and cleaned. Special attention must be then given to the
cleaning of the center pipe.
4.6.1.9. Then the screened catalyst will be loaded again. Generally a catalyst
make-up of 3 to 4% is required.

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

5. Conventional Operation Regulation


5.1. Temperature

5.1.1. Reactor inlet temperature and furnace gas pressure cascade control
Influencing factor Remedies
Fuel gas composition and Properly regulate gas flow
pressure change
Recycle compressor Troubleshoot compressor failure
malfunction causes H2 flow
fluctuation
Feed fluctuation Stabilize feed

5.1.2. C-71201 tower bottom temperature and F-71205 gas pressure cascade control
Influencing factor Remedies
Furnace operation fluctuation Regulate furnace operation
Tower pressure fluctuation Stablize pressure
Reflux rate fluctuation Stabilize reflux

5.2. Pressure

5.2.1. D-7120l Pressure, controlled through controller PIC2068


Influencing factor Regulation method
Temperature change, Enhance heating furnace
reforming conversion rate operation and stablize reactor
inlet temperature
Product quality change / Find cause and restore feed
Space velocity reduced or
feed interrupted
Recycle compressor failure Timely troubleshoot
Separator control valve failure Contact instrument maintenance

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

6. Analysis Control
6.1. Recommended Methods And Frequency
The frequencies given here below are related to routine operation.
Stream Test Item Test Method Frequency
SN
Name IFP SEI IFP SEI IFP SEI
Relative Density ASTM D4052 1/D 1/W
Distillation °C ASTM D86 2/W 1/W
ASTM ASTM
Sulfur,ppm 1/D 1/W
D4045 D5453
Nitrogen,ppm ASTM D4629 Occas
ASTM SH/T063
Bromine Index Occas 1/W
D2710 0
SH/T023
Hydrotreated Naphtha -Feed

Composition (PONA) IFP9301 2/W 1/W


9
Coulomb
Chlorine IFP9316 Occas
Analysis
SN-71201

Arsenic µg/kg IFP9312 RIPP 65 Occas


ASTM
Lead µg/kg IFP9406 Occas
D3237
Q/SHO18
Copper IFP9406 Occas
-0080
SH/T024
Water IP BR 94 Occas 1/D
6
ASTM
Doctor Test Occas
D4952
Mercury
IFP9606 Occas
Content
Silicon ASTM
Occas
Content D5184
Nickel
IFP9406 Occas
Content
H2S Detector Tube Occas
Q/SHO18
Composition IFP9603 1/D
.212
HCl Detector Tube Occas
SN- Recycle Dew
ASTM
71202 Gas Water Point Occas
D5454
Meter
Ammonia Detector Tube Occas
Chromoto
H2 Purity Online
graph

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

Stream Test Item Test Method Frequency


SN
Name IFP SEI IFP SEI IFP SEI
Q/SHO18
Composition 3/W
Chloride .212
SN- Absorber Detector
HCl 1/D
71203 Drum Inlet Tube
Gas Detector
H2S 1/W
Tube
Q/SHO18
Composition IFP 9603 1/D Occas
Chloride .212
SN- Absorber Detector
HCl 1/D
71204 Drum “A” Tube
Outlet Gas Detector
H2S Occas
Tube
Q/SHO18
Composition IFP 9603 1/D Occas
Chloride .212
SN- Absorber Detector
HCl 1/D
71205 Drum “B” Tube
Outlet Gas Detector
H2S Occas
Tube
ASTM
LPG Composition IFP 9603 1/D
D2163
Absorber
SN- Detector
Drum HCl Occas
71206 Tube
Overhead
Detector
Gas H2S Occas
Tube
ASTM
Stabilizer Composition IFP 9603 Occas
D2163
Reflux
SN- Detector
Drum HCl Occas
71207 Tube
Overhead
Detector
Gas H2S Occas
Tube
Relative ASTM
Occas
Density D4052
ASTM
Distillation °c Occas
D86
ASTM
Sulfur,ppm Occas
SN- Stabilizer D5453
71208 Feed Nitrogen,pp ASTM
Occas
m D4629
Bromine SH/T063
Occas
Index 0
Composition SH/T023
Occas
(PONA) 9

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

Stream Test Item Test Method Frequency


SN
Name IFP SEI IFP SEI IFP SEI
ASTM
Composition (PONA) ISO 7941 1/W 1/D
D2163
Vapor Pressure ASTM D1267 Occas
Copper Strip Test ASTM D1838 Occas
Total Sulfur ASTM D3246 Occas
ASTM D
Density 1/W
1657
ASTM D
Stabilizer Volatility 1/D
1837
Reflux
SN-
Drum Doctor ASTM D
71209 Occas
Liquid test 4952
(LPG)
ASTM D
H2S Occas
2420
Mercapta ASTM D
ns 3227 Occas

LPG
ASTM
sampling Occas
1265
method
Relative ASTM
1/W
Density D4052
ASTM
Distillation °c 1/D
D86
Vapor ASTM
2/W
SN- Pressure D323
Reformate
71210 Octane # ASTM
Occas
(RON) D2699
ASTM
Gum Occas
D381
SH/T023
Composition 2/W
9

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

7. Supplements

 Figure 20 (WAIT Correction For a Typical Hydrotreated S.R Naphtha)


o WAIT Vs WHSV

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

 Figure 21 (WAIT Correction For a Typical Hydrotreated S.R Naphtha)


o WAIT Vs Reactors Average Pressure

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

 Figure 22 (WAIT Correction For a Typical Hydrotreated S.R Naphtha)


o WAIT Vs RON

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

 Figure 23 (WAIT Correction For a Typical Hydrotreated S.R Naphtha)


o WAIT Vs Feed Quality (PNA)

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

 Figure 24 (WAIT Correction For a Typical Hydrotreated S.R Naphtha)


o WAIT Vs Feed Quality (MABP)

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

 Figure 27 (Regeneration Pressure Control and Bias)

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

 Figure 28 (Lift Gas Pressure Control and Bias – 3 Reactors)

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KRC REFORMING SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71200.08 REV.0

 DWG.PresureControl

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KRC REFORMING SECTION
PRODUCTION & OPERATION SHUTDOWN PROCEDURE
CCR UNIT KRCIM 71200.09 REV.0

Contents: This instruction outlines the shut-down procedure of the CCR reforming
Unit.The text includes:

1. Overall Shutdown Operation


2. Short Duration Normal Shutdown Scheme
3. Normal Shutdown Scheme
4. Normal Shutdown With Catalyst Unloading

1. Overall Shutdown Operation

1.1. Description
1.1.1. The normal shutdown applies to a shutdown planned long in advance
(preventive maintenance) or to unexpected events which are not of an
emergency nature. The shutdown shall then be performed in planned stages.
The operators of the upstream or downstream units shall be informed of the
shutdown to enable them to make the necessary adjustments and/or to plan
their own shutdown.
1.1.2. The general procedure to be followed for a total shutdown is:
 To lower the severity and the capacity of the unit.
 To shut down the reaction section.
 To shut down the catalyst circulation and the regeneration sections.
1.1.3. Note: If no external source of hydrogen is available the hydrotreater unit will
also have its capacity reduced first, then be shut down. Special care will be
taken during this period as to keep the hydrotreated product on specifications.
1.1.4. Several shutdown cases are considered:
 Short duration normal shutdown (less than 24 hours).
 Long duration normal shutdown.
 Shutdown with catalyst unloading.
 Normal shutdown of the catalyst circulation and regeneration only

2. Short Duration Normal Shutdown Scheme (Less than 24 hours)


Implementing shutdown scheme is to guarantee safety of shutdown process

Step 1
Start lowering reactors R-71201/202/203 inlet temperature to 470°C, by
increments of 5°C.

Step 2
One hour after the start of step 1, start reducing the feed flowrate, by
increment of 3t/h, to 60% of the design capacity (30 t/h), which must be
reached at 470°C. Adjust flow increments in order to maintain the product
quality within acceptable limit. At the same time the feed to the pretreatment
unit (71100) is proportionally reduced and its reaction temperature adjusted.

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PRODUCTION & OPERATION SHUTDOWN PROCEDURE
CCR UNIT KRCIM 71200.09 REV.0

Step 3
Simultaneously with the preceding step, increase the reaction section
pressure to approximately 0.350 MPa g (at separator drum D-71201). During
this pressure increase, watch carefully the catalyst circulation, the N 2 lift
PDV's opening and adjust the bias if required to maintain catalyst circulation

Step 4
Stop the catalyst circulation and the regeneration loop as described in
“Catalyst regeneration section” (Partial shutdown) 8.1 of KRCIM 71300.05

Step 5
Stop the feed to the pretreatment unit 71100 and when the level in the bottom
of the C-71101 stripper starts to decrease, stop the feed to the reforming unit
71200. Close FV2006. Line-up the product to the slop tank. Shut-off the
reduction heater K-71304 and close the H2 valve FV3017 to reduction
chamber and PDV3012 as well as HV3003 at reduction gas outlet

Step 6
Immediately after the feed cut off, shut down the H2 rich gas compressor K-
71202. Close in manual mode the spill back PIC2068C of the H 2 rich gas
compressor to avoid the quick depressurization of the recontacting section
into the reaction section and the release of the separator drum PSV. Shut
block valves at compressor K-71302 suction and discharge. Start lowering
reactor inlet temperatures at a rate of 25°C/h to 400°C. K-71201 remains
in operation, in the meantime, retain D-71201 pressure not less than 0.3MPa,
D-71201 liquid level retains 30%, if liquid level is higher, use P-71201 to
transfer oil to C-71201 through start-up line.

Step 7
When the level starts to decrease in D-71201, stop the pump P-71201 to the
recontacting section and isolate the block valves of LV2002.

Step 8
When the level starts to decrease in D-71203, isolate the block valves of
LV2008 to the LPG absorber drum D-71205

Step 9
When the level starts to decrease in D-71205, stop pump P-71204 to the
stabilizer and close the block valves of the FV2015

Step 10
Then isolate the bottom of the stabilizer C-71201, by closing reformate
FV2026 & LPG LV2019 block valves. Keep the column at total reflux
conditions.

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KRC REFORMING SECTION
PRODUCTION & OPERATION SHUTDOWN PROCEDURE
CCR UNIT KRCIM 71200.09 REV.0

2.1. Stand-by status


For a short duration shutdown, the unit will be kept in the conditions reached above
i.e.:
 Feed is shut down.
 H2 rich gas compressor K-71202 shut down.
 Catalyst circulation and catalyst regeneration partially shut down (i.e. catalyst
circulation stopped, regeneration compressor K-71301 and N2 compressor K-
71302 still on).
 Air compressor K-71304 running but air injection FV3007/3004 closed and
blocked.
 Recycle compressor K-71201 in operation.
 Heaters on and reactor inlet temperatures at 400°C.
 Block valves closed on separator drum PV2068A/B/C to flare and to fuel gas.
 Reaction section and recontacting sections (if possible) pressure maintained by H 2
make up from storage (or from other units).
 Stabilizer isolated, at total reflux.

3. Normal Shutdown Scheme


3.1. General
 Prepare adequate reformate in treated oil tank before shutdown.
 Implementing shutdown scheme is to guarantee safety of shutdown process and
create conditions for safe overhaul in next step.

3.2. Status
Before shutdown, all subunits and utilities are operating normally. During shutdown,
these parts will be stopped successively.

3.3. Shutdown sequence


 Reforming section cooling and quantity reduction .
 Regeneration section stop.
 Reforming section shutdown.
 Prehydrotreating section shutdown.
 WHB shutdown.

3.4. Shutdown preparation.


3.4.1. Contact production dispatch, determine concrete time of shutdown, uniformly
coordinate and guarantee the smoothness of oil line, offspec and slops oil line
and flare lines.
3.4.2. Contact upstream, downstream unit, ensure coordinated shutdown, mutual
support and smooth shutdown.
3.4.3. Contact production dispatch, guarantee the supply of medium pressure steam,
low pressure steam and nitrogen.
3.4.4. Contact waste water treatment units to prepare for handling sewage, slop oil,
waste dechlorination agent and waste drying agent, etc.
3.4.5. Prepare shutdown blind plate table. Put in details blind position, size and
operator signature of blind plate. Prepare complete job slip.

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KRC REFORMING SECTION
PRODUCTION & OPERATION SHUTDOWN PROCEDURE
CCR UNIT KRCIM 71200.09 REV.0

3.4.6. Before shutdown, organize staff members and workers to study shutdown
scheme.

3.5. Reaction Section Shutdown Procedure

Step 1
Start lowering reactors inlet temperature to 470°C, by increments of 5°C.

Step 2
One hour after the start of step 1, start reducing the feed flowrate, by increment
of 3t/h, to 60% of the design capacity (30 t/h), which must be reached at 470°C.
Adjust flow increments in order to maintain the product quality within acceptable
limit. At the same time the feed to the pretreatment unit (71100) is
proportionally reduced and its reaction temperature adjusted.

Step 3
Simultaneously with the preceding step, increase the reaction section pressure
to approximately 0.350MPag (at separator drum D-71201). During this pressure
increase, watch carefully the catalyst circulation, the N2 lift PDV's opening and
adjust the bias if required to maintain catalyst circulation

Step 4
Stop the catalyst circulation and the regeneration loop as described in “Catalyst
regeneration section” (Total shutdown) 8.2. of KRCIM 71300.05

Step 5
Stop the feed to the pretreatment unit 71100 and when the level in the bottom
of the stripper C-71101 starts to decrease, stop the feed to the reforming unit
71200. Close FV2006 and install a blind in the line. Line-up the product to the
slop tank. Shut-off the reduction heater H-71304 and close the H2 flow control
valve FV3017 to reduction chamber and PDV3012 as well as HV3003 at
reduction gas outlet

Step 6
Immediately after the feed cut off, shut down the H 2 rich gas compressor K-
71202. Close in manual mode the spill back PIC2068C of the H 2 rich gas
compressor to avoid the quick depressurization of the recontacting section into
the reaction section and the release of the separator drum PSV. Shut block
valves at compressor suction and discharge. Isolate with blinds all H2 outlet /
inlet lines to the unit. Start lowering reactor inlet temperatures at a rate of
25°C/h to 400°C. K-71201 remains in operation, in the meantime, retain D-
71201 pressure not less than 0.3MPa, D-71201 liquid level retains 30%, if liquid
level is higher, use P-71201 to transfer oil to C-71201 through start-up line 100-
P-2099

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PRODUCTION & OPERATION SHUTDOWN PROCEDURE
CCR UNIT KRCIM 71200.09 REV.0

Step 7
After 6 hours of hydrogen sweeping, allow the catalyst beds to further cool
down while decreasing reactor outlet temperatures progressively to 200°C,
then cut off the fired heaters F-71201/202/203. Continue circulating hydrogen
with the recycle compressor until the temperature in the reactor beds is 50°C.

Step 8
Depressurize D-71201 to the flare to 0.05MPa, fill D-71201 with nitrogen from
K-71201 outlet to 0.3MPa. Depressurize again to flare. Fill again to 0.3MPa,
ensure that the speed of pressure rise and fall per hour shall not exceed
0.1MPa. Drain at every low point and dead angle position of hydrogen system.
Lead-in instrument pressure line, nitrogen purging replacement at sampling
opening. D-71201 pressure is maintained at 0.3MPa, continue nitrogen
replacement from K-71201 outlet, control pressure and depressurize to flare.
When hydrogen and hydrocarbon content in sampling analysis is less than
0.5%, depressurize to 0.1MPa. Close PIC2068 manual valve, stop K-71201
and close block valves at inlet and outlet.

Step 9
When reforming system uses nitrogen for inerting, use K-71302 outlet to
replace hydrogen gas in lift lines with N2 from start-up line. If replacement is
qualified, stop K-71302 The (H2 + HC) content of the gas in the reaction section
shall drop to approximately 0.2 vol. %.

Step 10
M-71301 depressurize to flare system, feed nitrogen to inlet until hydrogen
hydrocarbon content of sampling analysis less than 1%.

3.6. Re-contact & Stabilization sections shutdown

Step 1
Before reforming feed cut, decrease D-71203, D-71204 & D-71205 liquid level
to 20-30%. Keep C-71201 level at 60% on total reflux and change gasoline to
offspec tank .

Step 2
Close reformate and LPG out valves

Step 3
Maintain liquid level of tower bottom at 60% and perform a single tower
circulation. Reduce F-71205 outlet temperature to 150˚C at the speed of 25-
30˚C/h, and stop F-71205. P-71202 continues circulation till tower bottom
temperature is less than 80˚C

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KRC REFORMING SECTION
PRODUCTION & OPERATION SHUTDOWN PROCEDURE
CCR UNIT KRCIM 71200.09 REV.0

Step 4
Connect nitrogen to K-71202 outlet and fill pressure to 0.8MPa, flush oil in D-
71203 and pipeline to D-71205. Isolate with blind D-71203 bottom. Then use
nitrogen to purge D-71204 overhead pipe to D-71205. Use P-71204 to transfer
oil to C-71201. If D-71205 is emptied then stop P-71204.

Step 5
After pump P-71204 is stopped, close FIC2015 valve and close gate valve from
D-71204 to D-71205. Depressurize from PIC2085 to flare, and conduct nitrogen
replacement of system.The (H2 + HC) content of the gas in the reaction and
recontacting sections shall drop to approximately 0.2 vol. %.

Step 6
Stop P-71202 and connect N2 to outlet and purge oil in furnace tubes into C-
71201. Send oil in D-71204 into C-71201, stop P-71203 and reduce C-71201
bottom oil to offspec tank.

Step 7
Drain all lines until you observe gas then close drains.

Note: Close all gate valves to isolate the control valve which you close

4. Normal Shutdown With Catalyst Unloading

Catalyst may be unloaded either for inspection of reactor(s) or regenerator or because it


is used and needs replacement.
First, the relevant sections of the unit must be freed from hydrocarbons. Then the catalyst
will be dumped:
 either under an atmosphere of nitrogen.
 or after a coarse decoking.

4.1. Proceed As Per The Long Duration Normal Shutdown, Then:


 Isolate now the reaction section from the recontacting section by installing a blind
at D-71201 bottom, at the spill back line 200-P-712034 of H2 rich gas to D-71207.
Blind also the PSVs and their by-pass in both sections, as well as PV2068A/B to
flare and fuel gas system. Remove the blind of the D-71201 PSV to atmosphere.
 Remove then the blind from the ejector J-71201 suction line and pull the vacuum
to the reaction section down to 0.050 MPa abs. Break the vacuum by injecting
nitrogen up to 0.010 MPa (g). Note that N2 lift loop and regeneration section are
already under N2 and are subject neither to N2 sweeping nor vacuum.
 If the catalyst is at the end of life and shall be replaced by a new one, the coked
catalyst will be dumped from the bottom of reactors and regenerator under
nitrogen into drums. If the catalyst is to be reused after unloading (shutdown for
inspection), the alternate procedure must be used.

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KRC REFORMING SECTION
PRODUCTION & OPERATION SHUTDOWN PROCEDURE
CCR UNIT KRCIM 71200.09 REV.0

Alternate procedure
4.2. The alternate to the above procedure, is the coarse decoking of the catalyst in the
regenerator, prior to unloading. Of course the oxychlorination will not be in service.
 Note 1: During these operations, the regeneration section is kept under nitrogen
atmosphere. Care should be taken to avoid stress corrosion by chlorine for the
stainless steel equipment
 Note 2: Another alternate to the dumping of coked catalyst from the reactor and
regenerator bottom is possible. It applies when the catalyst is to be replaced by a
fresh one, but when no reactor(s) or regenerator inspection is planned. It consists
in dumping the catalyst at the bottom of the lock hopper, while the reaction
section is in service at low severity, and in replacing it, in the same vessel, by
fresh catalyst, by means of the catalyst loading deveice, plugged atop the lock
hopper. In such a case, the regenerator is used only to dry the new.

ISSUE DATE: 20/03/06 - 208 -


KRC
PRODUCTION & OPERATION CATALYST REGENERATION SECTION
CCR UNIT

Table of Contents

INTRODUCTION (KRCIM 71300.01)


1. Unit introduction...............................................................................................1
2. Manual Structure..............................................................................................1

BASIC KNOWLEDGE (KRCIM 71300.02)


1. Basis of design.................................................................................................2
2. Unit Description................................................................................................4
3. Catalyst..........................................................................................................19
4. Chemistry.......................................................................................................19

PREPARATION FOR INITIAL START-UP (KRCIM 71300.03)


1. Plant Inspection..............................................................................................23
2. Cleaning of Piping and Equipment.................................................................25

START-UP/SHUTDOWN OPERATIONS (KRCIM 71300.04)


1. Start-Up Requirement....................................................................................26
2. Unit Purging...................................................................................................26
3. Initial Leak Test..............................................................................................31
4. Unit Dryout.....................................................................................................36
5. Catalyst Loading............................................................................................38
6. Second Leak Test And Partial Inerting..........................................................38
7. Unit Start-up...................................................................................................38
8. Catalyst Regeneration Section Shutdown.....................................................39

OPERATING CONDITIONS & CONTROL (KRCIM 71300.05)


1. Operation Influencing Parameters.................................................................41
2. Principles Of Key Parameters Control...........................................................42
3. Special Control Systems And Safety Devices...............................................46
4. Adjustment Of Operating Conditions.............................................................47
5. Troubleshooting.............................................................................................53
6. Analysis Control.............................................................................................56
7. Supplements..................................................................................................58

PROCESS AUTOMATION (KRCIM 71300.06)


1. Control Functions...........................................................................................60
2. Catalyst Transfer Sequence Description (UC2).............................................63
3. Catalyst Circulation Control............................................................................68
4. Hydrogen System Pressure Control (UC 3)...................................................71
5. Special Loops Description.............................................................................72
6. Temperature Control Optimization.................................................................75
7. Appendix........................................................................................................77

SPECIAL EQUIPMENT (KRCIM 71300.07)


1. Membrane Hydrogen Purification Unit (M-71301).........................................84
2. Regeneration Loop Dryer DR-71301.............................................................94
KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION INTRODUCTION
CCR UNIT KRCIM 71300.01 REV.0

Contents: This document outlines the structure of CCR (Catalyst Regeneration


Section) operation manual. The text includes:

1. Unit Introduction
2. Manual Structure

1. Unit Introduction

1.1. General
Continuous Catalytic Reforming Unit (CCR) of Khartoum Refinery Company is built
under the expansion project of the refinery, phase II. The unit is designed by
Sinopec Engineering Incorporation. The process utilizes Axens's "State of the art"
moving catalyst bed with continuous catalyst regeneration.
The unit is designed to process 400,000 metrics tons per year and to operate at a
severity of RON 98 with an on-stream factor of 8000 hours/year.

1.2. Configuration of the Unit


This unit consists of several components, including
 Pretreatment section (unit 71100)
 Reforming section (unit 71200)
 Catalyst regeneration section (unit 71300)
 Utilities section (unit 71400)
 Waste heat boiler section (unit 71500)

2. Manual Structure
The design information and operating instructions of the Continuous Catalytic Reforming
Unit (unit71) are covered by six different volumes as follow:

KRCIM 71100 is dedicated to pretreatment section


KRCIM 71200 is dedicated to reforming section
KRCIM 71300 is dedicated to catalyst regeneration section
KRCIM 71500 is dedicated to waste heat boiler section
KRCIM 71EMP is dedicated to emergency procedures
KRCIM 71TRS is dedicated to test run scheme

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71300.02 REV.0

Contents: This document outlines the general description of catalyst regeneration


and circulation section of CCR unit. The text includes:

1. Basis of design
2. Unit Description
3. Catalyst
4. Chemistry

1. Basis Of Design

1.1. Duty Of Unit


This section presents the various characteristics of the catalyst regeneration and the
catalyst circulation systems of the catalytic reformer unit.
The purpose is to regenerate continuously the catalyst during the normal operation
of the reformer unit and so to maintain a steady coke level in the reactors, and
optimum operating conditions for the octanizing unit. These operating conditions are
almost constant except for the catalyst end of life.
The catalyst circulation through the reactors and through the catalyst regeneration is
achieved automatically.
The capacity of the catalyst regeneration system is 32 kg of coke burnt per hour,
with a catalyst flowrate equal to 410 kg/h

1.2. Utilities And Flare Conditions (at battery limits)

1.2.1. Air

Plant air
(oil-free for catalyst regeneration)
Pressure Temperature
Minimum: 0.6MPa(G)
Normal: 0.8MPa(G)

Instrument air
Minimum: 0.6MPa(G)
Normal: 0.8MPa(G)

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1.2.2. Water

Cooling water - Supply Pressure Temperature


Minimum: 0.4MPa(G) 32°C
Maximum: 0.5MPa(G) 32°C

Cooling water - Return


Minimum pressure required for return: 0.25MPa(G)
Maximum temperature for return: 42°C

Process water (catalyst wash,


chemicals)
Normal: 0.4MPa(G) ambient
Source: demineralized water
Quality: provide detailed analysis

Process water (water wash)


Normal: 0.4MPa(G) ambient
Source: condensate, B.F.W., stripper
water
Quality: deaerated

1.2.3. Nitrogen

Availability: 0.8MPa(G) or 2.5MPa(G)


Quality: provide detailed analysis Purity:99.99%

1.2.4. Fuel

Fuel gas Pressure

Minimum: 0.30MPa(G)
Normal: 0.35MPa(G)
Maximum: 0.40MPa(G)
Quality : Thermal value:7000kcal/kg

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1.2.5. Flare header pressure

 Normal Pressure : 0.05MPa(G)

 Design Pressure : 2.5MPa(G)

1.3. Climatic Data

These data are required for reference only to indicate if a need exists for tracing or
winterizing.

 Maximum temperature: 46.7°C

 Design maximum ambient temperature: 45°C

 Minimum temperature: 6.2°C

 Relative humidity

o Average: 27%

o Maximum: 44%

 Barometric pressure

o Minimum: 96.3kPa

o Maximum: 96.9kPa

o Average: 96.56kPa

2. Unit Description

2.1. Catalyst Regeneration

To perform a good regeneration of the octanizing catalyst, the following operations


must be carried out:

 Coke burning.

 Catalyst oxychlorination.

 Catalyst calcination.

 Catalyst cooling.

 Catalyst reduction.

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The first three steps are performed in the regenerator, the fourth step in the first lower
hopper and the last step in the reduction chamber.

2.1.1. Regenerator

2.1.1.1. Storage zone

 Spent catalyst coming from the lock hopper D-71302 is stored in the
top of the regenerator during the equivalent of 1 to 2 hours of catalyst
circulation, where it is smoothly preheated by a part of the heat
released by the combustion zone.

 Then the spent catalyst flows from this zone to the burning zone by 6
descending pipes.

2.1.1.2. Burning zone

 The burning zone is composed of two radial beds. The two beds are
physically linked by 6 descending pipes.

 These radial beds are crossed by a combustion gas. The temperature


of this gas increases as the combustion reaction advances in those
beds.

 The controlling parameters are the combustion gas temperature and


the oxygen content in the combustion gas. The common values are
the followings:

O2 % mol Temp. (°C)

First bed 0.8 480

Second bed 0.8 480

 A quench line is provided to inject a small amount of cooling gas


between the two burning beds, in addition of the air make-up flow.
This injection will decrease the second burning bed inlet temperature
and will allow a better control of temperature inside the regenerator
during high severity operation.

 The catalyst is considered as free of coke at the bottom of the


second burning bed if oxygen consumption is incomplete and no
temperature increase occurs.

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2.1.1.3. Oxychlorination / calcination zone

 The catalyst is then collected by another set of 6 pipes and sent to an


axial bed where oxychlorination and calcination take place. In this
zone, the gas circulates upward.

 The oxychlorination gas is composed of:

o Air having crossed the calcination zone (typically 50 % of the


flowrate),

o The gas introduced in the oxychlorination bed containing the


chlorination agent and water (remaining 50 % of the flowrate).

 Common characteristics of oxychlorination gas are the following:

Oxygen content : 4 - 6 % vol

Temperature : 510 °C

 The calcination gas is introduced in the bottom part of the


regenerator. This gas consists of dry air. Common characteristics of
calcination gas are the following:

Oxygen content : 4 - 6 % vol

Temperature : 520 °C

Water content : less than 50 ppm vol

 A minimum pressure drop is maintained between the burning zone


and the oxychlorination / calcination zone to prevent the
oxychlorination gas, with high oxygen content, from mixing with
burning gas.

2.1.1.4. Black burning operation

 If the entire amount of coke is not burnt off at the end of the second
bed, the regenerator will be operated in black burning mode : the
catalyst, though not free of coke, flows through the oxychlorination
and the calcination zones, in which the air injection as well as the
chlorination agent and water injections have been previously totally
stopped.

 Consequently the catalyst returns to the reactors despite a certain


coke level. The octanizing unit can work under these conditions
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CCR UNIT KRCIM 71300.02 REV.0

 during a short period of time. It allows to maintain the catalyst


circulation while operating conditions are adjusted to recover an
acceptable coke level on the catalyst.

2.1.2. First lower hopper: catalyst cooling

 The catalyst at the bottom of the regenerator R-71301 is collected by 8


pipes and flows into the first lower hopper D-71304, which is under a slight
overpressure of nitrogen in order to prevent oxygen from entering into the
nitrogen lift gas system.

 The 8 pipes are not insulated in order to allow a natural cooling of catalyst
by convection.

 Catalyst flows from there down to the first lift pot D-71305, where it is lifted
by a flow of nitrogen gas into the first upper hopper D-71310, before being
introduced into the reduction chamber D-71311.

2.1.3. Reduction chamber

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 Reduction of the freshly regenerated catalyst is performed in the reduction


chamber D-71311. This operation is slightly exothermal and the inlet
temperature is adjusted in order to have around 480 °C at the reduction
chamber outlet.

 The reduction gas is an hydrogen-rich gas, produced in octanizing


reactions: a part of the hydrogen-rich gas recovered in the recontacting
drum is sent to the catalyst regeneration/circulation section and is split into
two streams:

o Hydrogen-rich gas for lift system.

o Hydrogen-rich gas for reduction.

 The latter is sent to the purification unit M-71301 to upgrade its purity up to
99 % mol minimum of H2. Residue of hydrogen purification unit is sent to
fuel gas. Permeate is preheated in the reduction exchanger E-71304. Then
an electrical heater (reduction heater H-71304) allows a precise adjustment
of the reduction inlet temperature.

 After reduction, the reduction effluent is split into two streams.

 The first stream preheats the inlet reduction gas in the reduction exchanger
E-71304, the second stream preheats the hydrogen-rich gas going to the lift
system in hydrogen lift gas exchanger E-71305. Both streams are then
mixed before being sent back to the reaction section.

 The reduced catalyst is then introduced into the first reactor R-71201.

2.1.4. Regeneration loop

2.1.4.1. Burning gas

 This main stream is mixed with air in order to reach an oxygen


content of 0.8 % mol and preheated in the burning feed/effluent
exchanger E-71301. An electrical heater, the burning heater H-71301,
allows to adjust the temperature of the gas before entering the
regenerator’s burning zone.

 This combustion gas enters the regenerator at the uppermost height


of the descending pipes (between the storage zone and the burning
zone) to preheat the catalyst. Then this gas flows through the first
radial bed, is collected in the center pipe, and is mixed at the outlet of
the regenerator with air and with a quench gas to adjust the oxygen
content and temperature at the inlet of the second bed. It finally flows
through the second bed and leaves the regenerator.

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 The burning effluent is sent to the burning feed/effluent exchanger E-


71301 to recover the main part of heat produced by the combustion
reaction.

 This burning effluent contains water, produced by combustion, but


also some traces of chlorine compounds. To avoid corrosion
problems at low temperature, this gas is sent to the washing section.

 Remark : The burning gas flowrate to the first bed as well as


oxychlorination and calcination zones is kept constant, whatever the
coke level of the catalyst, by means of the spill-back of the
regeneration loop compressor.

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CCR UNIT KRCIM 71300.02 REV.0

2.1.4.2. Quench gas

 This gas is mixed with the gas leaving the first burning bed. It is used to
adjust the inlet temperature of the second bed.

2.1.4.3. Oxychlorination / calcination gas

 This stream is mixed with air to obtain an oxygen content of 4 to 6 % vol,


then preheated through a calcination feed/effluent exchanger E-71302.

 Water is injected in this oxychlorination gas. Then the gas is heated through
an electrical heater H-71303 which allows to control the oxychlorination gas
inlet temperature and some chloriding agent is added just before entering
into the regenerator. Contacting is performed into M-71307 static mixer,
right downstream the injection point.

 The calcination gas is heated through an electrical heater H-71302 and is


sent to the bottom part of the regenerator.

 The oxychlorination gas and the calcination gas are mixed in the
oxychlorination bed. The oxychlorination effluent is sent to the calcination
feed/effluent exchanger E-71302 and then mixed with the combustion
effluent going to washing section in order to eliminate chlorine compounds.

 The air injected in the regeneration loop is taken from air instrument
network, compressed by means of a double stage air compressor (K-71304
A/B), cooled down by air trim cooler E-71308, passed through air dryer
drum D-71342 and then dried by air dryer DR-71302 (up to less than 50
ppm vol. of water).

 The pressure of the regeneration loop, measured at calcinations zone inlet,


is controlled by means of the split range between the gas purge and the
nitrogen injection at the top of the washing drum D-71306. The pressure of
the regeneration loop is reset by the pressure of the first reactor, through a
PDC which maintains the pressure of the regenerator bottom around 0.070
MPa above the pressure of the first reactor.

2.1.5. Washing section

 The burning and oxychlorination / calcination effluents are washed by


contacting with a caustic solution.

 This solution, pumped by recycle pumps P-71301 A/B, is injected through a


spray nozzle M-71305 in the line. Contacting is performed in M-71306 static
mixer, right after the injection point. Then the mixture is cooled in a trim
cooler E-71303 and sent to the washing drum D-71306, where a final

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CCR UNIT KRCIM 71300.02 REV.0

washing is done by contacting with demineralized water across several


bubble cap trays.

 The gas coming from the washing drum flows through a dryer DR-71301,
then through a filter M-71304 where possible particles, in particular
dessicant alumina particles, are trapped and finally to the regeneration loop
compressor K-71301 A/B.

 At the compressor discharge, the gas is split into the three streams
described above:

o Burning gas

o Quench gas

o Oxychlorination / calcination gas

2.1.6. Catalyst circulation

 The catalyst circulation is carried out almost continuously by means of a gas


lift system which conveys the catalyst from the bottom of each reactor to the
top of the following reactor. The catalyst then flows downward through each
reactor bed by gravity.

 Two lift gas sources are used:

Nitrogen gas for:

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CCR UNIT KRCIM 71300.02 REV.0

o Lift 1, between the regenerator R-71301 and the first reactor R-


71201.

o Lift 4, between the third reactor R-71203 and the regenerator R-


71301.

Hydrogen-rich gas in the reaction section, i.e.:

o Lift 2, between the first reactor R-71201 and the second reactor R-
71202.

o Lift 3, between the second reactor R-71202 and the third reactor R-
71203.

2.1.7. Catalyst circulation control

2.1.7.1. Catalyst flow in lifts

 The catalyst flow is adjusted as follows: the total flowrate of the lift gas
must remain as steady as possible because any change in this flow
will affect the velocity of the catalyst in the lift line. This flowrate must
be checked carefully because a too high velocity may lead to a higher
rate of catalyst attrition.

 This gas going to the lift pots D-71305 / D-71331 / D-71332 / D-71333
is divided into two streams:

o The primary gas which initiates the lift operation,

o The secondary gas which governs the catalyst flow.

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CCR UNIT KRCIM 71300.02 REV.0

 Within the proper operating range, the rate of catalyst flow is


proportional to the secondary flowrate of gas. When the secondary
gas is stopped no catalyst can be lifted.

 The pressure drop measured between the lift pot and the next upper
hopper indicates the catalyst flow: nearly null when there is no
catalyst flow, this pressure drop will increase to about 0.010 MPa
when there is catalyst flow. Therefore this measure is used as an
indication of catalyst flow in the control used for the follow-up of the
operation of the lifts.

2.1.7.2. Catalyst levels in upper hoppers

 Catalyst surge vessels (upper hoppers D-71310 / D-71312 / D-71313)


are provided at the top of each reactor in order to compensate for
differences in catalyst flow between the lifts. It is also a protection
against variations of void fraction of the catalyst in the reactors.

 Each upper hopper is equipped with gamma-ray level sensors. One


level sensor gives continuous information for the control, the other
(very low level) gives on/off information for catalyst lift cut-off (see
description of control sequences).

 The level will be adjusted at 60 % and the measure will be used


through a cascade to modify the set point of the PDC used to monitor
the catalyst flow (the pressure drop between the lift pot and the next
upper hopper).

2.1.7.3. Catalyst batches

 Spent catalyst is withdrawn from the bottom of the last reactor R-


71203 and then lifted up to the upper surge drum D-71301 to be sent
to the regenerator for the regeneration.

 Furthermore, spent catalyst is stored in this drum at a pressure


slightly lower than that of the last reactor. In the regenerator the
pressure is slightly higher (by around 0.070 MPa) than that of the first
reactor inlet. Therefore, a pressure adjustment is needed. This is
made in the lock hopper D-71302 and induces catalyst "batches", i.e.
a non-continuous circulation between the upper surge drum D-71301
and the regenerator.

 Pressure adjustment and catalyst "batches" are performed


automatically by a specific sequence.

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2.1.7.4. Nitrogen gas lift system: lifts 1 & 4

 Nitrogen gas from lift 4 is separated from the catalyst in upper surge
drum D-71301 and flows through a fines filter M-71303 where catalyst
dust is recovered.

 In this filter, the gas circulates in upflow: it enters at the middle of the
drum and flows through several cartridges of filtering elements where
catalyst dust is trapped. These cartridges are automatically cleaned,
when the pressure drop increases, by a counter current flow of
nitrogen.

 Nitrogen gas from lift 1 is separated from the catalyst in the first upper
hopper D-71310 with an elutriation system, and cleaned in a second
fines filter M-71302.

 A part of this gas is compressed in the elutriation blower K-71303 and


flows back to the first upper hopper D-71310 as elutriation gas, to
ensure the removal of catalyst fines and chips from the system.

 The other part of the gas is mixed with the nitrogen lift gas coming
from the upper surge drum D-71301.

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 The total nitrogen gas flow is cooled through the nitrogen loop trim
cooler E-71306 and circulated by means of a compressor K-71302
A/B to the lift 1 and to the lift 4. A spillback line of nitrogen loop allows
pressure control of N2 circuit.

 Fresh nitrogen addition from refinery header is made upstream of the


nitrogen compressor K.O.drum D-71307.

 In addition to use for elutriation and lifts 1 and 4, part of the


compressed nitrogen is cooled through the nitrogen storage trim
cooler E-71307 then sent to a storage drum D-71341 and used for the
following:

o seal above the reduction chamber D-71311,

o seal under the last reactor R-71203,

o seal above and under the regenerator R-71301,

o lock-hopper D-71302 pressurization,

o pressure regulation in the regeneration loop,

o fines filters M-71302 & M-71303 bottom cleaning.

2.1.7.5. Hydrogen-rich gas lift system : lifts 2 & 3

 The hydrogen-rich gas used for lift system is produced in the


octanizing reaction section. It is preheated in the hydrogen lift gas
exchanger E-71305 before being used in the lift system.

 This hydrogen-rich gas is recovered in the 2nd and 3rd upper hoppers
and mixed with the reactors feed. For instance, for lift 2, hydrogen-rich
gas is separated from the catalyst in the second upper hopper D-
71312 and mixed with the feed of the second reactor R-71202.

2.1.7.6. Isolation of regeneration section / reaction section

 Using nitrogen gas as lift gas between the regeneration and the
reaction section allows to isolate the regeneration section from the
reaction section which are connected by the catalyst circulation lines.

 Moreover, an important point is to prevent hydrocarbons (and


hydrogen) or oxygen from entering into the nitrogen lift gas system.

 Therefore, the following protections are foreseen :

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o Nitrogen sealing : a controlled flow of inert gas is used to keep


the drums connected with the reaction section at a slightly
higher pressure than that of the reaction section (between the
first upper hopper D-71310 and the reduction chamber D-
71311 and between the last reactor R-71203 and the fourth
lower hopper D-71323).

o Safety valves : if the nitrogen sealing fails for any reason, the
valve between the first upper hopper D-71310 and the
reduction chamber D-71311 and the valve between the fourth
lower hopper D-71323 and the fourth lift pot D-71333 will close
automatically, isolating the two sections.

o A safety valve between the first lower hopper D-71304 and the
first lift pot D-71305 is also provided to isolate the regenerator
R-71301 from the nitrogen gas system.

o In the same manner, a pressure differential is maintained


between the lock hopper
D-71302 and the top of the regenerator by a small flow of
nitrogen to prevent oxygen from entering the nitrogen gas
system.

o DN50 lines are installed between the first upper hopper D-


71310 and the reduction chamber D-71311 and between the
fourth lower hopper D-71323 and the fourth lift pot D-71333.
This way the pressure balance is made through small DN50
pipes full of catalyst, so that a very small flow of gas is
sufficient to create a significant pressure drop.

2.1.7.7. Catalyst addition and draw-off

 Catalyst can be added while the regeneration loop is in operation.

 This operation is performed in the Lock Hopper D-71302 : fresh


catalyst is introduced in the Lock Hopper through the cat-feeder which
allows to introduce one drum of catalyst without depressurization of
the Lock Hopper, and then transferred as usual down to the
regenerator
R-71301 where it will be dried before entering the reaction section.

 During exceptional withdrawal operations when functioning, the Lock


Hopper, full of spent catalyst, is isolated and depressurized to
atmosphere. The spent catalyst is then withdrawn from the unit by the
way of the side connection located underneath the lock hopper D-
71302. It goes down to the ground through a DN50 line and is
collected and stored into drums, previously filled-up with nitrogen.
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2.2. Catalyst Elutriation System


During long term the catalyst circulation and the regeneration, some catalyst
breakage may be foreseen, particularly when the catalyst circulation is unstable, or
the regeneration operation is not correctly tuned.

To avoid the reactors and regenerator basket screens plugging, two catalyst
elutriation systems are installed on the catalyst loop.

The first one, using the up-flow design (which requires less elutriation gas), is
installed at the inlet of the regeneration section (at the top of the upper surge drum)
to remove catalyst fines.

The second one, using the down flow design, installed before the reaction section (at
the top of the first upper hopper) to remove catalyst fines and ships

2.3. CCR Gas Atmospheres


The CCR unit can be separated into three different gas atmospheres, involving
oxygen, nitrogen and hydrogen (+ hydrocarbons). During a cycle, catalyst circulates
through these different gas atmospheres.

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Oxygen atmosphere, including the whole regenerator, except for the top part used
for a temporary storage of the spent catalyst. An entering nitrogen stream ensures
the seal function.

Nitrogen atmosphere, including the upper surge drum, the lock hopper, the top of the
regenerator, the first upper hopper, the first and last lower hoppers, and the first and
last lift pots. The seal function is ensured by a nitrogen gas stream leaving this zone.

Hydrogen rich gas atmosphere, including the upper hoppers (except for the first), the
reduction chamber, the reactors, the second, third, and fourth lower hoppers and lift
pots. In this zone, reactors are special areas allowing, in addition to hydrogen, the
presence of hydrocarbon molecules.

The three atmospheres are safely operated using:


 Nitrogen and Hydrogen Sealing system
 Safety Interlock System

The CCR atmospheres in a 4 reactors system

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3. Catalyst
The CCR reforming catalyst consists of metals impregnated on an alumina base. A wide
variety of metals can be used, but platinum is the chief metal. The alumina base acts as a
support for the metal. the alumina is also a support for chloride.

In reforming reactors, both the metal and the chlorided base help catalyze desirable
reactions. The chlorided alumina acid function catalyzes isomerization and cracking
reactions.

Optimum catalyst performance requires a proper balance of these two catalytic functions.
too much or little of one or the other will upset the selectivity and activity of the catalyst.
As a result, the performance of the catalyst will suffer.

The operation of the Catalyst regeneration section has a great effect on the proper
balance of the metal and chloride functions. Each of the four main steps of catalyst
regeneration must be done well to insure the proper balance is maintained. Proper
operation of the Catalyst regeneration section will help insure optimum performance of
the catalyst and long catalyst life.

In addition to its optimum catalytic properties, the catalyst also has strong physical
properties. It is specially made to resistant to attrition. Proper construction and operation
of the Catalyst regeneration section will help preserve the good mechanical strength of
the catalyst and minimize attrition.

4. Chemistry
The Catalyst regeneration process is a four-step (excluding cooling here) process where
the desirable regeneration reactionsare completed on the catalyst. The operating
conditions for each are designed to favor certain chemical reactions. Each step is
important in its own right, and all four steps must be performed correctly. The goal is to
restore the catalyst to a condition that is close as possible to that of fresh catalyst. the
basic regeneration chemistry is the same for all regeneration sections.

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Spent Catalyst
O2 Combustion

O O
O O
Pt Pt
Cl OH
Pt Pt Pt

Al2O3
Chloride
Compound Oxychlorination
+ O2 + H2O
Reactors
Cl Cl
Pt
OH Cl
O O

Al2O3

O2 Calcination

Cl Cl
Pt
OH Cl
O O

Al2O3

+ H2 Reduction

H H

Pt Pt OH Cl

Regenerated Catalyst

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4.1. Coke Burning


The first step burns coke off the catalyst. Coke burning takes place with oxygen by
the combustion reaction. It makes carbon dioxide and water and gives off heat
(exothermic):

Coke + O2  CO2 + H2O + Heat

This reaction is necessary and desirable to remove coke, but it can easily damage
the catalyst. It results in a temperature rise on the catalyst, and high temperatures
greatly increase the risk of permanent damage to the catalyst. So the burning must
be controlled. This is done by controlling the oxygen content during the burn. High
oxygen makes the burn temperatures high. But low oxygen makes the burning too
slow.

4.2. Oxychlorination
The second step adjusts the chloride content and oxidizes and disperse the metals
(i.e., platinum) on the catalyst. These reactions take place by complex reactions with

oxygen and an organic chloride compound. These reactions need both oxygen and
chloride. The chloride adjustment reactions can be summarized as follows:

Chloride Compound + O2  HCl + CO2 + H2O

HCl + O2  Cl2 + H2O

Base-OH + HCl  Base-Cl + H2O

Chloride is needed on the catalyst to keep the proper activity of the acid function.
But too much or too little chloride will have undesirable effects in the reforming
reactors. So the amount of chloride on the catalyst must be controlled. This is done
by controlling the injection rate of the chloride compound.

The oxidation and redispersion reactions can be summarized as follows:

Metal + O2 Cl2 Oxidized Metal (dispersed)

More evenly distributed metal on the catalyst surface results in better metal function
of the catalyst. The conditions that promote proper oxidation and re-dispersion of the
metal are high oxygen concentration, adequate residence time, correct temperature,
and correct chloride concentrations.

4.3. Calcination
The third step dries excess moisture from the catalyst. Excess moisture is present
from the coke burning step. Drying occurs when a hot, dry gas flows cross the
catalyst, removing water from the catalyst base:

ISSUE DATE: 20/03/06 - 21 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION BASIC KNOWLEDGE
CCR UNIT KRCIM 71300.02 REV.0

Base- H2O + Dry Gas  Base + Gas + H2O

The drier the catalyst is before it re-enters the reforming reactors, the better its
overall performance will be. This drying step is favored by high temperature,
adequate drying time, and adequate drying gas flow rates.

4.4. Reduction
The fourth step converts the metals from the oxidized state to a reduced state. This
must be done after the oxychlorination step to return the metals to a state that is
optimum before returning the reforming reactors. The reduction reaction takes place
with hydrogen by the following reaction:

Oxidized Metal + H2  Reduced Metal + H2O

The more complete the reduction, the better the metal will perform in the reforming
reactors. The conditions that favor this reaction are high hydrogen purity, sufficient
reduction chamber temperature and reduction gas flow rates adequate to ensure
good gas distribution.

ISSUE DATE: 20/03/06 - 22 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71300.03 REV.0

Contents: The information described hereafter concern the preliminary operations


prior to the first start-up of the Unit, that is those activities required to
bring the facilities to a "ready for Commissioning" condition after
Construction Completion. At that stage these Precommissioning
activities are implemented by the Construction Contractor
Precommissioning team, as they are part of his scope of work and
responsibility, and witnessed by KRC Personnel.
Unit operators may have to repeat some of the specific prior-to-start-up
activities detailed here, which are fully integrated in the start-up
sequence of this Unit, during subsequent Start-Up, especially after major
overhaul. The following topics are discussed:

1. Plant Inspection
2. Cleaning of Piping and Equipment

1. Plant Inspection
In addition to all points mentioned under same heading in KRCIM 71200.04, catalyst
regeneration section should be specifically inspected for the following:

1.1. Reactors
 The status prior to inspection is supposed to be as follows: reactor is erected
with all its internals installed. Piping is connected.
 Enough clearance must have been provided around the top of each reactor to
allow for the removal of the inlet elbow.
 Four catalyst pipes from the upper hoppers will be dismantled to ease the
removal of the inlet elbow. The inlet distributor is removed then and checked
for size and positioning.
 Air must be circulated through the reactor to allow for entry.

1.1.1. Upper section


 The sealing rings around the catalyst feed pipes must be checked for
free movement.
 Clearance between the various pieces must be checked. The
thermocouples, if any, must also move freely in the cover plate and their
dedicated seal ring must slide along the thermowell pipe.
 Remove four cover plates and one or two conical sectors in order to
access the space allowed for catalyst.

ISSUE DATE: 20/03/06 - 23 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71300.03 REV.0

1.1.2. Outer catalyst support grid or scallops


 The outer support or scallops grid will be checked for compliance with
AXENS's specifications.
 The clearance between the vertical wires of the screen is checked, for
conformity, using a random method. The screen will also be inspected
for abnormal wave amplitudes. They are the main causes of future
deformation.
 The concentricity of the grid is checked at the top part. The mobile
centering pieces are adjusted in order to have 10 mm between the edge
of the pieces and the shell.
 For the bottom part of the screen the bolts must be untightened in order
to check the clearance between the support ring and the lower flange of
the screen. Concentricity of the bottom part is checked at this occasion.
 Bolts are tightened according to AXENS's recommendations i.e. tighten
the bolts on the spacers not on the support ring. This is to provide for
thermal expansion of the outer grid (heating and cooling of the catalyst
beds).

1.1.3. Center pipe


 The center pipe is checked for its compliance with AXENS's
specifications.
 The clearance between the vertical wires is checked for conformity,
using a random process. Abnormal wave shapes could affect catalyst
circulation.
 Check the following:
o Holes in the perforated pipe must not be blinded by the
reinforcement bars of the screen.
o The three pins for the center pipe orientation are in place and
fastened with the keys.
o The seal rings in the lower centering ring are correctly fitted in
their groves.

1.1.4. Catalyst pipes


 Clean the catalyst pipes (reactor top and bottom) to remove debris,
scales etc.
 Calibrate each pipe individually, using for instance a calibrated ball. This
is to ensure the smooth finish of the weld -as recommended by AXENS-
is met.
 For the upper hopper catalyst pipe, remove the top section of the
hopper, check the catalyst pipe size and finish, check that the drum is
clean, and that the ring is the right one.

ISSUE DATE: 20/03/06 - 24 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PREPARATION FOR INITIAL START-UP
CCR UNIT KRCIM 71300.03 REV.0

1.2. Regenerator
 If the removable parts of the regenerator are not installed yet, they will be
cleaned, checked on ground and preassembled before being fitted in. If they
are already installed, they will be inspected from inside.

1.2.1. Upper manhole MH1:


 Open and check cleanliness.

1.2.2. Other manholes MH2, MH3, MH4, MH5:


 Check overall cleanliness.
 Check fixation and centering of the central collector.
 Check fastening of the internal catalyst support grid on the central
collector.
 Check concentricity of external and internal catalyst support grid.
 Check that the partitions trays between the different sections are
properly fixed.
 Check free movement of slide rings fitted on internal catalyst pipes.
 Check oxychlorination inlet and outlet screens.

1.3. Columns And Drums


Special attention is drawn to the following drums
 All drums in catalyst circulation (hoppers, lift pots...).
 The regeneration washing drum and tray arrangement.

Before closing the manholes of the equipment, a last inspection is carried out. The
aim is to check the presence of foreign bodies inside the equipment and to see
whether internals such as wire mesh, compartments, trays, vortex breakers, length
and position of the thermocouples, reflux and feed distributors, etc.. have the right
size and are properly fitted.

1.4. General Arrangement Reactor, Regenerator, Catalyst Circulation


The layout of the various equipment in the reaction section and regeneration section
including catalyst lift lines are checked for compliance with AXENS's requirement
with regard to their respective and relative elevation and slope (mainly for catalyst
circulation). The clearance and the access for dismantling critical parts for catalyst
loading/unloading is also checked.

1.5. Lift Pipes And Catalyst Pipes


The smooth finish of these pipes is of paramount importance to avoid excessive
catalyst attrition which is the source of various troubles.
AXENS has issued recommendations for the lift pipes isometrics as well as for the
quality of weld finish.
All defaults must be corrected prior to catalyst circulation startup.

2. Cleaning of Piping and Equipment


Proceed as per instructions under same heading in KRCIM 71200.04

ISSUE DATE: 20/03/06 - 25 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

Contents: This instruction outlines the procedure for the start-up of the CCR
regeneration Unit. The text includes:

1. Start-Up Requirement
2. Unit Purging
3. Initial Leak Test
4. Unit Dryout
5. Catalyst Loading
6. Second Leak Test And Partial Inerting
7. Unit Start-up
8. Catalyst Regeneration Section Shutdown

1. Start-Up Requirement
1.1. All overhaul activities and technical modifications influencing Start-up are completed.
All units, removal of equipment and pipeline blinds conform to process requirements.
1.2. Pressure gauges and safety valves are checked. Replacement work and installation
is completed.
1.3. All chemical raw materials are ready and sufficient.
1.4. All process lines and equipment has been purged, qualified in pressure test and
undergone final inspection according to the following procedures.
1.5. Disassembled or replaced equipment flanges are padded and screwed uniformly.
1.6. Safety valves in good condition and its set pressure meet the requirement.
1.7. Close all atmospheric relief valves and drain.
1.8. Verify all instruments are in good condition.
1.9. Utilities services are working normal.
1.10.Ensure complete fire appliances, place inflammables and explosives in fixed area,
clean sundries on site.
1.11.Contact dispatch, maintenance department, fitters, electrical maintenance and lab.
Complete corresponding support work.
1.12.Complete and examine all Start-up schemes, planning diagrams, all related
procedures sheet and work permits.
1.13.All maintained and revamped equipment has acceptance qualification sheet.
1.14.Inspection of the unit is done according to “Plant Inspection” procedure in (KRCIM
71300.04)

2. Unit Purging
2.1. Purging objective
2.1.1. Eliminate welds rods and slags, abrasive dusts, oxides and in general other
substances which might impede the normal unit operation or damage the
equipment (valves, pumps, compressors, turbines, etc.)
2.1.2. Timely find existing problems through process line. Ensure system operability.
2.1.3. Make operators further understand field flow path.

ISSUE DATE: 20/03/06 - 26 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

2.2. Preparation work before purging


2.2.1. All equipment and pipelines belonging to this unit should be inspected carefully
according to purging route before purging; any reassembled or newly installed
equipment should be repositioned completely; any problem found should be
handled in time.
2.2.2. Contact with dispatch to prepare steam and water supply.

2.3. Notices For Purging


2.3.1. Proceed with purging and flushing of the unit according to instructions in
“Cleaning of Equipment and Pipeline” in (KRCIM 71200.04).
2.3.2. Media used for flushing and purging
 Pipeline for handling liquid should be flushed with water; except that
condensed water system uses condensed water for flushing, others use
fire water for flushing.
 Pipeline for handling gas should be flushed with air or nitrogen;
instrument’s pneumatic line should use purified air for purging.
 Steam pipeline should use steam of corresponding pressure level for
purging according to different pressure levels.

ISSUE DATE: 20/03/06 - 27 -


KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

2.4. Purging Scheme

2.4.1. Purging of regenerator pipeline


Inject nitrogen from K-71301 inlet→K-71301A/B bypass →200-P-713017→200-P-713023→E-71301 inlet flange disconnects (purge up-
to-standard and then re-connect) →200-P-713024→H-71301 inlet flange disconnects (purge up-to-standard and then re-connect) →250-
P-713025→200-P-713030/200-P-713031→R-71301 1st bed inlet flange disconnects (blowing-up purging)

2.4.2. Purging of inlet pipelines of oxychlorination/calcination zones


N2 from K-71301 inlet →K-71301A/B →200-P-713017→80-P-713019→
80-P-713040→ disconnect check valve at air injection line and discharge steam
→E-71302 shell side inlet flange disconnects (purge up-to-standard and then re-connect)→
100-P-713041→80-P-713042→FV3009 bypass→80-P-713043 →20-SW-713013→water injection non-return valve reverses
→FT3108
bypass→P-71303A/B outlet non-return valves disconnect for purging
→PSV-71308/9 safety valves bypass →T-71302 top disconnects and
discharge steam
→80-P-713044→H-71303 inlet flange disconnects for purging (purge
to be up-to-standard and then re-connect) →80-P-713049→disconnect
inlet flange in oxychlorination zone
→chlorine injection non-return valve
reverses →FT3110 bypass →P-
71304A/B outlet non-return valves
disconnect for purging →PSV-
71310/11 safety valves bypass →T-
71303 top disconnects and discharge
steam
→80-P-713045→FV3019 bypass →80-P-713046→H-71302 inlet flange disconnects (purge to be up-to-standard and
then re-connect) →disconnect flange at calcination inlet

ISSUE DATE: 20/03/06 - 28 -


KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

2.4.3. Purging of quench gas pipeline


N2 from K-71301 inlet →K-71301A/B bypass →200-P-713017→100-P-713020→TV3003 bypass →
100-P-713021→250-P-713034→regenerator’s 1st bed outlet flange disconnects (blowing-up purging)
→250-P-713022→regenerator’s 2nd bed inlet flange disconnects(blowing-up purging)
→non-return valve of 2nd bed air injection line disconnects

2.4.4. Purging of regenerator outlet pipelines


N2 from K-71301 inlet →K-71301A/B bypass →200-P-713017→150-P-713026→FV3004 bypass →
150-P-713027→PDV3003A bypass →250-P-713028→E-71301 tube side inlet flange disconnects for purging (purge to be up-to-standard
and then re-connect) →250-P-713039→250-P-713037/8→regenerator burning zone outlet flanges disconnects for
purging (blowing-up purging)
→100-P-713048→PDV3003B bypass →100-P-713047→E-71302 tube side inlet flange disconnects (purge to be up-to-
standard and then re-connect) →100-P-713056→100-P-713054/5→outlet flanges in oxychlorination zone disconnects
(blowing-up purging)

2.4.5. Purging of regeneration gas pipeline to D-71306


Inject nitrogen from K-71301 inlet →K-71301A/B bypass →200-P-713017→150-P-713026→FV3004 bypass →150-P-713027→250-P-
713029→300-P-713008→E-71303 tube side inlet flange disconnects for purging (purge to be up-to-standard and then re-connect)
→300-P-713009→D-71306 inlet flange disconnects for purging (blowing-up purging)

2.4.6. Purging of pipeline from D-71306 to K-71301


Inject nitrogen from K71301 inlet →250-P-713015→250-P-713010/1→250-P-713010→D-71306 inlet discoannects flange for purging
(blowing-up purging)

2.4.7. Flushing of D-71306 water injection line


Introduce soft water at P-71305A/B inlets →50-SW-713003→D-71306 inlet disconnects flange for water flushing. (Flush to up-to-
standard and then re-connect flange)

ISSUE DATE: 20/03/06 - 29 -


KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

2.4.8. Flushing of P-71301A/B and P-71302A/B outlet and inlet pipelines and D-71306 outside pipeline
 Inject soft water into D-71306; when liquid level reaches a certain height, discharge it through upper and bottom liquid
level glasses simultaneously, and flush middle and bottom outlet pipelines.
 After D-71306 establishes liquid level, flush P-71301A/B inlet pipelines to clean, then, start up P-71301A/B to flush the
water in pump outlet pipeline, disconnect it at alkali-injection nozzle for discharging.
 Inject water into T-71301 to a certain liquid level, flush P-71302A/B inlet pipelines to clean, then, start up pump to flush
pump outlet pipeline, disconnect it at alkali-injection nozzle for discharging

2.4.9. Purging of burning air pipeline


Introduce air into unit →K-71304A bypass →80-IA-713003/4→E-71308 shell side inlet disconnects for purging (purge to be up-to-
standard and then re-connect) →D-71342 inlet flange disconnects for purging (purge to be up-to-standard and then re-connect) →D-
71342→80-IA-713009→UV3015 disconnects for purging (purge to be up-to-standard and then re-connect) →DR-71302 inlet flange
disconnects (purge to be up-to-standard and then re-connect) →
80-IA-713010→40-IA-713011→FV3007 bypass →40-IA-713014→UV3016 disconnects for purging (purge to be up-to-standard and then
re-connect)
→discharge steam at non-return valve
→40-IA-713015→UV3017 disconnects for purging (purge to be up-to-
standard and then re-connect)→ discharge steam at E-71301 inlet
→50-IA-713012→FV3002 bypass →50-IA-713013→discharge steam at non-return valve

ISSUE DATE: 20/03/06 - 30 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

3. Initial Leak (Air Tightness) Tests

3.1. Air Tightness Objective


Air tightness objective is to further inspect the quality of valve, flange, pipeline,
equipment, and welding seam using gas media (This unit uses nitrogen) to inspect
the leak sources in the system with field observation soap test method under the
regulated pressure.

3.2. Air-Tight Preparation


3.2.1. Air tightness test must be done after unit finishes purging, the pipe fittings such
as reassembled flanges, blind plates, and orifice plates etc. repositioned, the
existing problems have been rectified and improved and all flows reset.
3.2.2. Inspect the unit’s equipment, process pipelines, flanges, washer blind plates,
valves, safety valves, instruments, motors and pumps, etc. any problem should
be solved before air tightness test begin.
3.2.3. Contact with dispatcher to put the nitrogen source for air tightness into effect so
as to guarantee there is enough nitrogen supply.
3.2.4. Contact with dispatch to make preparation for transportation assurance of air
tightness gases
3.2.5. Contact with instrument to make air tightness to instruments related equipment
simultaneously with process system.
3.2.6. Prepare air tightness tools such as precision pressure gauge, spanner, soapy
water, brush, ear syringe, big and small barrels, etc. and organize personnel to
inspect and record by areas; workshop appoints special persons responsible
for handling of leakage points.
3.2.7. Inspect whether the air tightness points leak; use brush to brush soapy water or
use ear syringe to spray soapy water on air tightness points to observe whether
there is bubbles; if any, it means that the point is leakage point; then, mark it
with chalk or slate pencil and contact personnel to handle it in time.
3.2.8. For small space air tightness points, adhesive paper can be used to block the
flange, then, open a small hole on the adhesive paper, and then, inspect
whether the small hole leaks gas.
3.2.9. For the air tightness for drain points, their joints can be inserted into soapy
water for inspection.

3.3. Locations For Air Tightness Inspection


Air tightness inspection should be made to the system’s pipelines, equipment,
valves, flanges, pipe plugs, pressure gauges, instrument connecting positions,
pipeline welding seams, etc. They can be divided into reactor upper cap, lower outlet
flange, furnace inlet and outlet tubes, flanges in combined heat exchanger, high-
pressure separating tank liquid level gauge, pressure instrument flanges, etc.
according to locations.

ISSUE DATE: 20/03/06 - 31 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

3.4. Safety Considerations

3.4.1. Pressure boosting speed should be slow and air tightness test pressure should
comply with the regulations strictly without overpressure.
3.4.2. Any leak source found should be marked in time and the maintenance
personnel should be contacted for handling.
3.4.3. Pay attention to inspect whether there is interflow between systems and avoid
equipment overpressure strictly. Watch out for gas expansion in the system
and consequent equipment overpressure because of ambient air temperature
change.
3.4.4. During air tightness test, commands should be given uniformly and personnel
in all areas should contact with each other.
3.4.5. During air tightness test of each system, at least two pressure gauges should
be used to observe pressure with required pressure gauge precision of
magnitude 0.4, 1.5-2 times of the highest air tightness pressure.
3.4.6. Handling of leak sources under pressure is not allowed.

3.5. General Instructions

3.5.1. Initial leak tests will be performed under KRC or Engineering company
responsibility and the general instructions hereunder shall only be used as a
reminder.
3.5.2. The initial leak tests can be performed using air or nitrogen depending upon
local facilities. The test pressure will be the air or nitrogen system pressure or
the unit (or section of unit) design pressure, whichever is the lower.
3.5.3. The unit is isolated with blinds from adjacent sections containing hydrocarbons
(liquid or gaseous), and from utilities systems where pressure is lower than air
(or nitrogen) pressure.
3.5.4. The pressure rise must be checked on several manometers and possibly
checked on a pressure recorder. Leaks must be carefully located and
tightened. Their location must be recorded.
3.5.5. The leak test is satisfactory when the pressure decrease is lower than
0.005 MPa/hour over a period of 4 consecutive hours.
3.5.6. The air (nitrogen) used for leak tests should be purged out of the unit using low
points drains to remove free water, if any.
3.5.7. For the purpose of leak tests the unit will be divided into sections of
approximatively the same design pressure, as defined hereunder. Air (nitrogen)
will be injected at different locations depending upon check valves.

ISSUE DATE: 20/03/06 - 32 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

3.6. Recommended Sections For Leak Tests


For the purpose of leak testing reforming unit 71200 & Catalyst regeneration and
circulation unit are divided into the following sections.

A Reaction section (DWG. ReactionLEAK in KRCIM 71200.05)


The following vessels with their connections are included:
 The reactors, R-71201/202/203
 The upper hoppers except the first upper hopper, D-71312 & D-71313
 The balance drums, D-71352 & D-71353
 The lower hoppers, except the first, D-71321 & D-71322 & D-71323
 The reduction chamber, D-71311
 The heaters, E-71301/302/303/304
 The feed/effluent exchanger E-71201 (welded plate type, special care must be
taken),
 The reactors effluent air cooler, A-71201
 The separator drum, D-71201
 The lift pots, except the first and last ones, D-71331 & D-71332
 H2 lift lines, heat exchangers, E-71304/305
 H2 rich gas compressors KO drum. D-71207

In addition, all utilities lines, especially the ones connected to the flare and fuel gas
networks (including safety valves) will be fitted with blind flanges.
The reaction section is isolated as described on the following attached scheme.

The points of isolation are indicative only and must be reviewed on-site, to take into
account actual piping arrangement.

B Recontacting section (DWGS. RecontactLEAK1/RecontactLEAK2 in KRCIM


71200.05)
The following vessels with their connections are included:
 The recontactor feed air cooler, A-71204
 The chloride absorber, D-71206A/B
 The recontacting drum. D-71203

In addition all utilities will be fitted with blind flanges.


The absorber section is isolated as shown on the following attached schemes.
Note: The interstage aircooler and the interstage drum of the booster compressors
are to be tested separately.

C Stabilization section (DWG. StabilizationLEAK in KRCIM 71200.05)


The following vessels with their connections are included:
 The stabilizer absorber, D-71205
 The stabilizer feed / bottom exchanger, E-71208 A/B/C/D
 The stabilizer, C-71201
 The stabilizer reboiler, F-71205
ISSUE DATE: 20/03/06 - 33 -
KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

 The reformate trim cooler, E-71203 A/B


 The stabilizer overhead air cooler, A-71202
 The stabilizer reflux drum, D-71204

In addition all utilities will be fitted with blind flanges.


The stabilization section is isolated as shown on the following attached
scheme.

D Nitrogen section (DWG. NitrogenLEAK in KRCIM 71200.05)


The following vessels with their connections are included:
 The nitrogen lift gas lines,
 The first upper hopper, D-71310
 The first and last lift pots, D-71305 & D-71333
 The first and last catalyst lift pipes,
 The nitrogen loop trim cooler E-71306, storage cooler E-71307 and
storage drum, D-71341
 The upper surge drum, D-71301
 The catalyst fines filters, M-71302/303
 The nitrogen compressors KO. drum. D-71307

In addition all utilities will be fitted with blind flanges.


The nitrogen section is isolated as shown on the following attached scheme.

E Regeneration loop (DWG. RegenerationLEAK in KRCIM 71200.05)


The following vessels with their connections are included:
 The lock hopper, D-71302
 The burning, oxychlorination and calcination heaters, H-71301/303/302
 The regenerator and first lower hopper, R-71301 & D-71304
 The burning feed/effluent exchanger, E-71301
 The calcination feed/effluent exchanger, E-71302
 The regeneration loop trim cooler, E-71303
 The washing drum, D-71306
 The regeneration gas dryer package, DR-71301
 The air trim cooler E-71308, dryer drum D-71342 and dryer DR-71302.

In addition all utilities will be fitted with blind flanges.


The regeneration loop section is isolated as shown on the following attached
scheme.

ISSUE DATE: 20/03/06 - 34 -


KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

3.7. Leak Test Procedure

Nitrogen Section
Airtightness requirements and standard
 The airtightness media is nitrogen. The pressure tapping point for
airtightness of this part uses pressure of N2 compressor knockout drum
D-71307 as reference, namely, the highest operation pressure in D-
71307 of 0.225MPag.
 Airtightness standard

Static
Pressure Constant
Airtightness Airtightness allowed
boosting pressure
part phase pressure
MPa(G) speed time
MPa/5min h
drop
MPa/h
Nitrogen 0.225 0.1 8 0.005

Regeneration Section
Airtightness requirements and standard
 The airtightness media is nitrogen. The pressure tapping point for
airtightness of this part uses pressure of washing drum D-71306 as
reference, namely, the highest work pressure of 0.445MPa.
 Airtightness standard

Air tightness Air tightness Pressure Constant Allowed


section phase boosting pressure static
MPa g speed time pressure
MPa/5min h drop
MPa/h
Regeneration 0.445 0.1 8 0.005

Chronologically, once the initial leak tests are over, the drying out of the
unit takes place, prior to catalyst loading.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

4. Unit Drying
4.1. Drying Objective:
Reaction, catalyst circulation and regeneration sections must be dried out prior to
catalyst loading, firstly to avoid damaging the catalyst with water, secondly to
shorten the duration of the low severity operation after first oil in.

4.2. Drying Procedure Outlines


4.2.1. Unit dry out is conducted simultaneously with the heater refractory drying.
4.2.2. The dry out operation is carried out using hot nitrogen circulating in two loops,
physically separated. Temperature profile should strictly follow up the following
diagrams:
 Regeneration section drying curve (DWG. RegDryout)

4.2.3. The first loop uses the recycle compressor, the hydrogen rich gas compressor
and the nitrogen lift gas compressor and includes the reaction section,
absorber section and nitrogen section as defined above in chapter 3.6
"Recommended sections for leak tests". The fired heaters are used for warming
up.
4.2.4. The second loop is the regeneration section (regeneration section as defined in
3.6 "Recommended sections for leak tests") and uses the regeneration loop
compressor to circulate nitrogen which is heated in the electrical heaters
(burning, oxychlorination and calcination heaters). The regeneration drying loop
is isolated from the previous one by the special gas tight valves between the
lock hopper and the upper surge drum and the valve on the seal leg between
the first lower hopper and its lift pot.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

4.3. Preparation Work Before Unit Drying:


4.3.1. All TIs and TRs (in the firing box, in the process fluid, tube skin) have been
checked. The burners, dampers, control and safety systems have been
checked. All safety measures and control normally involved in the firing of
heaters must be followed in agreement with KRC or heaters manufacturer
procedures.
4.3.2. Make a list of required instruments and check that they are connected and in
service.
4.3.3. Check that orifices plates are installed where required and correctly calibrated
(coefficient adjusted for nitrogen) check that all safety valves are installed and
connected to atmosphere.
4.3.4. Make sure that all blinds between reaction section and Recontacting section
are removed.
4.3.5. The following compressors must be commissioned prior to start (blinds will be
removed and left in open position):
 Regeneration loop compressors K-71301 A/B

4.4. Drying Of Catalyst Regeneration Section


4.4.1. Typically, the drying of all the sections take place at the same time. However
the drying of the regeneration section may also be carried out separately. For
drying of reaction, recontacting and nitrogen sections please refer to chapter 4
of KRCIM 71200.05.
4.4.2. Drying procedure
4.4.2.1. Status:
The section is fully isolated from the reaction- recontacting - nitrogen
section by the special tight valves on top of the lock hopper
UV3001/UV3002 and by the valve on the seal leg UV3005 (on the lower
hopper bottom pipe)
4.4.2.2. When the equipment of the regeneration loop is lined-up, the regeneration
loop compressor K-71301 is pressurized up to 0.6 MPa (g) with nitrogen,
open the valves at suction and discharge of the regeneration compressor.
Make sure the system pressure is not lower than 0.3 MPa.
4.4.2.3. Start the machine and load the valves to circulate the gas, establishing
flows equivalent to design values, to the burning and to the
oxychlorination/calcination zones. Flow regulation requires, H-71301 flow
is 4870Nm3/h, H-71302 flow 245Nm3/h, H-71303 flow 230Nm3/h. When
circulation is established, drain free water from low points.
4.4.2.4. Switch-on heaters H-71301/H-71302/H-71303 and bring temperatures up,
at a rate of 20°C per hour, until the regenerator inlet temperature reaches
200°C.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

4.4.3. Follow-up and end of drying (Above DWG.RegDryout)


4.4.3.1. A procedure similar to the reaction section drying will be followed (rate of
temperature increase: 20°C per hour), except that the temperature is
limited to 400°C for the regeneration section.
4.4.3.2. After reaching 400°C with a total water draw off less than 1.0 liter per
hour, the temperature is lowered to 200°C, then heaters are switched off
and nitrogen circulation continued until the regenerator cools down to
40°C. Then nitrogen is replaced by air and the atmosphere checked
suitable before allowing entry to the vessels.
4.4.3.3. Reactors, regenerator and vessels are now ready for inspection
(thermal expansion of internal devices) and for catalyst loading.

5. Catalyst Loading
Please refer to chapter 5 of KRCIM 71200.05

6. Second Leak Test And Partial Inerting


6.1. After the catalyst loading, the reaction section and the regeneration section must be
leak tested again to inspect the removed positions for catalyst loading.
6.2. Leak test is combined with partial inerting: the objective is to reach an oxygen content
between 2 and 5% for the purpose of catalyst circulation. This is achieved by
successive pressurizations and depressurizations with nitrogen.
6.3. Leak test (using nitrogen):
 Reaction section, regeneration section and absorber section are isolated from
the rest of the unit. All pumps and compressors (suction / discharge valves) are
isolated.
 All connections to the flare are blinded.
 All safety valves are connected to atmosphere, if not possible, the collector to the
flare is blind to battery limit.
 Blind the hydrogen lines from the HP absorber to fuel gas system, to
downstream users and all lines going out to battery limits.
 A temporary blind is installed on liquid feed line to the LPG absorber.
6.4. All sections are pressurized with nitrogen up to 0.35 MPa gage.
6.5. The test is considered satisfactory when the average pressure decrease is lower than
0.005 MPa per hour during 4 hours.

7. Startup Of The Unit


For the CCR first start-up and subsequent start-ups, please refer to KRCIM 71200.06.

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PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

8. Catalyst Regeneration Section Shutdown


 Although the operation of the regeneration section on one hand and of the catalyst
circulation on the other hand are quite independent, it is recommended to start up
and shut down these sections in a proper sequence.
 Regeneration shutdown shall always lead to a simultaneous catalyst circulation
shutdown in order to avoid coked catalyst entering the calcination zone. If not,
special care will be required upon the next start up of the regeneration.
 In the case of catalyst circulation shutdown, if the operators take no action, the
oxygen requirement for combustion progressively decreases and air will be
progressively and automatically shut-off through the action of the O2 analyzer on
the air FV's. There is no harm in this situation but the entire catalyst of the
regeneration location will be fully regenerated with almost no residual coke left and
no gradient of coke content. The subsequent restart would be more troublesome.
 It is recommended to stop air injection to the regeneration, through operators
action if the catalyst circulation shutdown is expected to last more than a couple of
hours.
 Two levels of shutdown are considered: partial shutdown and total shutdown.
 A partial shutdown is undertaken when the reason is specific to the regeneration
loop and is expected not to exceed 24 hours. The policy is to maintain in operation
most of the equipment not directly involved to allow for a quick restart.
 A total shutdown of the regeneration and catalyst circulation can be caused:
o Either by a problem specific to the regeneration or catalyst circulation, of
some duration (over 24 hours). In this case the operation of the reforming
section can still be continued.
o Or by a total shutdown caused by other sections.

8.1. Partial Shutdown


8.1.1. Stop the catalyst circulation while closing FV's and PDV's to the lift pots
8.1.2. Close the two air injection FV's FV3002/3007. Keep air compressor K-71304
running using the spill-back PV3010.
8.1.3. Stop the chlorination agent and water injection pumps P-71304/303 (Inject
chlorine into reformer feed if reformer still operate).
8.1.4. Keep regeneration compressor K-71301 running
8.1.5. Keep the washing section (caustic recycle pump, water injection pump, caustic
injection pump) in normal operation.
8.1.6. Remark: If the shutdown is to last a few hours, a more efficient fines filters M-
71302/M-71303 back flushing can be performed, by decreasing lifts A-D gas
flows to 50%.

8.2. Total Shutdown


8.2.1. Close the two air injection FV's 3002 and 3007. Stop air compressor K-71304
8.2.2. Stop the chlorination agent and water injection pumps P-71303/304
8.2.3. Close the special tight manual valves below 1st and 2nd reactors and remote
operated valves (UVs) under the third reactor, the regenerator and between the
1st upper hopper and the reduction chamber UV3013/3005/3011

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION START-UP/SHUTDOWN OPERATIONS
CCR UNIT KRCIM 71300.04 REV.0

8.2.4. Decrease both electrical heaters outlet temperature to about 350°C. Then keep
the regeneration loop compressor K-71301 running to maintain about 300°C in
burning, oxychlorination and calcination beds.
8.2.5. Maintain the pressure in regeneration loop.
8.2.6. When burning and oxychlorination/calcination beds temperature are about
300°C, then:
 Stop the caustic make-up.
 Stop the caustic soda circulation.
 Stop the H2O make-up to caustic circulation.
 Stop the washing water injection.
 Stop regeneration loop compressor K-71301
 Close block valves on LV's 3001 and 3002 (washing drum bottom
outlet).
 Keep the regeneration loop under N2 pressure.
 Isolate the caustic recycle pumps P-71302, drain and wash them with
BFW.
8.2.7. Cool catalyst to below 50°C, by this time, regenerating section completely
shutdown.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

Contents: This instruction outlines the operating conditions and control of the catalyst
regeneration and circulation section. The text includes:

1. Operation Influencing Parameters


2. Principles Of Key Parameters Control
3. Special Control Systems And Safety Devices
4. Adjustment Of Operating Conditions
5. Troubleshooting
6. Analysis Control
7. Supplements

1. Operation Influencing Parameters

1.1. Catalyst Circulation and Catalyst Regeneration


Catalyst circulation and catalyst regeneration are two parameters closely linked. The
operators will have to master them in order to ensure a complete combustion of the
coke deposit without exceeding equipment design conditions.
The following must be kept in mind in order to understand how to control the catalyst
regeneration:

1.1.1. The regeneration is achieved by two steps of coke combustion, followed by an


oxychlorination and calcination step where the optimum amount of chlorine is
restored (Refer to DWG. “LoopControl” in KRCIM 71200.06).

1.1.2. The first combustion step operates with a limited inlet O2 content (0.6 to 0.8%
vol.) controlled through analyzer AIC3001 on first burning bed inlet resetting
analyzer AIC3004 on oxychlorination and calcination gas , which then resets
FIC3007 air flow. This limits the temperature increase. The 2 nd combustion step
operates with an excess of O2 (0.2 % vol. at outlet) to ensure a complete
combustion: the analyzer AIC3004 resets FIC3007 air flow.
 The regeneration is designed to burn a given amount of coke per hour.
Trying to exceed this limit results in excessive regeneration temperature and
possible catalyst damage.
 During the various steps of the regeneration, the catalyst must not be
overheated (max. temperature in calcination shall not exceed 520°C.).

1.1.3. The operators must then monitor the catalyst regeneration and set the catalyst
circulation with the following guidelines.
 A circulation rate (say between 60 - 90% of design rate) will be selected -
based on the trend in coke deposit (higher circulation when increased coke
deposit).
 Burning and oxychlorination/calcination gas flows are set to design values.
 Temperatures at burning beds inlets are adjusted through the electrical
heaters.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

 Air injections are adjusted to 0.6 - 0.8% vol. at first burning bed inlet and
0.2% vol. at second burning bed outlet.

Then operators must watch the first burning bed outlet temperature.
If this temperature is too high, the following options are possible:
 Decrease the TI at inlet temperature (not below 470°C ).
 Decrease catalyst circulation rate.
Note that if high regeneration temperature is due to an increased coke deposit
content, decreasing the catalyst circulation is only a short term solution, because
coke keeps building up, if the conditions which caused the increased coke are still
prevailing. In this case, sooner or later the severity must be lowered

2. Principles Of Key Parameters Control


The principles of the control of the operating parameters are explained below.

2.1. Catalyst Circulation


Refer to PIDs concerning reactors and catalyst circulation and Figs. 8 & 11 in
chapter 2.3 "Outline of circulation procedure and principle of catalyst transportation"
(KRCIM 71200.06).
2.1.1. The catalyst circulation rate is first set by the operators for lift A (between the
regenerator and the first reactor). Operators select the set point of PDIC3006 of
that lift.
2.1.2. The catalyst flow in the following lift i.e. lift B (from 1st to 2nd reactor) is then
adjusted through the relevant PDV3008 in order to maintain the catalyst level in
the first upper hopper. The cascade LIC3111 / PDV3008 is then set on.
Catalyst flow is then adjusted in the same manner in other lift pipes.
 Lift C from 2nd reactor to 3rd reactor
 Lift D from last reactor to regenerator

IMPORTANT: Catalyst inlet pipes must always be full of catalyst otherwise the
sealing system between nitrogen section and reaction section would not work. For
that purpose very low level (LALL) in regenerator upper section or in any of the
reactor upper hopper actuates the relevant "sequences" IS3014, or IS3018 or IS
3020 managing closure of the relevant lifts, i.e. stops withdrawal from the respective
reactor - through the closure of the relevant PDV on the secondary lift gas injection.

Example:
 The LALL3112 in the first reactor upper hopper actuates sequence IS3018
which closes the secondary gas injection and the relevant PDV3008 to the
first reactor lift pot and thus stops catalyst flow from this reactor.
 A high level in the upper surge drum LAHH3106 actuates sequence IS3021
which closes the secondary gas injection and the relevant PDV3011 to the
third reactor lift pot and stop catalyst flow from this reactor to upper surge
drum.

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

Catalyst circulation will be automatically shut down through any one of the following
interlocks:
 IS3019 related to N2 seal gas default to first reactor upper hopper. It closes
ON/OFF valve UV3011 between upper hopper and reduction chamber.
 IS3022 related to N2 seal gas default on the last reactor lower hopper. It
closes the ON/OFF valve UV3013 between last reactor lower hopper and lift
pot.
 IS3016 related to N2 seal gas default to first lower hopper. It closes ON/OFF
valve UV3005 between first lower hopper and lift pot.

The recommended figure for PDC3008 set point of lift A is between 0.012 to 0.020
MPa.
The PDC set points for the other lift pots are adjusted in order for the catalyst level in
the upper hoppers to stay constant. Operator must keep in mind that too high figures
for these set points may affect adversely the flow of catalyst into the lift pot, and end
up in a complete stop of the catalyst circulation.

2.2. Catalyst Regeneration

2.2.1. Coke burning


(Refer to DWG. “LoopControl” in KRCIM 71200.06)
The aim of the regeneration section is twofold:
 To make sure that the coke deposit of the catalyst is fully burnt before
entering the oxychlorination zone - otherwise temperature runaway could
occur and damage the catalyst.
 The temperaturse of the catalyst during oxychlorination and calcinations
operations are suitable to perform chlorine adjustment and catalyst
drying out.

To satisfy both criteria the catalyst is burnt in two steps:


 In the first burning zone, the amount of O2 is controlled through analyzer
AIC3001 on first burning bed inlet which resets AIC3004 on
oxychlorination/calcination gas which in turn resets FIC3007 air injection.
The TIC3001 of the inlet temperature to the first burning bed is controlled
through the electrical heater.
 In the second burning zone inlet temperature is controlled by
TIC3003 which allows quench gas from compressor discharge to adjust
the temperature at the required value. Also the amount of oxygen at 2nd
burning zone inlet is controlled through the analyzer AIC3002 which
resets FIC3002 air injection .

The oxychlorination and calcination temperatures are controlled via their


electrical heaters outlet temperatures.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

2.2.2. Pressure control and bias (Fig. 27)


Another important parameter to control is the pressure. The regenerator bottom
pressure must be maintained above the first reactor pressure to allow catalyst
lift from the regenerator to the first reactor upper hopper. In order not to upset
the catalyst flow each time the reactor pressure varies (changes in feed quality
or quantity) this differential pressure must be constant.

This is achieved as follows:


 A regeneration loop pressure controller is installed at the calcination gas
inlet to the regenerator, in order to maintain a positive DP between the
regenerator bottom and the regenerator lift pot. The set point of this
pressure controller is equal to the first reactor inlet pressure plus an
adjustable BIAS (about 0.060 MPa).
PIC 002 set point = PI 3123 + BIAS
 Once the appropriate value for the bias is selected it does not need to be
changed.

2.3. N2 Lift Gas Suction Pressure And Bias (Fig. 28)


The pressure at the N2 compressor suction drum is set by the pressure at the last
reactor outlet minus an adjustable bias -around 0.105 MPa- which is adjusted on
site.
The aim of this bias is to enable the 2 PDIC's downstream the catalyst fines filters, to
maintain the openings of the associated control valves PDV3018 and 3019 within
the middle of the range.
The bias value can be adapted to keep the PDV in an acceptable opening percent

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

Pressure
(barg)

N2 system Reaction
9.0

8.0

loop compressor
recycle compressor
7.0 top

bias 1 bottom
lift pot 1 +0.6 barg
6.0
N2 compressor

RX1
PDIC

5.0 lift pot 5


RX4 washing
drum

4.0

Recycle compressor: 35000 kg/h


ko drum separator
3.0 bias 2
-0.2 barg

Pressure
(barg)

N2 system Reaction Regeneration


9.0

8.0 loop compressor

7.0
recycle compressor

top

6.0 bias 1 bottom


N2 compressor

lift pot 1
+0.6 barg
RX1
PDIC
5.0
lift pot 5
RX4
washing
drum
4.0

Recycle compressor: 26000 kg/h

ko drum separator
3.0 bias 2
-0.2 barg

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

3. Special Control Systems And Safety Devices


The catalyst circulation in the reaction section and in the regeneration section involves a
few special control systems used in normal operation and a few safety sequences (mainly
lift shutdown sequences). Both are part of the Distribution Control System (DCS) logic.

A hardwired interlock logic (i.e. separated from the DCS) performs automatic emergency
shutdown actions upon the occurrence of potentially harmful situations.

In the DCS, four control sequences called UC (multiple variable control) have been
programmed to execute the following tasks:
 UC 1 Regeneration loop pressure control.
 UC 2 Catalyst transfer.
 UC 3 Hydrogen system pressure control.
 UC 4 Nitrogen loop pressure control (introduces automatically fresh nitrogen in the
nitrogen lift section, should the latter have been polluted with hydrogen or oxygen).

Also programmed in the DCS are sequences, related to catalyst lift pipes and their
associated lower and upper hoppers.
Upon the occurrence of undesirable event(s) such as (but not limited to) low level in upper
hoppers and high level in upper surge drum, the four relevant secondary lift gas PDV
valves would close.

Sequences result in catalyst circulation shutdown or regeneration stand by. When the
original conditions are restored the different systems affected go back on stream.
Sequences are the result and the way of correcting minor incidents but do not affect,
normally, the running of the unit.

3.1. Hardwired Interlocks


Hardwired interlocks are cabled logics aimed at performing automatically safety
tasks in case of undesirable events which otherwise could end up into:
 Damages to equipment: high level of liquid in compressor KO drums, cooler
failure.
 Damages to catalyst: recycle low flow.
 Operational hazards (related to the catalyst circulation and regeneration):
 Loss of N2 seal gas between:
o reduction chamber and upper hopper
o last reactor and its lower hopper
 Low overpressure of the N2 seal gas versus:

o reduction chamber
o first lower hopper and lift pot
 High temperature in the regenerator
Interlocks operate automatically upon the occurrence of the undesirable event(s) but
can also be activated by operators.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

4. Adjustment Of Operating Conditions

Circulation Loop
4.1. Lift Gas Flow
4.1.2. The lift gas flow needs to be adjusted each time the specific gravity of the H 2 lift
gas varies due to a change in the operating conditions.
4.1.3. This adjustment must be made to maintain a constant speed of catalyst in the
lift pipe and to prevent an excessive attrition of the catalyst.
4.1.4. The lift gas flow rate is modified as follows, in order to keep the actual lift gas
velocity constant:
Flow c = Flow r x MW
MW d x Pop Td
op Pd Top
Where: (Flow)c :corrected flow (vol.) for Pop, Top, MWop
(Flow)r :flow (vol.) reading for Pd, Td, MWd
Pop, Top, MWop :operating P, T and MW
Pd, Td, MWd :design P, T and MW for which the flow meter is calibrated
Temperature :must be expressed in R or K
4.1.5. For each change of feed quality and / or severity which can lead to a change of
the H2 rich gas composition, a lift gas flowrate check shall be made, using the
formula above to calculate the actual flow, at conditions, and the calculation
example hereunder to calculate the recommended flow.
4.1.6. When the unit operates at steady conditions a check is made once a week.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

Calculation of the recommended lift gas flow


Calculation basis
a) Lift pipe : Ø 3" - SCH 160
Ø i = 66.44 mm - S = 3.5 10-3 m2
b) Conditions
Lift gas = N2 or Hydrogen rich gas
N2=28.0
Molecular weight (MW)
H2 = to be calculated with gas chromato analysis
Pressure(P) Read at the gauges located downstream the gas
=
expressed in MPa a FV's
Temperature(T) Average temperature between lift pot and upper
=
expressed in °C hopper
MW x P x 273.15
Density at conditions
= =
(expressed in Kg/m3 (22 .414 ) x 0.1013 x (273.15 + T)
Free fall 7.67
= FF =
(FF) expressed in m/s 
Catalyst optimal velocity = 2.5 m/s
Gas lift velocity = GLV = FF + 2.5 (m/s)

Calculation examples
N2 Gas = T = 100 + 250 = 175 C
P(MPa abs) = 0.680 2
28.0 x 0.680 x 273.15
= = 5.11 Kg/m 3
22.414 x 0.1013 (273.15 + 175)
7.67
FF = = 3.39 m/s
5.11
Gas lift velocity = 3.39 + 2.5 = 5.89 m/s
Flow (volume) = 3.5 10-3 x 3600 x 5.89 = 74.2 m3/h (P and T)
Flow (weight) = 74.2 x 5.11 = 379 Kg/h
H2 Gas lift = P (MPa abs) = 0.610
T( C) = 200 + 250 = 225
2
MW = 3.9
3.9 x 0.610 x 273.15
= = 0.58 Kg/m 3
22.414 x 0.1013 (273.15 + 225)
7.67
FF = = 10.07 m/s
0.58
Gas lift velocity = 10.07 + 2.5 = 12.57 m/s
Flow (volume) = 3.5 10-3 x 3600 x 12.57 = 158.8 m3/h (P and T)
Flow (weight) = 158.8 x 0.58 = 92 Kg/h

A simple control can be done. It consists in checking the gas lift FV's and PDV's
opening. For a given catalyst flow a decrease of the lift pipe P is the consequence of
an increase of the actual lift gas flow, if all other conditions are unchanged.
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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

The graph below gives the recommended lift gas flow to maintain a catalyst velocity between
2.5 and 3 m/s, at various gas density. This graph is valid for 3" schedule 160 pipes.
Lift gas flowrate to minimise catalyst attrition
(lift pipe 3" sch.160)
500
vg=2.5m/s
vg=3 m/s

400

300
gas flowrate (kg/h)

200

100

0
0.0 1.0 2.0 3.0 4.0 5.0 6.0

gas density (kg/m3)

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

Regeneration Loop
4.2. General
4.2.1. The operating conditions of the regeneration loop are linked to the amount of
coke deposited on the catalyst and to the quantity of circulated catalyst.

4.2.2. In order to know the trends of carbon and chlorine contents, AXENS
recommends to analyze on a daily basis the carbon and chlorine on the spent
and on the regenerated catalyst and to plot on a chart the results versus time.

4.2.3. When the operating conditions are steady the coke level of the spent catalyst
shall be preferably maintained between 4 to 6% wt, depending upon the unit
capacity, the required severity and the feed quality. This is obtained through
adjustment of the catalyst circulation rate.

4.2.4. However, when operating at high severity, high flow rate and relatively poor
feedstock (paraffinic feeds), the percent of coke deposit may momentarily
exceed the above value. In this case, operators must remember that the
burning capacity of the unit is limited and that the catalyst circulation must
match the burning capacity.

4.2.5. Then catalyst circulation must not exceed the design capacity of the
circulation. The design coke burning capacity is 32 kg/h and catalyst flowrate
is 410 kg/h. Moreover regeneration temperature must be carefully watched.

4.2.6. It is obvious that, if the severity is such that the actual amount of coke build-
up is, on average, higher than the design coke burning capacity, the severity
must be lowered - or the feed rate reduced.

4.2.7. An increase of coke deposited on the spent catalyst or an increase of catalyst


circulation can lead to a prohibitive temperature increase (T°) in the burning
zone. In such a case, as the T° is related to the O2 in the burning zone, an
increase of regeneration gas flow and the decrease of the inlet O 2 analyzer
set point will decrease the T° and leave the burning quality unchanged.

4.2.8. Also care shall be taken in keeping an O2>0.2 vol. % at the 2nd burning zone
outlet, to be sure that full coke combustion takes place in the second burning
zone. Otherwise residual combustion will occur in the oxychlorination zone
inducing undesired T° and a possible shutdown by TAHH3132 and 3134
trips.

4.2.9. The quantity of air sent to the calcination zone should be higher (or equal)
than the quantity sent to the second burning zone. If necessary, analyzer
AIC3004 on the oxychlorination inlet shall be set higher to increase the air
flow to the oxychlorination (therefore to the 1st burning bed).

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

4.3. Temperatures
(Refer to DWG. “LoopControl” in KRCIM 71200.06)
Temperatures must be adjusted as follows :
4.3.1. The 1st bed inlet temperature is monitored at 480°C through the burning
heater.
4.3.2. The 2nd bed inlet temperature is adjusted at 480°C with the quench gas
recovered from the regeneration loop compressor.
4.3.3. However, the first burning zone outlet must be controlled between 535°C
to 545°C by action on inlet temperature and on inlet O 2 analyzer. Use
following rule of thumb: 0.1% O2 leads to 10°C temperature rise.
4.3.4. The temperature at the second burning zone outlet (TI3118) must not
exceed 510°C and simultaneously the outlet O2 content must be kept
above 0.2%. If the temperature exceeds 520°C one must:
 Either increase regeneration gas flow with a decrease in O2 set point.
 or increase slightly 1st bed O2 analyzers set point. It will result in a lower
T across second bed and a higher T across first bed.(This solution
only used if outlet temp of 1st bed is not already high)
 Or decrease inlet temperature into second bed(not less than 470°C)
 or decrease catalyst circulation to get the same temperature decrease.

4.3.5. Oxychlorination zone inlet temperature


This temperature is monitored by TI3005 at the outlet of the oxychlorination
heater and adjusted around 510°C through TIC3005 using the heater control.

4.3.6. Calcination zone inlet temperature


This temperature is monitored by TI3006 at the outlet of the calcination heater
and adjusted between 500°C and 520°C through TIC3006 using heater
control. If the requested temperature cannot be reached, check the PDV on
oxychlorination outlet line, tubes side outlet of calcination feed effluent
exchanger.

Note: If the differential pressure between the 2nd burning bed and the calcination
zone is set too low, some gas may flow back through the catalyst pipes to the
burning zone and the oxychlorination, calcination feed effluent / exchanger efficiency
will be reduced.

4.4. Catalyst Level In The Regenerator


The level of the upper section of the regenerator, before the transfer from the lock
hopper to the regenerator, must be monitored carefully. When it drops below 30% a
catalyst make-up is necessary.

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

4.5. Pressure
The pressure at the regenerator bottom (i.e. calcination gas inlet) is controlled
through PDV’s3002 A and B located on top of the washing drum. This pressure set
point is equal to the first reactor top pressure plus a selected increment (or bias).
The recommended value for the bias is 0.060 MPa.

4.6. Chlorination Agent Injection


Refer to 6.2.4. "Regeneration startup" in KRCIM 71200.06 for the amount to be
injected. This amount will be set by stroke adjustment of the injection pump and
checked by the calibrated gauge of the tank.

4.7. Water Injection


Refer to 6.2.4. "Regeneration startup" in KRCIM 71200.06. for the amount to be
injected. This amount will be set by stroke adjustment of the injection pump and
checked by the calibrated gauge of the tank.

4.8. Sodium Hydroxide Injection And Circulating Pump


Keep the caustic recycle pump flow close to the design figure (5550 kg/h)- whatever
the unit throughput. Add fresh sodium hydroxide to maintain 8.5 < pH < 9.5 in the
solution.
The total salt content in the circulating solution must not exceed 3% wt (expressed in
total sodium). this figure is adjusted through the quantity of water injected and
drained

4.9. Regeneration Recycle Gas Flow


Total recycle gas rate generally controlled around 1600Nm 3/h. Regeneration recycle
gas flow is divided into four ways as follows:
 Regeneration gas to 1st bed = 1180 Nm3/h
 Quench gas to 2nd bed = 162 Nm3/h
 Oxychlorination/Calcination gas = 109 + 109 Nm3/h
 Spill Back = 155 Nm3/h

4.10. Catalyst Reduction


 Reduction temperature must be 480˚C , controlled through H-71304 outlet
temperature.
 Reduction gas flow controlled by FIC3017. In normal operation it must
guarantee 100% flow design value ( 360 Nm3/ h).
 The reduction H2 gas is purified in M-71301 through membrane system to a
purity of 99 mol% and C2+ ≤0.2%.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

5. Troubleshooting
5.1. General
Mechanical troubles or failures which, hopefully do not result in immediate
shutdown, must also be considered. The most frequent are covered in this chapter:
 Failure of regeneration.
 Failure of nitrogen lift system.
 Failure of chlorine injection.
 Failure of catalyst circulation.
 Washing section default.
 Difficulties in controlling the regeneration temperatures.

5.2. High Pressure Drop In The Regenerator

5.2.1. Regenerator
An excessive pressure drop may also develop in the regenerator by the same
process as for the reactor(s).
5.2.1.1. As soon as the pressure drop reaches 0.100 MPa instead of the normal
figure of 0.002 MPa a catalyst unloading of the regenerator is
recommended. Fortunately this operation can be conducted without
shutting down the feed to the reforming unit.
 stop catalyst circulation,
 isolate the regenerator from the reaction section,
 let the regeneration loop cool down : shut down electrical heaters
and continue nitrogen circulation if applicable,
 depressurize the regenerator,
 unload the catalyst under the lower hopper,
 screen the catalyst.
 Depending upon the downtime available and the time to run until
the next planned shutdown, will decide to inspect the regenerator
or not, prior to reloading the catalyst.

5.3. Failure Of Regeneration


5.3.1. Regeneration may have to be shut down if:
 Both regeneration and air compressors failed (unlikely).
 A major leak occurred somewhere in the section.
 The regeneration gas dryer failed.
 One of the electrical heaters failed.
5.3.2. The following measures must then be taken:
5.3.2.1. Stop catalyst circulation.
5.3.2.2. If the shutdown is expected to be of long duration, close manual special
catalyst tight valves below the 1st and 2nd reactors as well as ON/OFF
remote operated valves UVs located under last reactor bottom,
regenerator bottom and between 1st upper hopper and reduction
chamber.
5.3.2.3. Keep the regenerator under pressure.

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

5.3.2.4. Stop air injection to the 1st and 2nd burning beds.
5.3.2.5. Switch off electrical heaters.
5.3.2.6. Stop caustic circulation pump, caustic injection pump, water to washing
drum.
5.3.2.7. Whenever possible, keep the regeneration section under pressure.

5.4. Failure Of Nitrogen Lift System


5.4.1. This system may have to be shut down if:
5.4.1.1. Both compressors failed (unlikely).
5.4.1.2. A major leak occurred and operation could not be sustained.
5.4.1.3. The N2 gas cooler failed (leak, cooling water default...).
5.4.2. The following measures must be taken:
5.4.2.1. Stop catalyst circulation.
5.4.2.2. Close manual special catalyst tight valves below the 1st and 2nd
reactors as well as ON/OFF remote operated valves UVs under last
reactor bottom under regenerator bottom and between 1st upper hopper
and reduction chamber.
5.4.2.3. Stop air injection to the 1st and 2nd burning beds.
5.4.3. If the shutdown is expected to be of short duration (24 hours or so).
5.4.3.1. Keep regeneration compressor on.
5.4.3.2. Maintain temperature in the regenerator beds.
5.4.3.3. Keep washing system on (caustic recycle pump, caustic injection pump,
water injection pump).
5.4.4. If the shut down is expected to be longer, proceed with total shutdown of
the regeneration section.

5.5. Failure Of Chlorine


5.5.1. If chlorine injection in the regeneration cannot be continued, stop water
injection.
5.5.2. For a few hours only: keep running without any change, the chlorine loss will be
compensated later.
5.5.3. For up to 8 hours: reduce catalyst circulation rate.
5.5.4. For more than 8 hours: proceed with regeneration partial shutdown (see 8.1
“Catalyst regeneration section” of KRCIM 71300.05) and start adding chlorine
in the feed.

5.6. Failure Of Water Injection In Oxychlorination Zone


5.6.1. If water injection in the oxychlorination gas cannot be continued:
5.6.1.1. For a few hours only: keep injecting chlorination agent, the chlorine pick-
up will be increased.
5.6.1.2. For up to 8 hours: reduce chlorination agent injection by about 20%.
5.6.1.3. For more than 8 hours: adjust the chlorine injection to reach the target
until the recovery of water injection.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

5.7. Failure Of Catalyst Circulation


5.7.1. If the expected downtime is less than 8 hours proceed with regeneration and
catalyst circulation partial shutdown.
5.7.2. If the expected downtime is more than 8 hours proceed with regeneration and
catalyst circulation total shut down (see 8.2 “Catalyst regeneration section” of
KRCIM 71300.05).

5.8. Washing Section Default


5.8.1. Due to the corrosivity of the regeneration gas, any default of the washing
section must be corrected shortly.
5.8.2. If the default cannot be fixed within a few hours, proceed with the total
shutdown of the regeneration section.

5.9. Difficulties In Controlling The Regeneration Temperature


(Refer to DWG. LoopControl in KRCIM 71200.06).
BLACK BURNING MODE
5.9.1. Not perfect combustion of the coke in the second bed, due to too high catalyst
circulation rate, or oxygen analysis failure, etc. leads to coke entry in
oxychlorination zone with an immediate temperature runaway in this area.
5.9.2. To abbreviate this problem, IS3030 switches automatically the regeneration in
black burning mode i.e.:
 UV3016 air to oxychlorination / calcination zones is closed, while
 UV3017 air to 1st burning bed is open.

Note that the modifications of the set point of FV3007 on air injection is
automatically placed under the direct control of analyzer AIC3001 at the inlet of
first burning bed.

5.9.3. If, in spite of this, temperature tends to follow its increase:


 Stop catalyst circulation to avoid more coked catalyst to ingress in the
oxychlorination zone.

 When temperature in oxychlorination zone are again normal restart gently


the catalyst circulation, then adjust it at previous conditions. Black burning
conditions can be stopped when coke at the 1st upper hopper catalyst
sampler is lower than 0.2 wt%.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

6. Analysis Control
6.1. Recommended Methods And Frequency
The frequencies given here below are related to routine operation.

Test Item Test Method Frequency


SN Stream Name
IFP SEI IFP SEI IFP SEI
SN- Washing Drum GB/T692
PH 1/D
71301 Side Water 0
SN- Washing Drum GB/T692
PH 1/D
71302 Bottom Water 0
Q/SHO1
O2 IFP 27731 Occas
8.0019
IFP 27731 or
Q/SHO1
CO2 Draeger (tube Occas
8.0019
CH 19701)
IFP 27731 or
Q/SHO1
CO Draeger (tube Occas
SN- Regneration 8.0019
CH 23501)
71303 Gases
Draeger (tube Detector
SO2 Occas
CH 24201) Tube
Draeger (ref. Detector
HCl Occas
6728181) Tube
Dew
H2O Point Occas
Meter
Regeneration Dew
SN-
Loop Dryer Inlet H2O Point 1/W
71304
Gas Meter
Regeneration Dew
SN-
Loop Dryer H2O Point 1/W
71305
Outlet Gas Meter
RIPP-
Carbon ASTM D3178 1/D
106
IFP 9303/ IFP
Chlorine RIPP-36 1/D
9304
SN- RIPP-
Spent Catalyst Sulfur IFP 9303 Occas
71308 106
Silicon RIPP-36 Occas
Iron RIPP-36 Occas
RIPP-
Sodium Occas
117

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

Test Item Test Method Frequency


SN Stream Name
IFP SEI IFP SEI IFP SEI
RIPP-
Carbon ASTM D3178 1/D
106
IFP 9303/ IFP
Chlorine RIPP-36 1/D
9304
RIPP-
Sulfur IFP 9303 Occas
106
SN- Regnerated Platinu
IFP 9405 Occas
71309 Catalyst m
Silicon RIPP-36 Occas
Iron RIPP-36 Occas
RIPP-
Sodium Occas
117
Specific Surface ASTM
BET Occas
Area D4657
Composit Q/SHO1
1/D
SN- ion 8.212
Reduction H2
71310 Detector
HCl 1/D
Tube
SN- Composit Q/SHO1
Lift N2 1/D
71311 ion 8.212
Dew
SN-
Air Dryer Outlet H2O Point 1/W
71312
Meter
Sodium Titration 1/D
Silicon
Titration 1/D
Oxide
Iron Titration 1/D
**** Saturated Steam

Copper Titration 1/D

Hardnes
******
s
Iron Titration 1/D
Copper Titration 1/D
Silicon
Titration 1/D
Oxide
Sodium Titration 1/D
Boiler Feed Dissolve
****
Water d Titration 1/D
Oxygen
PH Titration 1/D
Oil UV
1/D
Content Method
Phosphat
Titration 1/D
e
Alkalinity Titration 1/D

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

7. Supplements

Figure 27 (Regeneration Pressure Control & Bias)

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PRODUCTION & OPERATION OPERATING CONDITIONS & CONTROL
CCR UNIT KRCIM 71300.05 REV.0

Figure 28 (Lift Gas Pressure Control & Bias)

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PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

Contents: This document describes specific functions (control logics, automation


sequence..) used for the control and automation of the catalyst
regeneration and circulation loop. These functions are implemented in
the DCS system or equivalent of the unit. The text includes:

1. Control Functions
2. Catalyst Transfer Sequence Description (UC2)
3. Catalyst Circulation Control
4. Hydrogen System Pressure Control (UC 3)
5. Special Loops Description
6. Temperature Control Optimization
7. Appendix

1. Control Functions
The following control functions are necessary for the sequence and must be implemented
in the system.
1.1. Function : ON/OFF VALVE MONITORING
This function is used when one of the On/Off valves involved in the catalyst transfer
from the upper surge drum D-71301 to the regenerator R-71301 (refer to figure 1 in
appendix) is commanded.
The function executes sequentially 3 actions described hereafter.

Action 1 : Test of the valve mode


The mode of an On/Off valve determines who has the control on the valve. A valve
in AUTO mode is commanded by the sequence and a valve in MANUAL mode is
commanded by the operator (during maintenance operation, for example). The
valves are normally in AUTO mode but the operator is allowed to switch at any time
to MANUAL mode.
For a sequence command, the function does the test as follows :
 If the valve is in AUTO mode :
o the treatment of the command continues normally
 If the valve is not in AUTO mode :
o the sequence is stopped (frozen).
o a message is displayed to request the operator to set the valve in
AUTO mode.
Example : "SET VALVE UV 001 IN AUTO"
o the operator must acknowledge the message
o when the valve mode has been changed, the operator must
acknowledge to restart the sequence : the sequence restarts and tests
again the valve mode.
For an operator command, the function does the test as follows :
 If the valve is in MANUAL mode :
o the treatment of the command continues normally
 If the valve is not in MANUAL mode :
o no treatment : the operator must change the valve mode.
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PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

Action 2 : Test if the command is allowed by the software interlocks


The valve operations are protected by interlocks (described in the paragraph
2.7 "Software interlocks"). They filter both the operator commands and the sequence
commands.
For a valve sequence command, the function does the test as follows :
 If the command is allowed by the interlocks :
o the treatment of the command continues normally
 If the command is not allowed by the interlocks :
o the sequence is stopped (frozen).
o a message is displayed. Example : "UV 003 NOT ACTUATED DUE TO
INTERLOCK"
o the operator must acknowledge the message
o when the problem has been solved, the operator must acknowledge to
restart the sequence
o the sequence restarts and tests again the interlock.
For a valve operator command, the function does the test as follows :
 If the command is allowed by the interlocks :
o the treatment of the command continues normally
 If the command is not allowed by the interlocks :
o a message is displayed. Example : "UV 003 NOT ACTUATED DUE TO
INTERLOCK"
o the operator must acknowledge the message
o when the problem has been solved, the operator must reenter the
command

Action 3 : valve discrepency test


The function tests the limit switch open (ZSO) and the limit switch close (ZSC) in
order to check if the valve has moved to the requested position.
A time (noted feedback time) is allowed for each valve to match the requested state.
If after the feedback time, the valve still does not match the requested state, the
valve is considered as failed.
Depending on the valve command, the valve is declared FAILED TO OPEN or
FAILED TO CLOSE. The discrepency can be due to a valve failure (valve blocked or
moving too slowly) or to a limit switch failure.

For a valve requested to open : (FB: feedback time)


Time (t) Limit switches state Valve state
ZSO ZSC
t=0 0 1 Valve CLOSE
t < FB 0 0 Valve MOVING
t ≥ FB 1 0 Valve OPEN
t ≥ FB 0 0 Valve FAILED TO OPEN (valve or limit switch
failure)
t ≥ FB 0 1 Valve FAILED TO OPEN (valve failure)
t ≥ FB 1 1 Valve FAILED TO OPEN (limit switch failure)

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PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

For a valve requested to close : (FB: feedback time)


Time (t) Limit switches state Valve state
ZSO ZSC
t=0 1 0 Valve OPEN
t < FB 0 0 Valve MOVING
t > FB 0 1 Valve CLOSE
t ≥ FB 0 0 Valve FAILED TO CLOSE (valve or limit switch
failure)
t ≥ FB 1 0 Valve FAILED TO CLOSE (valve failure)
t ≥ FB 1 1 Valve FAILED TO CLOSE (limit switch failure)

For a sequence command, the function does the test as follows :


 If a valve discrepency is detected :
o the sequence is stopped (frozen)
o a message is displayed (example: "VALVE UV 004 FAILED TO
OPEN")
o the operator must acknowledge the message
o when the problem has been solved, the operator must acknowledge to
restart the sequence
o the sequence restarts and tests again the valve state
 If no valve discrepency is detected :
o the valve command is normally completed and the sequence continues
For an operator command, the function does the test as follows :
 If a valve discrepency is detected :
o a message is displayed (example: "VALVE UV 005 FAILED TO
CLOSE")
o the operator must acknowledge the message
o when the problem has been solved, the operator must reenter the
command
 If no valve discrepency is detected :
o the valve command is normally completed

1.2. Function : WAIT FOR CONDITION


This function is used when a wait order is executed by a sequence. The sequence
waits until a condition becomes true. When the condition becomes true, the
sequence executes the next order.
A waiting timer is started when the sequence executes the wait order. A maximum
waiting time (time-out) is predefined. If the waiting time exceeds the time-out, a
message is displayed and the sequence restarts waiting. The waiting timer is
restarted.
For example, in the catalyst transfer sequence described in paragraph 4.7.2, there is
the order :
"WAIT PI 3116 = PI 3136  0.005 MPa, 5 M".

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PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

The sequence waits until the pressure in the lock hopper (PI 3116) becomes nearly
equal to the pressure in the upper surge drum (PI 3136). If after 5 minutes, the
pressures are not equalized, a message is displayed and the sequence continues to
wait.

2. Catalyst Transfer Sequence Description (UC2)


2.1. Introduction
Periodically when the upper surge drum (D-71301) is full, the catalyst is transfered
by gravity to the lock hopper (D-71302) and then from the lock hopper to the
regenerator (R-71301) Refer to figure 1 given in appendix.
However the pressure in the upper surge drum (D-71301) is much lower than the
pressure in the regenerator (R-71301). Consequently, to allow this transfer, the
pressure between the drums must be equalized.
These transfer operations are done automatically. A sequence (noted TRANSFER
sequence) is programmed in the DCS. This sequence uses process information,
pressure, level and on/off signals such as LAL, LALL, limit switches. According to
the state of these parameters, the sequence will open or close on/off valves.
This sequence is divided in two main phases : LOAD and UNLOAD. The LOAD
operation is dedicated to the transfer from the upper surge drum to the lock hopper
and the UNLOAD operation to the transfer from the lock hopper to the regenerator.
Each phase lasts approximatively 20 minutes.
Interlocks (described in paragraph 2.7 "Software interlocks) are implemented in the
DCS to forbid direct communication between the upper surge drum and the
regenerator. These interlocks filter the valve requests done automatically by the
sequence or manually by the operator.
At any time, on the DCS console, the operator can stop the transfer. After a stop, the
operator can restart the sequence with a LOAD or an UNLOAD phase.

2.2. Transfer Sequence Description


All drums, valves and instruments involved in the transfer are shown in the figure 1
given in appendix.
The normal TRANSFER sequence executes permanently and in turn the LOAD
phase and the UNLOAD phase. These phases are detailed hereafter.

LOAD phase
1. Check that the conditions are good to start the LOAD :
The valves UV 3001, UV 3002, UV 3003, UV 3004, UV 3006, UV 3008, UV 3009,
and UV 3010 must be closed and there must be a low level (LAL 3109) in the
lock hopper
2. Open valve UV 3008 to depressurize the lock hopper
3. Wait until PI 3116 = PI 3136 +/- 0.005 MPa (adjustable value)
4. Close valve UV 3008
5. Open valve UV 3006 to equalize pressures between upper surge drum and
lock hopper.
6. Wait for enough catalyst in the upper surge drum : LI 3107 > 65 % (adjustable
value).

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PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0
7. Open valve UV 3002

8. Open the valve UV 3001: the catalyst will fill up into the lock hopper.
9. Wait for high level in the lock hopper (LAH 3108). The lock hopper is now full of
catalyst.
10. Close the catalyst valve UV 3001.
11. Wait 10 seconds (adjustable value). The tight gas valve UV 3002 must not be
actuated in presence of catalyst
12. Close the valves UV 3002 and UV 3006.

UNLOAD phase
1. Wait for the good conditions to start the UNLOAD :
The valves UV 3001, UV 3002, UV 3003, UV 3004, UV 3006, UV 3008, UV 3009
and UV 3010 must be closed
2. Open valve UV 3010 to increase the pressure in the lock hopper by nitrogen
injection.
3. Wait until PI 3116= PI 3106 +/- 0.005 MPa (adjustable value)
4. Close valve UV 3010
5. Open valve UV 3009 to equalize pressures between lock hopper and regenerator.
6. Wait for low level in the regenerator storage : LI 3103 < 30 % (adjustable value).
7. Open valve UV 3004
8. Open UV 3003 : the catalyst is unloaded from lock hopper into the top of the
regenerator.
9. Wait for low level in the lock hopper : LAL 3109. The batch of catalyst has been
transferred in the regenerator.
10. Close the valve UV 3003.
11. Wait 10 seconds (adjustable value). The tight gas valve UV 3004 must not be
actuated in presence of catalyst
12. Close the valves UV 3004 and UV 3009.
Note : The operator must be able to change the adjustable parameters without
stopping the sequence.

2.3. Calculations
After each UNLOAD phase, the following statistics must be calculated and displayed
on the DCS console.
 the number of catalyst transfers since the last statistics reset
 the quantity of catalyst transferred during the last transfer
 the quantity of catalyst transferred averaged over the the 10 last transfers
(adjustable value)

2.4. Abnormal Conditions Detected By The Sequence


When the sequence is running, an abnormal condition can happen during a valve
operation or a wait for conditions. Refer to paragraph 1 "Control functions". This
abnormal condition
can be due to:
 an incorrect valve mode
 a software interlocks
 a valve or limit switch failure
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PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

 an instrument (level, pressure, temperature) failure


 a process trouble (loss of nitrogen…)
The sequence is then frozen at its current order. The operator can either request the
sequence execution restart from the current order or request the stop as described
in next paragraph.

2.5. Stop Requested By Operator


At any time, the normal sequence can be interrupted on the DCS console. A STOP
button must be configured.
A stop sequence must be programmed in addition of the normal sequence. This stop
sequence checks permanently if the operator requests a stop.
When a stop request is detected, the normal sequence is disabled immediately and
all valves are closed.

OPERATOR REQUEST NO
=
STOP (HS 3115)

YES

DISABLE NORMAL SEQUENCE

Close UV 3001
Close UV 3002
Close UV 3003
Close UV 3004
Close UV 3006
Close UV 3008
Close UV 3009
Close UV 3010

AUTHORIZE RESTART IN
PHASE LOAD OR UNLOAD

- STOP sequence -

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

2.6. Start / Restart Requested By Operator


When the sequence is stopped, the operator can request on the DCS console :
 a normal start : the sequence executes the LOAD and UNLOAD phases in
turn as described in paragraph 2.2.
 a load restart : the sequence executes first a LOAD phase with no test on the
lock hopper level
 an unload restart : the sequence executes first an UNLOAD phase with no
test on the regenerator level

The START, LOAD RESTART and UNLOAD RESTART must be configured on the
DCS console.

1) Normal start

OPERATOR REQUEST NO
=
START

YES

NORMAL SEQUENCE :
PHASE LOAD

NORMAL SEQUENCE :
PHASE UNLOAD

2) Restart sequence (with LOAD)

OPERATOR REQUEST NO
=
RESTART IN LOAD PHASE

YES

Close UV 3001
Close UV 3002
Close UV 3003
Close UV 3004
Close UV 3006
Close UV 3008
Close UV 3009
Close UV 3010

EXECUTE PHASE LOAD


no test on lock hopper level
(LAL 3109)

NORMAL SEQUENCE : NORMAL SEQUENCE :


PHASE LOAD PHASE UNLOAD

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

3) Restart sequence (with UNLOAD)

OPERATOR REQUEST NO
=
RESTART IN UNLOAD PHASE

YES

Close UV 3001
Close UV 3002
Close UV 3003
Close UV 3004
Close UV 3006
Close UV 3008
Close UV 3009
Close UV 3010

EXECUTE PHASE UNLOAD


without test on regenerator level
(LI 3103)

NORMAL SEQUENCE : NORMAL SEQUENCE :


PHASE LOAD PHASE UNLOAD

2.7. Software Interlocks


Software interlocks are programmed for the valves : UV 3001, UV 3002, UV 3003,
UV 3004, UV 3006, UV 3008, UV 3009 and UV 3010.
There are four interlocks :
interlocks 1 and 2 : this interlock forbids direct communication between the upper
surge drum (D-71301) and the regenerator (R-71302).
interlock 3 : this interlock forbids nitrogen injection (valve UV 3010) in another
equipment than the lock hopper (D-71302).
interlock 4 : this interlock forbids depressurization to atmosphere (valve UV 3008)
of another equipment than the lock hopper (D-71302).

Interlock 1 :
When at least one of the valves UV 3003, UV 3004, UV 3008, UV 3009, or UV 3010
is open, the software interlock forbids to open the valve UV 3001 or the valve UV
3002 or the valve UV 3006.

Interlock 2 :
When at least one of the valve UV 3001, UV 3002, UV 3006, UV 3008 or UV 3010 is
open, the software interlock forbids to open the valve UV 3003 or the valve UV 3004
or the valve UV 3009.

Interlock 3 :
When at least one of the valves UV 3001, UV 3002, UV 3003, UV 3004, UV 3006,
UV 3008 or UV 3009 is open, the software interlock forbids to open the valve UV
3010.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

Interlock 4 :
When at least one of the valves UV 3001, UV 3002, UV 3003, UV 3004, UV 3006,
UV 3009 or UV 3010 is open, the software interlock forbids to open the valve UV
3008.

Interlock bypass :
A bypass for each interlock to allow valve operation during start-up or test periods
should be configured. These bypasses must be under restricted access.
If an interlock is bypassed, the commands on the corresponding valves are no more
filtered. In this case, when these valves are commanded, a message must be
displayed (Example: "INTERLOCK ON VALVE UV 002 BYPASSED ").

3. Catalyst Circulation Control


 The different equipment and instruments involved in the catalyst circulation control
are displayed in the figures 2, 3, 4, 5 and 6 given in appendix.
 The purpose of the catalyst circulation control is to minimize catalyst attrition and to
maintain a continuous catalyst circulation.
 The primary stream (which governs the lift gas flow-rate) is controlled by a flow-
rate controller (FIC). A calculation block is programmed to adjust the operator
setpoint in order to maintain a correct catalyst velocity. This calculation block is
described in paragraph 3.1 "Lift gas flow-rate adjustment (for all the lifts)".
 The secondary stream (which governs the catalyst flow-rate) is controlled by a
pressure difference controller (PDIC). The quantity of catalyst circulating in the unit
is adjusted through the PDIC of the lift 1 (lift master). A calculation block is
programmed to correct the operator setpoint. This calculation block is described in
paragraph 3.2. "Catalyst flow-rate adjustment (lift 1 only)".
 The lifts are started manually as explained in the Operating Instructions manual.
Once the steady-state conditions are reached, the control of the lifts 2, 3, 4 is
made through a controller cascade. For these lifts, the PDIC on the secondary
stream is cascaded by the level controller (LIC) on the upper hopper above.
 The principle of this cascade control is :
 For each lift (except lift 1) when the catalyst level in the corresponding upper
hopper exceeds the requested level (usually 60 %), the LIC increases the PDIC
setpoint. Consequently, the PDIC valve opens and the catalyst flow-rate is
increasing.
 Reciprocally, when the level in the upper hopper is lower than the requested
setpoint, the LIC decreases the PDIC setpoint. Consequently, the PDIC valve
closes and the catalyst flow-rate is decreasing.
 The lifts can be stopped automatically on detection of abnormal events. Refer to
paragraph 3.3 "Automatic lift stop".

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

3.1. Lift Gas Flow-Rate Adjustment (For All The Lifts)


 The lift gas flow-rate is controlled by a flow-rate controller (FIC) whose
setpoint is calculated by a calculation block. There is a calculation block for
each lift.
 These calculation blocks are used to adjust the lift gas flow-rate in case of
change in the operating conditions in order to maintain a correct catalyst
velocity. This velocity is a parameter entered by the operator.
 Whatever the operating conditions, the catalyst velocity must not be too high
to prevent excessive attrition of the catalyst. A typical value is 3.0 m/s.
 The temperature, the pressure in the lift pot and the lift gas density have an
effect on the lift gas velocity. For example, if the temperature in the lift pot
increases, the velocity will increase.
 These parameters are linked to the operating conditions : for example, any
change of the reforming feed quality can lead to a change of the H 2 rich gas
density (this gas is produced in the reaction section and used as lift gas).
 The calculations implemented are described in next paragraph

Equations implemented in the calculation blocks

Catalyst optimal velocity : Spd (m/s) (entered by operator)

Operating parameters
lift gas molecular weight : MW (g/mol) entered by operator
lift pot absolute pressure : P (kg/cm²) measured by DCS
lift pot temperature : T (°C) measured by DCS

Calculation of the flowrate setpoint (FLOWRATEC) :


The lift gas density  (kg/m3) is calculated :
MW P 273
  
22.4 1 T  273
The lift gas velocity in the pipe SPEED (m/s) is calculated :
 moy
SPEED  SPD  5.7 

moy is the average catalyst ball diameter ( = 1.8 mm)
The lift gas mass flowrate FLOWRATE (kg/h) is calculated :
FLOWRATE  SPEED Section    3600
Section is the catalyst pipe internal section (m²)
Depending on the DCS, a corrective parameter K (no unity) is calculated :
K  1 (if the FIC performs orifice correction)
P (T 273) MWd
K ( d  )
P (T 273 ) MW
d (if no correction provided by DCS)
Pd (kg/cm²) is the absolute pressure for which the flowmeter is calibrated
Td (°C) is the temperature for which the flowmeter is calibrated

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

MW d (g/mol) is the gas molecular weight for which the flowmeter is calibrated
The lift gas corrected mass flowrate FLOWRATEC (kg/h) is calculated :
FLOWRATE c  FLOWRATE  K

3.2. Catalyst Flow-Rate Adjustment (Lift 1 Only)


The first lift is not controlled by a LIC/PDIC cascade but only by the PDIC : the
setpoint of the controller determines the total catalyst flow-rate in the unit.
The setpoint is entered by the operator. A choice of correction is allowed. In case of
correction choice, the setpoint fixed by the operator is corrected as follow:

Setpoint calculated  Setpoint operator  T - Tref   C1  1  C2   DTMAX  C1  C2  C3


with :
Tref lift pot temperature in steady state conditions (typical value : 200°C)
entered by engineer
DTMAX range of temperature
T lift pot temperature
C1 corrective coefficient (typical value 0.0005) entered by engineer
C2 corrective coefficient :
= 1 if T - Tref > DTMAX
= 0 if T - Tref  DTMAX
C3 corrective coefficient (typical value 1) entered by engineer

C2=1 Setpointcalculated = Setpointopérator - [DTMAX*C1*C3]

C2=0 Setpointcalculated = Setpointopérator - [ (T-Tref)*C1]


DTMAX
>0
T ref
C2=0 Setpointcalculated = Setpointopérator - [ (T-Tref)*C1]

<0

- Pressure drop control -

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

3.3. Automatic Lift Stop


On detection of an abnormal condition, a lift can be stopped automatically by a
shutdown logic. The shutdown logic forces the PDIC valve on the corresponding lift
to close by action on its solenoid.
A shutdown logic is dedicated for each lift and a shutdown logic (noted catalyst
circulation stop) is dedicated for all the lifts together.
When a lift is automatically stopped, the LIC/PDIC cascade must be cancelled and
the PDIC forced in MANUAL mode with 0% output value.
When all the stop conditions have disappeared, the PDIC valve can be actuated
again.

4. Hydrogen System Pressure Control (UC 3)


A logic must be configured in the DCS to shutdown smoothly the hydrogen circulation
(lifts 2 and 3) in case of trouble in the hydrogen network.
On detection of a very low pressure in hydrogen network (typically lower than 90% normal
pressure), the following actions must be done :
 FIC 3017 is set in AUTO mode with setpoint equal to turndown flowrate of the
hydrogen purification unit.
 Control valve HV 3003 on reduction effluent is closed by action on its solenoid
 HIC 3003 is set in MANUAL mode at 0% output
 a signal is transmitted to ESD to trigger the second lift shutdown logic
 a signal is transmitted to the ESD to trigger the third lift shutdown logic

After a delay (usually 20 seconds), the following actions are done :


 Control valve FV 3012 (second lift primary stream) is closed by action on its
solenoid
 FIC 3012 set in MANUAL mode at 0% output value
 Control valve FV 3013 (third lift primary stream) is closed by action on its solenoid
 FIC 3013 set in MANUAL mode at 0% output value

On detection of the shutdown of the hydrogen purification unit (M-71301), the following
actions must be done :
 FIC 3017 is set in MANUAL mode with 0% output value.
 Control valve HV 3003 on reduction effluent is closed by action on its solenoid
 HIC 3003 is set in MANUAL mode at 0% output
 a signal is transmitted to ESD to trigger the second lift shutdown logic
 a signal is transmitted to the ESD to trigger the third lift shutdown logic

After a delay (usually 20 seconds), the following actions are done :


 Control valve FV 3012 (second lift primary stream) is closed by action on its
solenoid
 FIC 3012 is set in MANUAL mode at 0% output value
 Control valve FV 3013 (third lift primary stream) is closed by action on its solenoid
 FIC 3013 is set in MANUAL mode at 0% output value

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

5. Special Loops Description

5.1. Oxygen Content Control


The oxygen injected in the regenerator must be maintained at correct values. This
oxygen content control takes automatically into account any variations in the
process. This control is described hereafter and also displayed in figure 7 given in
appendix.
Depending on the operation mode (normal mode or blackburning mode), the control
is different.

Oxygen content control in normal mode


Oxygen injected in oxychlorination and calcination zone (and consequently with the
recirculation of the effluents, in the first burning bed) passes through FV 3007. In
normal mode, setpoint of FIC 3007 is modified by AIC 3004 through HS 3124 so that
oxychlorination/calcination gas contains 4 to 6 % vol. of oxygen. The oxygen content
of 0.8% vol. in the burning gas going to the first bed is reached through AIC 3001.
This controller modifies AIC 3004 setpoint.

Oxygen content control in blackburning mode


When blackburning mode is actuated (either manually by an operator or
automatically through IS 3030), the selector HS 3124 redirects the information
coming from AIC 3001 directly to FIC 3007, since AIC 3004 is not operating any
more.

Note : There is also an oxygen content control at the second burning bed inlet : the
setpoint of FIC 3002 is modified by AIC 3002 so that the second burning bed inlet
contains 0.8 % vol. oxygen. This control does not depends on the operation mode.

5.2. Regeneration Loop Compressor Spill-Back Control


During normal operation, the valve FV 3004 on the compressor spill-back is used to
adjust the flow-rate in the regeneration loop. This valve is controlled by FIC 3004.
If the pressure at the regeneration loop compressor outlet becomes too high (around
0.780 MPa), the PIC 3117 overrides FIC 3004 and controls directly the valve FV
3004. The control valve will open until the pressure recovers a normal value.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

5.3. Nitrogen Loop Pressure Control (UC 4)


To enable the catalyst lift, pressure in the nitrogen system must follow reaction
section pressure fluctuations. Thus, the pressure in the nitrogen compressor KO
drum must be slightly lower (by around 0.005 MPa) than the pressure at the last
reactor outlet.
For this purpose, a pressure difference between the nitrogen compressor KO drum
and the pressure at the last reactor outlet is controlled by PDIC 3017 which is acting
in split range on the valves PDV 3015A (nitrogen injection) and the valve PDV
3015B (gas purge).
The PDIC 3017 control is acting as follows :
In steady state conditions, the pressure difference between the nitrogen loop and the
reaction section is equal to the setpoint (about 0.005 MPa). The controller PDIC
3017 is at 50 % output value and the control valves are both closed.
If the delta pressure exceeds the setpoint (due to an increase of the nitrogen loop
pressure for example), the gas purge valve will open. In the opposite case, the
nitrogen injection valve will open.
To avoid continuous pressure fluctuations, a dead band in the split range is
valve
opening (%)
PDV 3015A PDV 3015B
(N2 injection) (gas purge)
100%

0%
0% 50% 100%
dead PDIC 3017
band output (%)
foreseen. This dead band is usually 10% (no action between 45% and 55% output).

Start-up mode / normal mode :


During start-up or other transient operations, the regenerator loop pressure control is
performed by a simple pressure control (PIC 3016).
The operator can switch with HS 3121 from the control in normal mode (PDIC 3017)
to the control in start-up mode (PIC 3016) and reciprocally.
The switch between the two controllers must be done without jump. The output of
the controller currently used must be copied permanently (tracking) by the other
controller.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

5.4. Regeneration Loop Pressure Control (UC 1)


To enable the catalyst flow in the first lift, the pressure in the calcination inlet (PT
3001) must be higher (by around 0.060 MPa) to the pressure at the first reactor inlet
(PT 3123) :
For this purpose, the pressure difference between the calcination inlet and the first
reactor is controlled by PDIC 3002 which is acting in split range on the valves PDV
3002A (gas purge) and the valve PDV 3002B (nitrogen injection).
The PDIC 3002 is acting as follows :
In steady state conditions, the pressure difference between the regeneration loop
and the reaction section is equal to the setpoint (about 0.060 MPa). The controller
PDIC 3002 is at 50 % output value and the control valves are both closed.
If the delta pressure exceeds the setpoint (due to an increase of the regeneration
loop pressure for example), the gas purge valve will open. In the opposite case, the
nitrogen injection valve will open.
To avoid continuous pressure fluctuations, a dead band in the split range is
foreseen. This dead band is usually 10% (no action between 45% and 55% output).
valve
opening (%)
PDV 3002B PDV 3002A
(N2 injection) (gas purge)
100%

0%
0% 50% 100%
dead PDIC 3002
band output (%)

Start-up mode / normal mode :


During start-up or other transient operations, the regenerator loop pressure control is
performed by a simple pressure control (PIC 3002).
The operator can switch with HS 3002 from the control in normal mode (PDIC 3002)
to the control in start-up mode (PIC 3001) and reciprocally.
The switch between the two controllers must be done without jump. The output of
the controller currently used must be permanently copied (tracking) by the other
controller.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

5.5. Pressure Difference Control Between Burning Zone And Oxychlorination Zone
To prevent oxychlorination gas with high content in oxygen from flowing upward in
the burning section, a pressure difference (typically 0.002 MPa) must be maintained
between the burning zone and the oxychlorination zone. However this pressure
difference must not be too high to avoid damaging the baffle between the two zones
in the regenerator.
For this purpose, the pressure difference between the burning zone and the
oxychlorination zone is controlled by PDIC 3003 which is acting in split range on the
valves PDV 3003A (burning section outlet) and the valve PDV 3003B
(oxychlorination outlet).
The PDIC 3003 is acting as follows :
In steady state conditions, the pressure difference between the burning zone and the
oxychlorination zone is equal to the setpoint (about 0.002 MPa). The controller PDIC
3003 is at 50 % output value and the control valves are both closed.
If the pressure difference exceeds the setpoint, the oxychlorination outlet valve will
close to increase the pressure in the oxychlorination zone. The pressure difference
will decrease.
In the opposite case, the burning outlet valve will close to increase the pressure in
the burning zone. The pressure difference will increase.
To avoid continuous pressure fluctuations, a dead band in the split range is
foreseen. This dead band is usually 10% (no action between 45% and 55% output).

valve
opening (%)
PDV 3003A PDV 3003B
(burning outlet) (oxychlor. outlet)
100%

0%
0% 50% 100%
dead PDIC 3003
band output (%)

6. Temperature Control Optimization


All parameters used in the control must be adjustable easily during operation.

6.1. Regenerator first burning bed inlet


The temperature of the first bed inlet is controlled by TIC 3001 which is acting on the
burning heater (R -71301).
The temperature of the first outlet is checked by TI 3116.
The temperature in the first bed inlet is normally set to 470°C but if the temperature
of the first bed outlet (TI 3116) is too low, the setpoint of TIC 3001 will increase from
470°C to 490°C in order to provide a good burning in the first bed. This optimization
is done when the controller is in AUTO mode.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

TI 3116 > 495°C + dead band/2 (TIC 3001) setpoint will ramp from 490 to 470°C
TI 3116 < 495°C - dead band/2 (TIC 3001) setpoint will ramp from 470 to 490°C

The dead band (10°C for example) around 495°C is used to avoid permanent
change of the setpoint.

6.2. Regenerator second burning bed inlet


The purpose of this control is to avoid a too high temperature in the second burning
bed.
The temperature at the second bed inlet is controlled by TIC 3003 which is acting on
the quench gas flow (valve TV 3003).
The temperature in the second burning bed outlet is measured by TI 3118.
The setpoint of TIC 3003 is normally set to 480°C. However if the temperature out of
the bed is too high (TI 3118), the setpoint is decreased 480°C to 460°C. This
optimization is done when the controller is in AUTO mode.

TI 3118 < 523°C - dead band/2 (TIC 3003) setpoint will ramp from 460 to 480°C
TI 3118 > 523°C + dead band/2 (TIC 3003) setpoint will ramp from 480 to 460°C

The dead band (10°C for example) around 550°C is used to avoid permanent
change of the setpoint.

6.3. Reduction chamber inlet


The purpose is to avoid too high temperature in the reduction chamber.
The temperature of the hydrogen gas inlet is controlled by TIC 3007 which is acting
on the reduction heater (H-71304). The setpoint is normally fixed by the operator but
a possibility of setpoint correction is provided : the setpoint is reduced by 20°C
(adjustable value) if the temperature (TI 3143) in the reduction chamber exceeds
480°C (adjustable value).
When the correction option is enabled, the setpoint is modified as follows :
TI 3143 > 480°C + dead band/2 (TIC 3007) setpoint will ramp from (operator
setpoint) to (operator setpoint - 20 °C)
TI 3143 < 480°C - dead band/2  (TIC 3007) setpoint will ramp from (operator
setpoint -20°C) to (operator setpoint)
The dead band (10°C for example) around 480°C is used to avoid permanent
change of the setpoint.
Note : The output of TIC 3007 must be bounded between two limits which will be
tuned during start-up.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

7. Appendix

Figure 1
CATALYST TRANSFER

TO FINES
FILTER

PI 3136

EQUILIBRIUM LINE

LI 3107

2. UPPER
UV 3006
SURGE
4. D-
DRUM LIFT 4
71301

UV 3001

ATM
UV 3008 UV 3002
3002
PI 3116

LAH 3108
EQUILIBRIUM LINE
N2
UV 3010 LAL 3109

3. LOCK
5. D-
HOPP
UV 3003
UV 3009
71302
ER

UV 3004

EQUILIBRIUM LINE
PI 3106

LI 3103

1.1 Regenerat
or

6. R-

71301

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KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

TO FINE
FILTERS

FROM
LOCK HOPPER
Figure 2 LSHH 3110
LIFT 1 CONTROL 1st upper
hopper
D-71310

LSLL 3103
Regenerator
R-71301

LIFT 1
Reductor
D-71311

N2
HEADER
D-71304
R-71201

Catalyst
First flow-rate UV 3005 PDSLL 3114
lift stop
adjustmen
PDIC 3006 t LIFT 1 STOP
Causes :
D-71305  LSLL 3103
TI  LSHH 3110
Lift 1 gas  ZSC 3005
FIC 3010 flow-rate 3153  REGENERATOR SEAL (IS 3016)
N2 PI 3153 (PDSLL 3114 or HS 3114)
LIFT adjustmen  CATALYST CIRCULATION STOP (IS 3015)
t (regenerator shutdown or HS 3116)

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KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0
TO FINE Figure 3 H2 LIFT
FILTERS RETURN
LIFT 2 CONTROL
D-71312
FSLL 3114
LIC 3111
N2
D-71310
HEADER
LSLL 3112

Second
reactor
R-71202
UV 3011 PDSLL 3122

Reductor
LSLL 3113 D-71311
LIFT 2

First
reactor R-
71201

LIFT 2 STOP
Second Causes :
D-71321  LSLL 3112
lift stop
 LSLL 3113
 ZSC 3011
PDIC 3008  FIRST REACTOR SEAL (IS 3019)
(PDSLL 3122 or FSLL 3114 or AAHH 3104B or
AAHH 3105B or HS 3118)
D-71331
 REDUCTION HEATER SHUTDOWN (IS 3017)
H2 pressure TI 3147 Lift 2 gas  H2 PRESSURE CONTROL (UC 3)
FIC 3012
control flow-rate  CATALYST CIRCULATION STOP (IS 3015)
(regenerator shutdown or HS 3116)
PI 3124 adjustment
H2 LIFT

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KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

H2 H2
NETWORK NETWORK

LIC 3117
D-71312 D-71313
LSLL 3119

Third
Second
reactor
reactor
R-71203
R-71202
LIFT 2 LIFT 3

Figure 4
LIFT 3 CONTROL

D-71322

Third
lift stop

PDIC 3009
D-71332
TI 3149 Lift 3 gas
LIFT 3 STOP
flow-rate Causes :
H2 pressure adjustment  LSLL 3119
control FIC 3013 PI 3129  H2 PRESSURE CONTROL
 CATALYST CIRCULATION STOP (IS 3015)
(regenerator shutdown or HS 3116)
H2 LIFT

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KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0
TO TO
Figure 5 FINE FILTERS FINE FILTERS
LIFT 4 CONTROL

LSHH 3106
LIC 3120
LSLL 3122

9. D-
8. D-
713
713
LIFT 4 LIFT 3 13
01

7. T
PDSLL 3137
H
IR
D N2
HEADER
R UV 3014
E FSLL 3117
D-71323
A
C
T
UV
O 3013
LIFT 4 STOP Fourth lift PDIC 3011
Causes : stop R
 LSLL 3122
 LSHH 3106
R-
D-71333 TI 3153 Lift 4 gas
 ZSC 3013 71 flow-rate
 THIRD REACTOR SEAL (IS 3022) FIC 3015 20 adjustment
(PDSLL 3137 or FSLL 3117 or ASHH 3104B PI 3153
or ASHH 3105B or HS 3114) 3
 CATALYST CIRCULATION STOP (IS 3015) N2 LIFT
(regenerator shutdown or HS 3116)

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KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

Figure 6
LIFT GAS RETURN LIFT GAS RETURN

LAHH 3106 LAHH 3110


LI 3107 FIC 3011
LIC 3111
LALL 3112
ATM
15.2 D 16.1.5 N
UV 3012 9.3 D
LIFT GAS RETURN
- 2 -
LIFT GAS RETURN
7 UV7 3011

1 1
LAH 3108 AH AH
3 3 LIC 3117 LIC 3120
LAL
LAL 031
3109 LALL 3113
0 1 LALL 3119 LALL 3122
9.2 D
1 LIFT 4 0
-
13. D 12. D- 11. D-
7
- 71 713
LI 3103 1
7 13
LSLL 3104 3
31
1 2
1
3
1
0

16. R-2
10. R- 15. R 14. R- FIC 3016
PDIC 3007 713
712 - 712
01
01 7 03 UV 3014 15.1.1
16.1.2UVN3007
2 D-71304
LIFT 1
D-71322
LIFT
D-71321
1 16.1.1 L 2 3 D-71323

I 0

UV 3005 F 2 UV 3013
T
PDIC 3006 D-71305 PDIC 3008 D-71331 D-71332 D-71333
PDIC 3009 PDIC 3011
2
FIC 3012 FIC 3013 FIC 3015

FIC 3010

16.1.3 N
16.1.4 H
ISSUE DATE: 20/03/06 - 82 -
2
2
L
L
KRC CATALYST REGENERTION SECTION
PRODUCTION & OPERATION PROCESS AUTOMATION
CCR UNIT KRCIM 71300.06 REV.0

Figure 7
OXYGEN CONTENT CONTROL

REGENERATOR
FIRST BED INLET

AIC 3001

QUENCH GAS

SECOND BED INLET


BURNING ZONE

FIC 3002 AIC 3002


WASHING
DRUM
AIR
LOOP
COMPRESSOR Blackburning SECOND BED OUTLET
mode
UV 3017

HS 3124
SELECTOR
FIC 3007
Normal
AIR mode OXYCHLORINATION OUTLET
UV 3016

AIC 3004 OXYCHLOR. /


OXYCHLORINATION INLET CALCINATION
ZONE

CALCINATION INLET

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION SPECIAL EQUIPMENT
CCR UNIT KRCIM 71300.07 REV.0

Contents: This instruction outlines the special equipment technology used in catalyst
regeneration section. The text includes:

1. Membrane Hydrogen Purification Unit (M-71301)


2. Regeneration Loop Dryer DR-71301

1. Membrane Hydrogen Purification Unit (M-71301)

1.1. Objective
To boost the reduction hydrogen purity

1.2. Technology
Membrane separation technology realizes gas separation by taking advantage of
gas molecules passing through membrane at different speeds. Gases permeating
faster concentrate richly on permeation side while gases permeating slower on feed
side. Membrane separation is mainly characterized by low energy consumption,
simple equipment, easy operation, few moving parts, and high operating reliability.

1.3. Process Flow And Main Equipment


The equipment is divided into two parts, i.e. pretreatment and membrane separation,
in which membrane separation is the main part thereof. Membrane separator is the
central device for the main part, with the core of which is composed of tens of
thousand of hollow fibers. Any rash operation in an irresponsible manner will bring
loss to separator that is not remedial. For this reason, operators are required not
only to be technically qualified but also to have a serious and conscientious attitude
toward work, strictly observing related requirements of operating procedures and
mastering skillfully the technological process and features of the equipment, as
necessary premises to ensure normal operation of membrane separator.

1.3.1. Process flow


 An introduction to the technological process is given below (please see
diagram SDQHS-04.05 for the flow for hollow fiber separation equipment
with control points).
 Feed gas is composed of H2, CI, C2, C3, C4 and C5 with a pressure
(absolute pressure) being 2.08MPa. It is desired to separate hydrogen
from it with a membrane separator.
 Feed gas enters into water cooler (E-71341) first (through membrane
regulating valve HV3452), in which the temperature reduces to 35 °C
before entering into cyclone separator (D-71342) where solid and liquid
particles with diameter> 10 µm are removed with the separated liquid

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CCR UNIT KRCIM 71300.07 REV.0

to be discharged from the bottom thereof. D-71342 effluent gas enters


into three-stage efficient filter (D-71343) after being discharged from the
top of cyclone separator. Further separation will be achieved to residual
oil in liquid state with particles diameters greater than 0.01 µm to be
removed by filtering. The final liquid oil content should be less than
0.01mg/m3.
 To avoid oil condensation resulting from cooling and temperature drop in
pipelines and membrane separator which might result in membrane
separator performance reduction, filtered gas must be treated with
heating. Feed gas is heated in heater (E- 71344A) to 45 ̊C.
 Feed gas after passing water cooler, cyclone separator, three-stage
efficient filter, and heater is sent to membrane separation equipment for
separation. The separation equipment is composed of six Ф150X
1200mm hollow fiber membrane separators, which are divided into two
groups with three separators each, being in parallel connection. Each
separator can be disconnected or connected with a valve. Membranes
can be put into service according to different volumes of treatment to
change hydrogen purity and recovery rate.
 After feed gas enters into membrane separator, hollow fiber membrane
is highly selective to hydrogen and as a result, the speed of hydrogen
penetrating membrane is far quicker than other gases. Separation is
realized depending on the pressure difference between internal and
external sides of hollow fiber membrane as the driving force and going
through such steps as permeation, dissolving, spreading, and resolving,
so that hydrogen rich gas flow is formed in hollow fiber membrane with
inert gas flow to be formed on the external side. The former is called
permeating gas and the latter tail gas.
 After feed gas is separated under six membrane separators, over 85%
hydrogen is separated with the hydrogen left in the tail gas being very
few and to be discharged via tail gas membrane regulating valve
FV3442

1.4. Main equipment


Hollow fiber membrane separator is mainly composed of the following parts.

1.4.1. Water cooler (E-71341)


Water cooler tube pass PN4.0, Ф 400X3700, shell pass, one set. Cooling
medium: water, which is in float head structure.

1.4.2. Cyclone separator (D-71342)


Cyclone separator: PN4.0, Ф 500X2200, one set, which works in the principle of
centrifugal and gravity separation and has a function to remove large solid
particles initially and large liquid drops (water drops, oil drops). The equipment
requires operators to discharge liquid automatically or manually on a regular
basis via liquid level regulating valve HV345 according to liquid content in feed
gas and liquid level indication on cyclone separator.

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CCR UNIT KRCIM 71300.07 REV.0

1.4.3. Efficient filter (D-71343)


Efficient filters: PN4.0, Ф 219X1000, six sets. The first stage is pre-filter, the
second is precision filter, and the third is super precision filter with filter cores
being indifferently silicon-boron fiberglass. The equipment has two groups with
3 sets each, with one in service and the other in standby. It has a function to
remove effectively tiny solid particles and oil mist, water fog as well as aerosol
and aggregation included in gas. The accuracy of the filter for mechanical
particles reaches 0.01 micron with residual oil content less than 0.01mg/m3.
The equipment is provided with valves in the bottom for discharging liquid
manually every hour. To prevent filter from being punctured by fluids, the
maximum fluid linear velocity is required to be less than 3m/s for the
equipment. The filter core has a lifespan of 8,000 hours or can be replaced
above certain pressure difference according to differential pressure gauge
indication.

1.4.4. Feed gas heater (E-71344A)


As a set of tube type heat exchanger, the function is to increase gas
temperature. Feed gas is heated to 45 ̊C. Keep the feed gas passing through
membrane away from the dew point to avoid part of oil getting condensed on
membrane surface leading to membrane being unable to achieve its
performance sufficiently or even to damage membrane. Temperature
adjustment is made through membrane regulating valve TV3413A.

1.4.5. Hollow fiber membrane separator (M-71345)


Hollow fiber membrane separator group: consisting of six Ф 150X1200
membrane separators in the identical structure being divided into two groups.
The membrane separator is the main part or core of the equipment. The
equipment has three ports, i.e. feed gas inlet, tail gas outlet and permeating
gas outlet. The highest operating temperature for membrane core is 60 ̊C with
the pressure 3.5MPa, the pressure difference 2.5MPa and no pressure buildup
in opposite direction to be allowed (pressure on the permeation side greater
than that on feed gas side). Membrane separator core is composed of tens of
thousands of hollow fiber tubes. Feed gas enters from the feed gas inlet of
membrane separator and flows along fiber bundle surfaces, which experience
the process of permeating, dissolving, spreading, and resolving when
contacting with hollow fiber membrane. As different gas molecules penetrate
hollow fiber membrane at different speed, the purpose of separation is
achieved. For example, hydrogen penetrates membrane at a speed tens of
times that of such hydrocarbon molecules as C1, C2, etc. Hydrogen gas enters
into each hollow fiber tubes and discharges from the permeating gas outlet
after concentrating. Tail gas without permeation is discharged from the tail gas
outlet of membrane separator.

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CCR UNIT KRCIM 71300.07 REV.0

1.4.6. Permeating gas heater (E-71344B)


It is a set of tube type heat exchanger with a function to increase gas
temperature. Permeating gas is heated to 90°C. The temperature adjustment is
made through membrane regulating valve TV3414A to achieve control of steam
supply.

1.5. Operating Instructions

The operations of hollow fiber membrane separator can be generalized into three
aspects, i.e. startup procedure, shutdown procedure, and normal operational
requirements.
The startup procedure consists of feed gas purifying, feed gas heating and pre-
emptying, and changeover from pre-emptying to membrane separator. Pre-emptying
during startup is mainly to inspect the oil content in feed gas and temperature
conforming to related requirements after being treated with purification and heating.
It is required that the oil content in feed gas after purifying should be less than
0.01mg/m3 with the temperature of feed gas reaching 45 °C after being heated.
Qualified feed gas must be then changed over slowly from emptying to membrane
separator under the condition of continuous purifying and heating. The whole
equipment will go into normal operation after feed gas being emptied is changed
over to membrane separator. In the circumstances that no fault occurs to auto
control instruments, the operation is simple with the process and operation
parameters able to be adjusted from time to time on different points.
No matter what shutdown it will be, i.e. normal shutdown, emergency shutdown or
fault shutdown, a shutdown instruction has to be input through the safety interlock
control system to realize shutdown after such instruction is received. Meanwhile, the
equipment will go into enclosed protection state automatically. Except HV3451 that
is kept open, all regulating valves in other positions will be closed. After shutdown,
the feed gas in the equipment will be in static pressure state, however, at this point
the pressure of feed gas is still higher than that of permeating gas, so the
permeation process is still going on, which is demonstrated by the pressure of feed
gas in separator decreasing gradually and the pressure of permeating gas
increasing gradually.
The safety interlock system of the equipment can have an auto shutdown control
over super high and low limits of cyclone separator liquid level, feed gas over-
temperature, etc.
Operational requirements will be described below for each process in the equipment:

1.5.1. Startup procedure


1.5.1.1. Preparations before startup

1.5.1.1.1. Inform related posts to be prepared for startup.


1.5.1.1.2. The stop valves are fully closed in the process pipelines to which
pressure transmitter and differential pressure transmitter are
connected, blow-off valves are fully closed, and stop valves for
pressure gauges are fully opened.

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PRODUCTION & OPERATION SPECIAL EQUIPMENT
CCR UNIT KRCIM 71300.07 REV.0

1.5.1.1.3. Be prepared for analytical sampling.


1.5.1.1.4. Check extensively the open and close state of process valves during
equipment startup.
Valves to be fully opened:
FZ02,FZ04,FZ06,FZ17 ,FZ18,FQ0l ,FQ02,FQ03,FQ04,FQ06.
Valves to be fully closed:
Other valves accept that to be fully opened.
State of auto regulating valves before startup
HV3451 will open and other auto regulating valves will all be in close
state.

1.5.1.2. Feed gas purification treatment

1.5.1.2.1. Cyclone separator purification: As shown in Diagram SDQHS-


04.05, open valve FZ0l, the feed gas coming into the system at
2.08MPa via membrane regulating valve HV3452 will first pressurize
cyclone separator. The pressurization speed should not be too fast,
which will be put under control at 0.3-0.5MPa per minute. When
pressurizing is up to 2.08MPa, regulating valve HV3452 will fully
open with A71341 to feed gas sampler.
1.5.1.2.2. Pneumatic ball valve HV3451 is a bypass valve, which is closed
during normal startup and opened during shutdown.
1.5.1.2.3. The liquid level in cyclone separator and discharge are manually
controlled with membrane regulating valve HV3453 for timed
discharges. Valve FZ15 will be fully opened during startup.
1.5.1.2.4. The indicated liquid level value is low or nil immediately after startup.
The liquid level is required to be lower than 30% during operation.
1.5.1.2.5. Instrument functions and parameters:
 HV3452 – Regulates feed gas intake, which are fully opened
during startup and encloses the equipment for protection after
shutdown.
 HV3453 – On/Off liquid discharge from cyclone separator for
level adjustment.
 LIA3421 - Indicate liquid level. High liquid level alarm value for
is 30%, the interlock value is 50%.
 LG3422 - Field liquid level indication. Should be less than 30%
 PG3481 - Field feed gas pressure indication. (2.08MPa)
 PG3482-Field cyclone separator pressure indication
(2.08MPa)
1.5.1.2.6. High efficient filter purification. The feed gas discharged from top
of cyclone separator enters into high efficient filter (D-71342) through
valve FZ02-1. Separated liquid oil is timed for manual discharge
through valve FZ19, which is initially fixed at one discharge per hour.
After startup, the discharge interval will be adjusted according to
actual liquid content.

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CCR UNIT KRCIM 71300.07 REV.0

1.5.1.2.7. Instrument functions and parameters:


 PdIA3431- Forward and back pressure difference 0-0.15MPa
as indicated with alarm value 0.18MPa.
 PdG3431- Forward and back pressure difference as indicated
on field, and when the pressure difference reaches the scale
as indicated, change over to another filter group or replace
filter cores.

1.5.1.3. Feed gas heating and pre-emptying

1.5.1.3.1. Feed gas heating.The feed gas exiting from cyclone separator and
high efficient filter will be heated to 45̊C by heater (E-71344A) and
then is sent into membrane separator for separation. In addition to
mentioned reason for heating, increasing temperature is also an
important factor to improve the permeable performance of a
membrane separator. Permeability of a membrane increases as
temperature rises, resulting in a higher hydrogen recovery rate.
However, too high temperature will have an unfavorable influence on
the strength and lifespan of a membrane. The temperature is under
control of membrane regulating valve TV-3413A.
1.5.1.3.2. Instrument functions and parameters:
 TIC3413A- Heating temperature indication control, 45 ̊C;
 TIA3415A- Heating temperature indication, alarm and
interlock. Upper heating temperature value for alarm 55 ̊C,
interlock value 60 ̊C.
 TG3463- Temperature as indicated on field after heating, 45
̊C.
1.5.1.3.3. Pre-emptying. The feed gas being purified, heated should not come
into membrane separators immediately, which must experience pre-
emptying treatment through valve HV-3455. The purpose of pre-
emptying is to inspect that feed gas purification and heating
temperature conform to requirements of indicators. A71343 is a
sample-analyzing valve. Valve FZ06 will be opened during startup.

1.5.1.4. Membrane separation system


The operating process of a membrane separation system includes feed
gas input, discharge of permeating gas and tail gas.

1.5.1.4.1. Feed gas input. The feed gas being purified and heated to related
requirements is gradually changed over from pre-emptying to
membrane separators. Feed gas changeover is an important part of
operations that should be grasped skillfully.
1.5.1.4.2. Before changeover, keep the two groups of membrane inlet master
valves FZ05 and bypass valve FL04 in close state, close pneumatic

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PRODUCTION & OPERATION SPECIAL EQUIPMENT
CCR UNIT KRCIM 71300.07 REV.0

ball valve HV3457 in the main permeating gas line, close the tail gas
regulating valve FV3442 and FZ07, FZ08, open permeating gas and
tail gas emptying valves FZ09, FZ13, with the regulating valve
HV3456 for permeating gas emptying being 30% opened, the inlet
valves for membrane separators, open the outlet valves for tail gas,
permeating gas.
1.5.1.4.3. Check that the states of the mentioned valves are correct. Open
slowly inlet sub-line valve FL04 to feed air to membrane separators,
at this point permeating gas and tail gas are emptied.
1.5.1.4.4. In 3-5 minutes, close emptying valves FZ13, FZ09, HV3456. When
the pressure in membrane separator rises to 2.08MPa, first open
pneumatic ball valve HV3457, fully open regulating valve HV3454
and then open sequentially valves FZ08, FZ05, FZ07 and close FL04
again and set tail gas regulating valve FV3442 to auto. Until now, the
process for feed gas to change over from pre-emptying to membrane
separators is completed.
1.5.1.4.5. Open valve FZ10, set regulating valve TV3414A to auto and control
the permeating gas heating temperature. In this operating process,
the above procedure must be strictly followed to prevent counter-
pressure buildup in membrane separators, which refers to
permeating gas pressure being higher than that of membrane inlet.
1.5.1.4.6. Instrument functions and parameters:
 PI3403- Indicate membrane penetrating feed gas pressure,
(0.695 MPa)
 FI3441- Indicate membrane penetrating feed gas flow,
(2762Nm3/h)
 HIC3454- Regulating valve, which is fully opened during
normal operation and closes automatically during shutdown.
 TIC3414A- Permeating gas temperature controller, (90°C)
1.5.1.4.7. Discharge of permeating gas. The permeating gas separated from
six membrane separators concentrates in the header with a pressure
0.695MPa for going to subsequent procss. During normal operation,
pneumatic ball valve HV3457 will open and close during shutdown,
playing a role of enclosed protection to membrane separators.
Regulating valve HV3456 is used for replacement and emptying
during startup and for permeating gas emptying during shutdown,
which is closed during normal operation. Valves FH1, FH3 are check
valves to prevent counter-pressure. A71346 is sample-analyzing
valve.
1.5.1.4.8. Instrument functions and parameters:
 PI3404- Indicate permeating gas pressure, (0.695MPa)
 FIC3442- Permeating gas flow controller, (2762Nm3/h)
1.5.1.4.9. Tail gas discharge. 85% H2 in feed gas will be separated in six
membrane separators with the remaining tail gas to be discharged
after the flow being stabilized by membrane regulating valve. The tail
gas regulating valve shall be mainly used for flow control and

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PRODUCTION & OPERATION SPECIAL EQUIPMENT
CCR UNIT KRCIM 71300.07 REV.0

regulating, i.e. controlling the flow of permeating gas, which plays a


ole of protecting membrane separators during shutdown interlock.
1.5.1.4.10. Valve FZ13 shall be used for replacement and emptying during
startup, which is closed during normal operation. Valve FH2 is a
check valve, which prevents counter-pressure during shutdown. A
71345 is sample-analyzing valve.
1.5.1.4.11. Instrument functions and parameters:
 FV3442-Permeating gas flow control and regulating valve
 PI3405-Indicate tail gas pressure, (1.8MPa)
1.5.1.5. Replacement with nitrogen should be made first for the whole equipment
during startup.
Use nitrogen in startup with the requirements for pressure, temperature
to be the same as that for normal startup procedure.

1.5.2. Shutdown procedure

1.5.2.1. Normal shutdown

1.5.2.1.1. Notify related posts about shutdown.


1.5.2.1.2. Press the shutdown button, pneumatic baIl valve HV3451 will open,
other regulating valves and pneumatic baIl valves will simultaneously
close, and membrane separators will go into enclosed protection
state automatically.
1.5.2.1.3. Close valve FZ0l, FZ05, FZ07, FZ08.
1.5.2.1.4. Open regulating valve HV3456 for permeating gas emptying to empty
permeating gas slowly.
1.5.2.1.5. In case of temporary shutdown, the part of feed gas under
pretreatment shall not be necessary to be emptied. In case of long
shutdown, the part of feed gas under pretreatment must be emptied
through regulating valve HV3455.
1.5.2.1.6. Filling nitrogen for protection shall be necessary if the shutdown will
remain for 8 hours.
1.5.2.1.7. After shutdown, open differential pressure transmitters, and
differential pressure balance valves.

1.5.2.2. Emergency shutdown

1.5.2.2.1. In case of receiving any request for other posts or any failure to the
equipment requiring emergency shutdown, operate to normal
shutdown procedure.
1.5.2.2.2. When any operating parameter of the equipment exceeds that as
required, the equipment will shut down under automatic control of the
safety interlock system and enter into enclosed protection state. At
this point, operators should deal with it by following step 1.5.2.1.3 to
1.5.2.1.7 for normal shutdown.

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KRC CATALYST REGENERATION SECTION
PRODUCTION & OPERATION SPECIAL EQUIPMENT
CCR UNIT KRCIM 71300.07 REV.0

1.6. Attentions In Operation

1.6.1. Operations must be kept slowly for increasing and decreasing pressure during
the process of startup, shutdown.
1.6.2. The difference in pressure between feed gas and permeating gas must be put
under strict control below 2.5MPa. Excessive pressure difference can result in
damage to separator.
1.6.3. No counter-pressure shall be allowed regardless of which state a membrane
separator is it, startup, shutdown, or operation, i.e. the pressure of PI3404
should never be greater than that of PI3403.
1.6.4. Keep the temperature under strictly control at 45 °C during temperature rise for
heating feed gas.
1.6.5. Forward and back difference in pressure must be within the permissible range
for filter. When the pressure difference is too high, it is necessary to change
over to another filter group to ensure efficient filter working normally.
1.6.6. Maintain frequent inspections, maintenance to control instruments to keep them
under normal working state.

1.7. Process Parameters Under Normal Operation

Instrument Operation High alarm High interlock


Unit
number value value value
PI3401 2.08 MPa(g)
PI3402 2.08 MPa(g)
PI3403 2.0 MPa(g)
PI3404 0.695 MPa(g)
PI3405 1.8 MPa(g)
TI3411 40 °c
TI3412 35 °c

TI3413 45 °c

TI3414 90 °c

TI3415 45 55 60 °c

TI3416 <30 °c
LIA3421 <30 30 50 %
PdIA3431 <0.15 0.18 . MPa(g)
FI3441 2652-2762 Nm3/h
FI3442 2072-2158 Nm3/h

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PRODUCTION & OPERATION SPECIAL EQUIPMENT
CCR UNIT KRCIM 71300.07 REV.0

Field indications:
Instrument number Operation value unit
PG3481 2.08 MPa
PG3482 2.08 MPa
PG3483 2.05 MPa
PG3484 2.0 MPa
PG3485 2.0 MPa
PG3486 1.8 MPa
PG3487 1.8 MPa
PG3488 0.695 MPa
PG3489 0.695 MPa
PG3490 >0.8 MPa
PG3491 1.0 MPa
PG3492 >0.4 MPa
PG3493 0.3 MPa
TG3461 40 °C
TG3462 35 °C
TG3463 45 °C
TG3464 45 °C
TG3465 90 °C
TG3466 180 °C
TG3467 <30 °C
LG3422 <30 %
PdG0l-06 Green zone

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PRODUCTION & OPERATION SPECIAL EQUIPMENT
CCR UNIT KRCIM 71300.07 REV.0

2. Regeneration Loop Dryer DR-71301


2.1. Dryer principle:
2.1.1. Purpose: Dry recycle gas in regeneration loop to meet the water content
required.
2.1.2. If regeneration gas is not dried, water content in circulation loop gas will return
to regenerator and contact with catalyst leaching chlorine from the catalyst.
This phenomena cause severe fall of catalyst activity; Moreover, catalyst
attrition might occur producing heavy catalyst powders and causing failure of
catalyst circulation system and shutdown of complete unit.
2.1.3. Dryer is also safeguarding regeneration gas compressor against damage.

2.2. General Description


2.2.1. The DR-71301 dryer is an adsorption dryer with thermal regeneration loop. The
desiccating is carried out by adsorption on solid balls of desiccant put in proof
vessel withstanding pressure.
2.2.2. When the desiccant has absorbed a certain quantity of water, it must be
regenerated.
2.2.3. To obtain a continuous working, the dryer includes two vessels. One vessel is
in drying phase (at network pressure) when the other one is in regeneration.
The heating of desiccant is carried out by a steam heater where a part of the
gas flow is heated. Regeneration of desiccants ends by cooling by means of
the same part of the gas flow.
2.2.4. The gas distribution and the change over of the vessels is achieved by means
of valves which are driven by PLC. Some sensors (temp, pressure, level and
position) check continuously the correct running of the unit in accordance with
PLC.

2.3. Process Description


2.3.1. The unit's dryer has two switchable adsorbers through valve YV4 and YV2. Gas
enters adsorber, pass through desiccant bed and moisture is adsorbed by drier.
Dried gas flows out of the unit through valve YV1 and YV3.
2.3.2. Regeneration recycle gas from D-71306 enters the dryer through master
separator (PF). Outlet gas is separated into two streams. One to undergo
drying through the drying vessel (D1/D2) and other stream to perform
regeneration of other drum.
2.3.3. Desiccant drying gas enters heater (H), superheated, and pass through tee
valveYV4 and four-way valve YV2 to (D1/D2) for desiccant regeneration. Out of
the top of (D1/D2), through four-way valve YV1 and tee valve YV3,
regeneration outlet gas enters cooler (C1) and (SEP1) for dehydration.
2.3.4. After dehydration, regeneration outlet gas combines with the gas from other
outlet stream of (PF). Combined gas enter (D2/D1) through four-way valve YV1
for gas drying.
2.3.5. After drying, gas from (D2/D1) bottom, pass through four-way valve YV2, and
enters regeneration loop filter M-71303. Gas is filtered and enters K- 71301 for
recycle use.

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CCR UNIT KRCIM 71300.07 REV.0

2.4. Major Technical Parameters:


 Media: Nitrogen 81.11%vol CO2 16.43%vol O2 0.78%vol
 Max Cl content in gas: 20ppm (v)
 Processing capacity: 7888 m3/h
 Operating pressure: 0.36 MPa
 Inlet temperature: 42˚C
 Inlet water content: 1.68% (Saturated at normal operating conditions)
 Outlet temperature: less than 57˚C

2.5. Efficiency
H2O content at outlet is less than 50ppm(v)

ISSUE DATE: 20/03/06 - 95 -

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