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07 - GAS DEHYDRATION - Rev 8.3
07 - GAS DEHYDRATION - Rev 8.3
GAS DEHYDRATION
Exploration & Production – DGEP/DEV/ED/ECP
PRODEM Date : 02/2011
Section N° VII-A
GAS DEHYDRATION
Dehydration methods
PRODEM
SECTION N° VII-A
GAS DEHYDRATION
DEHYDRATION METHODS
REVISIONS
L. PAGNON
8 02/2011 Major Revision T. BRENAS A. GERVAIS A. ROCHER
ENEA Consulting
CONTENTS
Revisions........................................................................................................................................ 1
References ..................................................................................................................................... 2
Definitions ..................................................................................................................................... 3
Overview ....................................................................................................................................... 5
1. Purpose of Gas Dehydration .................................................................................................... 6
1.1. Gas water content ......................................................................................................................... 6
1.2. Gas Dehydration process ............................................................................................................... 6
1.3. Gas dehydration unit in the plant ................................................................................................... 6
2. Main Gas Dehydration Processes ............................................................................................. 7
2.1. First group: Gas dehydration by absorption process........................................................................ 7
2.2. Second group: Gas dehydration by adsorption process ................................................................... 8
2.3. Third group: Gas dehydration by refrigeration with hydrate inhibition ............................................ 9
3. Selection of Gas Dehydration Process .................................................................................... 10
3.1. Dehydration methods operating range ......................................................................................... 10
3.2. Gas dehydration methods comparison ......................................................................................... 11
FIGURES
Figure VII-A. 1 – Operating window for absorption and adsorption process ................................................ 11
TABLES
Table VII-A. 1 – Dehydration methods comparison ..................................................................................... 14
REFERENCES
Internal
External
[3] F.S. Manning & R.E. Thompson - Oil Field Processing of Petroleum (1991)
Natural gas, Vol. 1
Pennwell Books Publishing Company - Tulsa (Oklahoma)
DEFINITIONS
Absorption: Gas absorption is a unit operation in which components of a gas mixture are transferred from gas
to liquid phase via physical solubility or via chemical bond.
Azeotrope: Mixture of two or more liquids (chemicals) in such a ratio that its composition cannot be changed
by simple distillation.
Azeotropic distillation: Distillation is the most widely used separation technique in the chemical and petroleum
industry. However, not all liquid mixtures are amenable to ordinary fractional distillation. When the
components of the system have low relative volatilities, separation becomes difficult and expensive because a
large number of trays are required and, usually, a high reflux ratio. Refer to PRODEM Chapter XII – Gas
Sweetening (Hyperlink)
Critical Velocity: The critical velocity is the terminal velocity of the liquid droplets which have the smaller
diameter value. Its expression is obtained from the Newton’s law, taking for droplet diameter the value 80μm.
See PRODEM Chapter XVII – Liquid/Vapor separators (Hyperlink) for further information.
L V
C 0.048 * Eqn 2
V
C : Critical Velocity in m/s.
3
L : lean glycol density at absorber operating conditions in kg/m .
3
V : dry gas density at absorber operating conditions in kg/m .
Distillation: Distillation is a physical separation process using external heat input. Components from a liquid
boiling mixture are separated based on their different volatilities. In continuous distillation mode, gas / liquid
phase contact is performed using random or structured packing, or trays.
Dew point depression: The dew point depression is the difference between the temperature and dew point
temperature at a given pressure. Water dew point depression is one way to specify the moisture content of
the dehydrated gas.
Kvalue: Kvalue is called the gravity separator factor, and is dimensionless. It is used to define the maximum
allowable velocity value for a mist elimination system, according to the following equation:
Kvalue*c Eqn 3
: Maximal allowable velocity in m/s.
C : Critical Velocity in m/s.
Hydrocarbon Dew Point: The hydrocarbon dew point is the temperature (at a given pressure) at which the
hydrocarbon components of any hydrocarbon-rich gas mixture, such as natural gas, will start to condense.
Stripping: Liquid stripping with a gas stream is a separation process where volatile components from liquid are
transferred to gas phase according to thermodynamic gas-liquid equilibrium. Stripping gas may be introduced
as an external gas source (fuel gas, inert gas, steam) or generated by reboiling the liquid using external heat
input or by decreasing pressure (vacuum column). Stripping or desorption is the opposite operation of
absorption.
Reclaimer: Main equipment (contactor or column) part of reclaiming process that restores the properties of
the solvent contaminated by salts as impurities, like calcium or sodium chlorides for glycols. The reclaiming
process should not be confused with the glycol regeneration process. Vacuum distillation or ion exchange are
the main industrial processes used to treat salty glycols.
Regenerator: Column and associated equipment that aim at regenerating the absorption properties of the
solvent for re-use in the absorber. In glycol dehydration, the regenerator is composed of the reboiler, the still
column and the reflux condensers and drum.
Water-saturated: A gas is said "water saturated" when it contains the maximum of the amount of water
vapour possible at given conditions. This maximum depends on pressure, temperature, and composition.
Water Dew point: A water-saturated gas at given conditions (pressure and temperature) is said at its "water
dew point", meaning that water-vapor begins to condens, when gas is slightly cooled at constant pressure. The
water content of a gas is very often defined by the couple of pressure and temperature values of the "gas
water dew point".
OVERVIEW
Introduction
As part of the Total E&P PRODEM manual, this chapter provides a reference tool for Total E&P process
engineers. PRODEM aims to provide the user with technical information and a standard set of tools to
facilitate process design. The contents of this chapter are relevant to all Total E&P process engineers.
General Content
This section is an introduction to the other sections of the Gas Dehydration PRODEM chapter. It deals with:
General information regarding gas dehydration.
The fundamentals of the principle gas dehydration methods: physical absorption, physical adsorption,
and gas refrigeration.
The typical application of the different methods summarized in a comparative table.
Reservoir fluids are always saturated with water at reservoir conditions, thus natural gas at wellhead
conditions is always saturated with water.
Gas water content is further discussed in PRODEM chapter IV - Fluid Behaviour (Section A – Water content of
natural gas and associated gases).
The process of gas dehydration consists in reducing water content from the saturated wet gas stream in
order to lower the temperature at which water will condense or hydrate or ice will appear, at a given
pressure. This temperature is called the "water dew point" of gas for a given operating pressure.
For the European Consortium (Germany, Belgium, Netherlands, France), the typical value of water dew point is
minus 15 °C at 69 bar abs.
It corresponds to a maximum amount of water in the gas at Standard conditions of approximately 40 kg/10 6
Sm3 or 2.5 lb/106 Scf.
In terms of capital investment and energy, gas dehydration is often a minor part of the total plant. On offshore
platforms, the dehydration unit is often the largest single package and strongly affects weight and layout
requirements.
Natural gas can be dehydrated by several processes depending on the specifications to be reached: pipeline
transport, sales gas, NGL recovery or gas liquefaction.
These processes can be classified in three main groups:
Absorption process
Adsorption process
Refrigeration with hydrate inhibition process
Absorption and adsorption units are designed with two functions: gas dehydration and solvent / media
regeneration.
Absorption
Diethylene glycol (DEG), triethylene glycol (TEG) and tetraethylene glycol (TREG) possess the above
characteristics. However, TEG is more often used than DEG or TREG.
Absorption units are used for common applications where required water dew point depressions are in the
order of 30°C to 70°C (average 50°C).
Regeneration
During this dehydration process, glycol needs to be continuously regenerated, conventionally by reboiling with
or without gas stripping or by azeotropic distillation like in the DRIZO process.
Adsorption
In adsorption water molecules from the gas are held on the surface of a solid by surface forces.
Adsorbents may be divided in two classes: those which owe their "activity" to surface adsorption and capillary
condensation, and those which react chemically. Only the first class of adsorbents is used in the dehydration of
natural gas, a process referred to as "physical adsorption processes".
Activated alumina, silica gel and molecular sieves are materials which meet these characteristics and are
common in commercial use. Molecular sieves possess the highest water capacity and produce the lowest
water dew point. For these reasons they are currently the most common desiccant used.
Molecular sieve dehydrators are commonly used ahead of NGL recovery plants where extremely dry gas is
required due to very cold temperatures reached (around - 80°C) Molecular sieves are also used for the same
reason in natural gas liquefaction plants where temperature of - 165 ° C is reached in the process.
Compared with the other gas dehydration processes, molecular sieve is the most expensive due to dessicant
costs.
Regeneration
Regeneration of dessicant beds consists in heating steps in order to desorb water. Dehydrated process gas is
usually heated and used to sweep the dessicant beds. Heat ramp up speed is defined by dessicant supplier to
prevent destroying dessicant beds (by bursting bubbles). Once water is desorbed, heater is turned off and
sweep gas will cool down the dessicant beds.
Regeneration of silica gel and alumina can be accomplished at 150°C. Molecular sieve requires 260-290°C to
maintain the low dewpoint potential. High temperatures may increase desiccant life by providing more
complete removal of adsorbed hydrocarbons.
This 3rd group is also called expansion refrigeration or Low Temperature Separation (LTS) process. Feed gas is
chilled and condensate and water are separated in a 2-stage 3-phase separator, called “hot separator” for the
1st stage and “cold separator” for the 2nd stage.
The LTS process enables to meet water and HC dew points simultaneously specified by pressure and
temperature of the cold separator.
The expansion refrigeration requires high pressure gas feed while the external refrigeration is CAPEX
consuming. Due to low temperature reached by refrigeration, icing and hydrate inhibition is performed by
monoethylene (MEG) or diethylene (DEG) or methanol injection. Selection of inhibitor depends on operating
conditions and is driven by inhibitor viscosity limitation for low temeprature, vapor loss limitation for high
temperature, water – condensate separation efficiency and foaming tendancy, and limitations due to the
refrigeration process itself (e.g. liquid droplets to be avoided at inlet of expansion turbines).
Regeneration
Low Temperature Separation processes using methanol do not always have a regeneration unit for mild
depression value or low gas volumes. Methanol is usually lost in the gas and condensate. A dedicated
regenerator is required if methanol is recirculated.
Low Temperature Separation processes using glycols (MEG typically) do regenerate the used glycol.
Preliminary selection is usually between glycol contactor and solid dessicants while refrigeration is typically
used in specific process like NGL recovery, LNG production or simultaneous water and HC dew-pointing. For
the refrigeration case, a dedicated comparative study among the three options for gas chilling, is usually
required prior decision making process.
Outside these specific applications, some criteria are given below on when to select the refrigeration unit with
hydrate inhibitor injection:
Low gas flowrate: CAPEX and / or lay-out usually prohibits a contactor – regenerator system
Infrequent or periodic hydrate formation conditions or temporary hydrate formation conditions in the
course of phased field development
Acceptable methanol consumption (but needs to be within sales gas / condensate specifications)
High feed gas pressure required for Joule Thompson valve or turbo-expander
Preliminary indication for selecting suitable dehydration method between absorption and adsorption is given
in Figure VII-A. 1.
Adsorption process is generally used over adsorption for lower gas water content applications.
Source : [6]
Main characteristics of the three groups are summarized in the following Erreur ! Source du renvoi
introuvable.
1
DRIZO process can even achieve water dew point temperatures of -100°C.
2
Higher dew point depressions can be achieved by enhanced processes: from 80°C to 100°C and more by DRIZO processes.
3
Less than –100°C can be accomplished with special design and strict operating parameters.
4
Dehydration to between –80°C and –100°C dewpoint is possible with IFPEXOL (at 80 bar abs).
5
Achievable with the use of limited chemical injection. In chemical free operation, Twister can achieve a water dew point of –10°C at 80 barg.
6 6 3 6 3
Glycols can dehydrate natural gas to about 8 kg H2O/10 Sm , but 4 kg H2O/10 Sm can be achieved with a stripping gas and a stripping column which is
6 3
currently a standard equipment. DRIZO process allows to limit water vapour content to 1 kg H 2O/10 Sm .
7
Prosernat, licensor of the IFPEXOL process, uses its owns in-house conversion from water dew point to water content specification. This value can’t be
compared with the water content specifications claimed by other licensors and processes.
8 6 3
With limited chemical injection. In chemical free operation, the water vapour content is 45 kg H2O/10 Sm .
DIRECTION GENERALE EXPLORATION PRODUCTION
This document is the property of Total. It must not be stored, reproduced or disclosed to others without written authorisation from the Company.
Exploration & Production – DGEP/DEV/ED/ECP
PRODEM Date : 02/2011
Section N° VII-A
GAS DEHYDRATION
Dehydration methods Page 13
Glycol make-up is easily accomplished. Recharging solid desiccant towers is time- Methanol injection has a low investment
consuming and sometimes requires the cost but a high operating cost due to the
Requires less regeneration heat per kg of
Operational interruption of gas sales. chemical consumption.
water removed, lowering utility costs.
costs High regeneration heat requirements and Injection of MEG or DEG requires a higher
high utility costs. initial cost but a relatively low operating
cost.
9
Low pressure drop. High pressure drop . Low pressure and cryogenic temperatures.
Operational
Dessicants less affected by small changes in No heat is required for the process and no
conditions
gas pressure, temperature or flowrate. atmospheric venting takes place.
9
Thus, if regeneration gas cannot be used as fuel gas, a regeneration gas compressor is required and the dehydration unit capacity shall be increased to take
into account this regeneration gas (about 10 % of the feed gas).
DIRECTION GENERALE EXPLORATION PRODUCTION
This document is the property of Total. It must not be stored, reproduced or disclosed to others without written authorisation from the Company.
Exploration & Production – DGEP/DEV/ED/ECP
PRODEM Date : 02/2011
Section N° VII-A
GAS DEHYDRATION
Dehydration methods Page 14
This point is particularly important for field - Alumina regeneration requires much heat
DEG: not recommended generally below
units such as wellhead or flowline streams - Silica gels can’t handle H2S concentration
minus 10°C because of its viscosity and the
Agent containing treatment chemicals and solids, higher than 5 - 6 wt % as sulfur deposits can
requirements difficulty of separation if oil is present.
e.g., sand, pipeline scale and rust (fine iron block their surface.
and Above minus 10°C, it might be preferred as
sulfide, etc...). - Molecular sieves are alkaline and subject to
vulneranility there is less vaporisation on loss than MEG
attack by acids..
Glycol loss in case of a foaming problem can or methanol.
be excessive and costly. Glycols are Mechanical breaking of desiccant particles.
susceptible to contamination, which induces Dessicants can poison heavy hydrocarbons,
corrosivity. methanol, treatment chemicals and solids.
PRODEM
SECTION N° VII-B
REVISIONS
T. BRENAS
P. CHILLEMI
8 12/2011 Major Revision A. GERVAIS A. ROCHER
L. PAGNON
ENEA Consulting
CONTENTS
Revisions........................................................................................................................................ 1
References ..................................................................................................................................... 5
Glossary ......................................................................................................................................... 6
Acronyms ....................................................................................................................................... 7
Overview ....................................................................................................................................... 8
1. General information regarding Physical Absorption Process .................................................. 10
1.1. Gas – liquid mass transfer principle .......................................................................................10
1.2. Absorption principle ...............................................................................................................11
1.2.1. Absorption and regeneration ..........................................................................................................11
1.2.2. Absorbing agents: Glycol .................................................................................................................11
1.2.3. Solubility ..........................................................................................................................................13
1.2.4. Azeotropes .......................................................................................................................................14
1.3. Main processes description....................................................................................................18
1.3.1. Basic TEG absorption method..........................................................................................................19
1.3.2. Enhanced stripping processes .........................................................................................................22
1.4. Selection criteria of physical absorption processes ...............................................................33
2. Glycol Dehydration Process Design ........................................................................................ 35
2.1. Equipment characteristics ......................................................................................................35
2.1.1. Conventional TEG Unit .....................................................................................................................35
2.1.2. TEG regeneration with stripping gas ...............................................................................................52
2.1.3. DRIZO process: additional equipments ...........................................................................................53
2.2. Simplified calculation method to define main parameters of TEG dehydration ...................55
2.2.1. Information required for calculation ...............................................................................................55
2.2.2. Simplified calculation method to determine the minimum lean TEG concentration and flowrate 55
2.2.3. Example............................................................................................................................................65
2.2.4. Economical approach.......................................................................................................................67
2.2.5. Calculation tool ................................................................................................................................68
2.2.6. Calculation tool manual ...................................................................................................................70
2.2.7. Previous designs ..............................................................................................................................71
3. Operational Data................................................................................................................... 73
3.1. Usual Operation Conditions ...................................................................................................73
3.1.1. Usual glycol unit operating temperatures .......................................................................................73
3.1.2. Usual glycol losses ...........................................................................................................................73
3.1.3. Usual glycol circulation rate.............................................................................................................74
3.2. Control in TEG units ................................................................................................................74
3.3. Troubleshooting operating problems and solutions ..............................................................75
3.3.1. Inlet scrubbing .................................................................................................................................75
FIGURES
Figure VII-B. 1 – DEG and TEG density, heat capacity and viscosity ................................................................................. 13
Figure VII-B. 2 – Solubility in TEG .................................................................................................................................... 14
Figure VII-B. 3 – Positive or minimum boiling azeotrope ................................................................................................ 14
Figure VII-B. 4 – Negative or maximum boiling azeotrope .............................................................................................. 15
Figure VII-B. 5 – Positive azeotrope of the water-benzene mixture ................................................................................ 15
Figure VII-B. 6 - TEG, water and benzene mixture equilibrium mapping ......................................................................... 16
Figure VII-B. 7 - Boiling temperature of the TEG and water mixture, and the TEG and water-benzene azeotrope mixture
............................................................................................................................................................................... 16
Figure VII-B. 8 – Influence of the positive deviation on the separation efficiency ........................................................... 17
Figure VII-B. 9 – Absorption column ............................................................................................................................... 18
Figure VII-B. 10 – Glycol type gas dehydration with integrated condenser ..................................................................... 20
Figure VII-B. 11 – Glycol type gas dehydration with external condenser ......................................................................... 21
Figure VII-B. 12 – Typical schematic flow diagram of a DRIZO unit .................................................................................. 24
Figure VII-B. 13 – Process scheme of COMART-COLDFINGER process.............................................................................. 26
Figure VII-B. 14 – BS&B process scheme ......................................................................................................................... 27
Figure VII-B. 15 – Progly process scheme ........................................................................................................................ 28
Figure VII-B. 16 – Lussagnet PROGLY photograph ........................................................................................................... 28
Figure VII-B. 17 – Dehydration performance for countercurrent and cocurrent contactors ............................................ 29
Figure VII-B. 18 – Equipment weight compositions for the Asgard B case ....................................................................... 29
Figure VII-B. 19 – Process flow diagram of DRIGAS-1 ...................................................................................................... 30
Figure VII-B. 20 – Performance of DRIGAS in comparison to conventional and improved stripping ................................ 31
Figure VII-B. 21 – Process flow diagram of DRIGAS-2 ...................................................................................................... 31
Figure VII-B. 22 – Process flow diagram of DRIGAS-3 ...................................................................................................... 31
Figure VII-B. 23 – Process flow diagram of ECOTEG-1 ..................................................................................................... 32
Figure VII-B. 24 – TEG purity and water dew point ......................................................................................................... 34
Figure VII-B. 25 – Glycol Absorber................................................................................................................................... 37
st
Figure VII-B. 26 – Mellapack (1 generation – Sulzer) ..................................................................................................... 38
nd
Figure VII-B. 27 – Mellapack Plus (2 generation – Sulzer) ............................................................................................. 38
Figure VII-B. 28 – SULZER MELLAPACK PLUS ................................................................................................................... 39
Figure VII-B. 29 – Shell swirl tube tray ............................................................................................................................ 40
Figure VII-B. 30 – Column diameter for different internals ............................................................................................. 41
Figure VII-B. 31 – V-mister flow arrangement ................................................................................................................. 42
Figure VII-B. 32 – SULZER V-MISTER ................................................................................................................................ 43
Figure VII-B. 33 – Swirltube deck functioning.................................................................................................................. 43
Figure VII-B. 34 – Swirltube deck configurations ............................................................................................................. 44
Figure VII-B. 35 – Shell swirltube deck ............................................................................................................................ 44
Figure VII-B. 36 – Packing................................................................................................................................................ 46
Figure VII-B. 37 – TEG regeneration with stripping gas ................................................................................................... 52
Figure VII-B. 38 – DRIZO additional equipments ............................................................................................................. 53
Figure VII-B. 39 – Equilibrium water vapour content of sweet natural gas (Wichert Chart) ............................................ 57
Figure VII-B. 40 – Equilibrium H2O Dewpoint vs. Temperature at Various TEG Concentrations ..................................... 59
Figure VII-B. 41 – Activity coefficient for H20 concentration at various temperatures .................................................... 60
th
Figure VII-B. 42 – Iterative procedure for 6 step ........................................................................................................... 61
Figure VII-B. 43 – Densities of aqueous TEG solutions ..................................................................................................... 62
Figure VII-B. 44 – Effect of Stripping Gas on TEG Concentration...................................................................................... 63
Figure VII-B. 45 – Physical absorption design calculation sheet example ........................................................................ 70
Figure VII-B. 46 – DRIZO temperature control ................................................................................................................. 79
Figure VII-B. 47 – Nkossa DRIZO photographs ................................................................................................................. 80
Figure VII-B. 48 –DRIZO reboiler heaters position ........................................................................................................... 82
Figure VII-B. 49 – Nkossa DRIZO PFD and equipments .................................................................................................... 82
TABLES
REFERENCES
Internal
External
[3] F.S. Manning & R.E. Thompson - Oil Field Processing of Petroleum (1991)
Natural gas, Vol. 1
Pennwell Books Publishing Company - Tulsa (Oklahoma)
th
[5] G.P.S.A. Engineering Data Book 12 edition Section 20
Gas Processors Suppliers Association, 6526 East 60th Street, Tulsa (Oklahoma)
[7] D.L. Katz and R.L. Lee, Natural gas Engineering. Production and Storage
Mc. Graw Hill Publishing Company
th
[8] A. Kohl and R. Nielsen, Gas purification 5 edition, 1997
Gulf Publishing Company – Book Division
[10] Daniel Egger and Kurt Breu, Sulzer Chemtech Ltd - Economical glycol contactor design
determined by novel column internals
GLOSSARY
METRIC IMPERIAL
SYMBOL DEFINITION
UNITS UNITS
LATIN CHARACTERS
A Absorption factor - -
c Minimum rich TEG weight concentration wt % wt %
Cmin Minimum lean TEG weight concentration wt % wt %
C Lean TEG weight concentration wt % wt %
Ci Molar concentration of a species in a mixture. mol/m3 mol/ft3
Co Standard molar concentration (1 mol/m3) mol/m3 mol/ft3
D Absorber diameter with structured packing m ft
DBubble cap Absorber diameter with bubble caps. m ft
Dsc Stripping column diameter m ft
F Flow factor - -
J Diffusive flux mol/(m2*s) mol/(ft2*s)
k°H Henry’s law constant for solubility in water mol/kg*bar mol/lb*psi
Kvalue Gravity separator K value - -
Kvs Vapor/solid equilibrium - -
L Glycol molar circulation rate kmol/h kmol/h
Lvol Glycol volumetric circulation rate m3/h ft3/h
M Lean glycol molecular weight kg/kmol lb/kmol
MG Gas molecular weight kg/kmol lb/kmol
m Minimum lean TEG circulation rate kg/h lb/h
mG Gas mass flowrate kg/h lb/h
mL Liquid mass flowrate kg/h lb/h
Q Maximum wet gas flowrate Sm3/day Scf/day
r Amount of lean TEG circulation rate per unit of removed water - -
Re Reynolds number - -
Sc Schmidt number - -
Sh Sherwood number - -
V Fluid velocity m/s ft/s
Wi Water vapour content of inlet gas kg/Sm3 lb/ Scf
Wo Water vapour content of inlet gas kg/Sm3 lb/ Scf
Wr Amount of water to be removed from gas, kg/hr lb/h
xw Molar fraction of water in lean glycol. mol % mol %
yw Molar fraction of water in gas mol % mol %
yws Molar fraction of water in gas at saturation, usually equal to the mol % mol %
molar fraction of water in the inlet gas
GREEK CHARACTERS
Activity coefficient for water in the TEG-water system - -
i Activity coefficient of a species in a mixture. - -
ρ Fluid density kg/m3 lb/ft3
ρG Gas density at absorber conditions kg/m3 lb/ft3
ρL TEG density at absorber conditions kg/m3 lb/ft3
ν Superficial velocity m/s ft/s
νc Critical velocity m/s ft/s
Table VII-B. 1 – Glossary
Note: The equations used in this chapter are meant to be used with metric units. Should the user prefer the
imperial units, the conversion should be done only once the calculation has been performed with the metric
units based equation, converting the inputs beforehand and the results afterwards. The conversion
coefficients from metric to imperial units and reverse are given in chapter 1 of PRODEM.
ACRONYMS
SYMBOL DEFINITION
BTEX Benzene, Toluene, Ethyl-benzene and Xylenes
DEG Diethylene glycol
HC Hydro carbons
TEG Triethylene glycol
TREG Tetraethylene glycol
vol volumetric
wt weight
Table VII-B. 2 – Acronyms
OVERVIEW
Introduction
As part of the Total E&P PRODEM manual, this chapter provides a reference tool for Total E&P process
engineers. PRODEM aims to provide the user with technical information and a standard set of tools to
facilitate process design. The contents of this chapter are relevant to all Total E&P process engineers.
This particular section is dedicated to physical absorption process design, part of gas dehydration methods.
The physical absorption process removes water from gas, thus preventing hydrate formation and corrosion.
Guidelines
General information regarding physical absorption processes, such as:
Detailed process description, including the absorption and regeneration phases
Operational feedback:
Description of operational conditions
Description of gas dehydration process control
Operational feedback on troubleshooting operating problems and solutions and preventive
maintenance
Examples of TEG units studied or operated by TOTAL
In film theory, gas – liquid interface is described as superimposed 2 layers: gas phase boundary layer and liquid
phase boundary layer. gas – liquid interface being the contact surface of these two.
Gas – liquid mass transfer flux of a solute is described by Fick’s law:
J = D * a * C/y Eqn 1
For highly soluble gas (H << 1): KG = kg : Mass transfer limitation is on gas side
For sparingly soluble gas (H >> 1): KL = kl : Mass transfer limitation is on liquid side
The above equations highlight that mass transfer is driven by gas or liquid film conductance, interfacial area
and concentration gradient. Both film conductance and interfacial area are functions of hydrodynamic
conditions and fluid properties.
Dimensionless analysis of mass transfer problems usually correlates the Sherwood number Sh to Reynolds
number Re and Schmidt number.
The Sherwood number designates the convection mass transfer divided by the diffusion mass transfer.
The Schmidt number designates the viscous diffusion divided by the molecular diffusion.
Sc = μ/ρ.D Eqn 5
Early 1930s, glycerol, calcium chloride and diethylene glycol were used for gas dehydration.
Nowadays, liquids commonly used for dehydrating natural gas, are triethylene glycol (TEG), diethylene glycol
(DEG) and tetraethylene glycol (TREG). The use of monoethylene (MEG) is less frequent.
Compared to TEG, DEG has a large carry-over loss, offers less dew point depression and regeneration to high
concentrations is more difficult. Therefore, it is difficult to justify a DEG unit although a few are built each year.
DEG is preferred below around 10°C due to too viscous TEG. Otherwise TEG is recommended for temperature
below around 50°C.
TREG is more viscous and more expensive than the other processes. The only real advantage is its lower
vapour pressure which reduces absorber carry-over losses. It may be used in those relatively rare cases where
gas temperature exceeds about 50°C.
Glycol blends containing side products from manufacturing process, available at low cost, can be used for gas
dehydration but their efficiency is lower than high purity glycol.
Physical properties of glycols are given in Table VII-B. 3. Additional characteristics of TEG and DEG are given in
Material Safety Datasheet (MSDS) in Appendix 1.A and Appendix 1.B.
TEG is the most commonly used glycol. Water dew point depressions range from 20°C to 70°C (average 50°C)
while inlet gas pressures and temperatures vary respectively from 5 to 170 bar abs and from 25°C to 60°C.
Enhanced processes can even achieve greater dew point depression: DRIZO process can thus achieve water
dew point depression of more than 100°C.
This section will thus only address gas dehydration with TEG.
1
Glycols decompose at temperatures below their atmospheric boiling point. Given decomposition temperatures are approximate,
based on laboratory tests.
Source: [5]
Figure VII-B. 1 – DEG and TEG density, heat capacity and viscosity
In gas process where liquid hydrate inhibitor is injected directly in the gas stream, Methanol and MEG are
often used. Methanol is preferred for cryogenic process (below -25 to -40°C) because of the high viscosity of
glycol at low temperature. MEG can be used for moderate gas temperature. (Refer to Section VII.D)
1.2.3. Solubility
Use of glycols in some gas dehydration processes (DRIZO for instance) also relies on the respective solubility in
glycols of aromatics and usual hydrocarbons.
Aromatics are by far more soluble in glycols than n-alcanes. For instance, benzene is completely soluble in TEG,
and toluene solubility in TEG at 25°C is as high as 24.8%.
Solubilities of n-alcanes in TEG are as shown on Figure VII-B. 2.
The reasons that make TEG suitable for water absorption is the following:
TEG and water are fully miscible liquids thus solubility of water in TEG is very high.
Solubility of hydrocarbons in TEG is poor compared to water (by the way TEG and hydrocarbons, even
aromatics, are partially miscible liquids up to a saturation solubility level)
1,E+00
1,E-01
Hexane
1,E-02
Decane
1,E-03
Methane
1,E-04
Source: Bryan Research and Engineering
Figure VII-B. 2 – Solubility in TEG
1.2.4. Azeotropes
The term azeotrope refers to a mixture of two or more components where the equilibrium vapor and liquid
compositions are equal at a given pressure and temperature. More specifically, the vapor has the same
composition as the liquid and the mixture boils at a temperature other than that of the pure components
boiling points:
If the mixture boils at a lower temperature than the boiling temperature of any of the pure components,
the azeotrope is called positive, or minimum boiling as illustrated on Figure VII-B. 3
If the mixture boils at a higher temperature than the boiling temperature of any of the pure
components, the azeotrope is called negative, or maximum boiling as illustrated on Figure VII-B. 4
The composition of azeotropes is unchanged by distillation, when boiling at a given temperature. Azeotrope
properties are used during so-called azeotropic distillations.
More component
1 in vapor phase
than liquid phase
The properties of the positive azeotrope are used in the DRIZO application, with a ternary TEG-Benzene-Water
azeotrope. A schematic representation of this ternary mixture equilibrium is shown on Figure VII-B. 6.
Benzene and water form a binary positive azeotrope (see Figure VII-B. 5). The mixture between this
composition and TEG has a boiling temperature lower than the binary mixture TEG and water (as shown on
Figure VII-B. 7). This explains why the distillation temperature is lower in the DRIZO application (193°C) with
regards to the usual glycol dehydration process (204°C).
As shown on Figure VII-B. 7, for a given expected purity, the required boiling temperature is lower in the
benzene-water-TEG mixture (red) compared to the water-TEG mixture (blue).
Furthermore, with the same benzene-water-TEG mixture, azeotropic properties induce an increase in the
efficiency of glycol regeneration: For the same given number of distillation stages the glycol regeneration
efficiency is improved. The formation of a minimum-boiling azeotrope is induced by a positive deviation from
Raoult’s law: The components “dislike” each other. The attraction between identical molecules is stronger
than between different molecules. The positive deviation thus induces a better efficiency as illustrated on the
schematic Figure VII-B. 8 here below:
y
1
x
y
Positive 1
deviation
3
x
Increase in
efficiency (purity)
The following three variables influence the treated gas dew point for a given inlet composition:
number of theoretical stages in the contactor
glycol circulation rate
glycol concentration
The concentration of the lean glycol is crucial. Indeed, gas dehydration efficiency depends on the lean glycol
concentration, resulting from the glycol regeneration.
Regenerating processes depend on the required TEG concentration to meet stringent gas dehydration
requirements:
TEG concentrations from 98.5 wt % to 99.0 wt % are achievable in a simple atmospheric pressure still
(gas purification).
When significantly higher concentrations are required (99.000 to 99.990 wt %), the use of enhanced
stripping techniques is necessary. Injection of a stripping gas is often used, with or without an additional
column.
Very high TEG concentrations from 99.990 to 99.999 wt % may be required in order to reach higher
water dew point depression. These concentrations are achievable in the patented DRIZO TEG
dehydration unit.
Figure VII-B. 10 provides a PFD of a basic glycol dehydration system with integrated condenser. A description
of this process is given below and compared with glycol dehydration with external condenser (Figure VII-B. 11).
Glycol regeneration
The rich glycol leaves the bottom of the absorber and flows first to a reflux condenser integrated at the top of
the regenerator still column (7). When the condenser is not integrated, as shown on Figure VII-B. 11, the flow
is directed to a lean glycol-rich glycol heat exchanger for preheating (7bis).
The heated rich glycol then enters a flash drum (8) where most of the volatile components, entrained and
soluble, are vaporized. The flash drum pressure typically ranges from 3 to 6 bar abs with a temperature
between 60 and 90°C. Leaving the flash drum (9), the rich glycol flows through the glycol filters (solid particles
and activated carbon filters). The glycol is then directed to the rich-lean glycol exchanger4 (10) where it
exchanges heat against the hot lean glycol. Finally, the rich glycol enters the regenerator still column (11).
In the regenerator, water is removed from the glycol by distillation and the glycol concentration is increased to
the lean glycol requirement. The regeneration unit is designed to operate at prevailing atmospheric pressure.
The top temperature is maintained at 100°C by an integrated (12) or an external condenser (12bis). An
electrical heater maintains the regenerator reboiler temperature very close to 204 °C for TEG5 (13). Other
heating means are described in 2.1.1.5.
Fuel gas coming from the fuel gas network is preheated in the regenerator reboiler (14), and is then
introduced at the stripping column where it strips water from the liquid glycol as it rises up (15).
The hot regenerated glycol flows out of the reboiler into the stripping column (16). Then it is cooled by heat
exchange against rich glycol (17) and flows to the accumulator (18). Finally, the lean glycol is pumped back into
the top of the absorber (19) through a cooler to control its inlet temperature in the absorber.
2
Cooling the entering wet gas with air or suitable water ahead of the glycol dehydration unit is the least expensive form of
dehydration. Lowering the capacity of the glycol dehydration unit allows lowering the investment costs.
3
Bubble cap trays have been used historically but structured packing is more common today. See dedicated section for details.
4
When the still column condenser is not integrated as shown on Figure VII-B. 11, two lean glycol/rich glycol exchangers are required.
5
TEG measurable decomposition begins to occur at 207°C.
6
12
11
4
16 13
5
15 14
2
1 17
10
3
9 18
8
19
7 bis
Fuel gas stripping, DRIZO process and Coldfinger process are the most common enhanced stripping processes.
Other processes based on TEG conventional dehydration exist and may easily be added to a conventional
glycol regeneration system. Such processes are described after.
Gas dew point is related to TEG purity: lower gas dew point depression requires higher TEG purity, as
illustrated by Figure VII-B. 40.
TEG purity commonly achieved through a standard regeneration process is around 98.5 wt % for a reboiling at
204°C and atmospheric pressure.
Stripping of residual water from this lean glycol can be enhanced without exceeding its decomposition
temperature by reducing the effective partial pressure of H2O in the vapour phase of the glycol reboiler.
Different mechanisms can be used: gas stripping, azeotrope formation, vacuum stripping, or condensation of
water from vapour phase.
DRIZO basis
DRIZO™ is a glycol (TEG) based gas dehydration process. Originally patented by the Dow Chemical Company in
the mid 70s, the license exclusivity was acquired in 1986 by OPC Engineering who further improved the
process. OPC DRIZO Inc has been acquired by PROSERNAT in 1998. PROSERNAT claims more than 60 industrial
references to date. This technology can be retro-fitted to existing glycol unit.
DRIZO™ regenerates the glycol by solvent stripping instead of the conventional gas stripping. This allows
obtaining much higher glycol purities than gas stripping, reaching concentrations above 99.990 wt % to 99.999
wt %. Consequently, it allows getting much larger water dew point depressions: up to 100 °C and even higher
in some cases.
DRIZO HP is a variation of DRIZO™ process with a dryer included in the solvent loop; it allows achieving lower
water dew point than with DRIZO™.
A process schematic of a DRIZO unit is illustrated in Figure VII-B. 12. The DRIZO system uses an 80 to 100 mol
wt hydrocarbon solvent to produce an hetero-azeotrope with water which increases the volatility of water in
the solution. Vaporized solvent and water act as the stripping gas in the stripping column and in the rich glycol
still column. After condensation of regenerator overhead vapour phase, separation between solvent and water
is achieved just by decantation. The liquid solvent required is usually absorbed from the natural gas itself (e.g.
BTEX) or can be introduced externally (e.g. heptane). In most cases the regenerating process will even produce
some liquid hydrocarbons6 that will be evacuated from the solvent/water separator as excess solvent with
aromatics.
The presence of aromatics in the DRIZO solvent loop allows benefiting from a lower boiling temperature
(193°C versus 204°C). Azeotropic distillation has been further described beforehand.
DRIZO application
Low water dew pointing, 95%+ recovery of BTEX vapour content, high dehydration efficiency.
6
Liquid hydrocarbons are collected from glycol filters or at the absorber bottom
4
6
8
2
TO
7
PRODUCTION
1
INLET
SCRUBBER
BTEX removal
Glycols used to dehydrate natural gas also absorb some hydrocarbon particularly aromatic components such
as benzene, toluene, ethylbenzene and xylene isomeres (called BTEX). Absorption of aromatics depends on
their solubility in the glycol, concentration in the feed gas and contactor operating conditions (pressure,
temperature, number of trays, glycol circulation rate). Some of the absorbed hydrocarbon is flashed in the
flash drum, the remaining is carried up to the glycol regenerator.
DRIZO™ removes and recovers (BTEX) components absorbed by the glycol which otherwise might be vented or
flared with conventional regeneration units.
BTEX emissions from the regenerator vent or loss to flare are reduced by 95 % or optionally to zero, with no
vent vapour compression.
7
Reid L. S., 1975 “Coldfinger, and Exhauster for Removing Trace Quantities of Water from Glycol Solutions used for Gas
Dehydration” Proc. Gas Conditionning Conference, University of Oklahoma, Norman, OK
DIRECTION GENERALE EXPLORATION PRODUCTION
This document is the property of Total. It must not be stored, reproduced or disclosed to others without written authorisation from the Company.
Exploration & Production – DGEP/DEV/ED/ECP
PRODEM Date : 12/2011
Section N° VII-B
GAS DEHYDRATION
Physical absorption process Page 26
Vapour pressure is equilibrated between Surge Drum and reboiler via a dedicated balance line. Part of the
vapour in the Surge Drum, is condensed with the cooling coil. A collecting tray placed underneath the coil
recovers HC condensate and water which are routed back to reboiler.
Condensation of water from the vapour phase shifts the water vapour – liquid equilibrium in the surge drum,
leading to leaner glycol in the surge drum than in the reboiler.
VAPOR
TC STILL COLUMN
COLDFINGER PROCESS P-32
REFLUX CONDENSER
TIG
CONTACTOR
BALANCE LINE
LEAN TIG / DRY GAS
HEAT EXCHANGER
DRY GAS
LC
RICH TIG
LEAN TIG
WET GAS LC
Flashed Gas
STAND PIPE
LC
LC
P-2
RICH TIG
TIG PREHEATER
RICH/LEAN TIG
LEAN TIG Cartridge
HEAT EXCHANGER
CHARCOAL Filter
GAS Filter
Dry Gas
Water Vapor
STILL COLUMN
GLYCOL CONTACTOR
Water vapor
VACUUM DRUM
and Glycol
Wet Gas
Throttlng valve
RICH GLYCOL
Regeneration under vacuum however suffers from undetected air leakage. Presence of oxygen in the glycol
system leads to glycol oxydation and to corrosion issue.
PROGLY efficiency
Glycol purity : 99,7 wt%
Water Dew point : -30°C
TO FLARE CONDENSED
HYDROCARBON
CONDENSER (AROMATICS)
DRY GAS VACUUM PUMP
GLYCOL COOLER
WATER
SURGE TANK STILL/VACUUM
COLUMN
GLYCOL
CONTACTOR
FUEL GAS
FLASH
WATER REFLUX
DRUM
THERMAL REGENERATOR
DRY GLYCOL
Source: Prosernat
Figure VII-B. 15 – Progly process scheme
There is one reference of the PROGLY process within TOTAL, at Lussagnet: TEG Regeneration unit of 10 m3/h.
1.3.2.7. DRIGAS
SIIRTEC NIGI S.p.A has developed and patented DRIGAS process which can regenerate TEG up to 99.985%wt
without wasting stripping gas while minimizing environmental pollution.
In DRIGAS-1, a blower recycles the non condensable gas from top of still column as stripping gas which, in a
standard process would be flared out or burned.
The more volatile dissolved gas in rich TEG is removed in the flash drum (S-1) and burned as fuel gas in the
reboiler firebox. Remaining heavier gas from rich glycol is released in the reboiler and will mix with the
stripping gas. As stripping gas system is a closed loop without consumption, a bleed is required to avoid gas
build up and maintain regeneration system pressure. Bleed is taken at blower outlet where pressure is higher.
This purge gas may be used to complement fuel gas to burner but it does require boosting with a small ejector
using flash drum gas as motive fluid. DRIGAS-1 process is very sensitive to condenser temperature as seen in
figure below.
Reference: There is one industrial reference at Pineto Gas Terminal in Italy operated by ENI. The main process
characteristics of this unit are indicated below:
DEG flow ~= 7 m3/hr
Stripping gas ratio ~= 150 m3 stripping gas/ m3 Glycol
Regeneration TEG purity ~= 99,8%
Two other configurations are proposed (DRIGAS-2 and DRIGAS-3) depending on the TEG purity required. They
require a small absorber to dehydrate the stripping gas.
In DRIGAS-2, a small packed atmospheric absorber (C-4) is used with recirculation of rich TEG for
dehydration. SIIRTEC NIGI claims that 99.96%wt purity can be reached with DRIGAS-2.
In DRIGAS-3, a second packing (C-5) is installed in the previous absorber where a slip stream of
regenerated TEG is circulated after cooling in a rich / lean TEG cross-exchanger (E-6). SIIRTEC NIGI claims
that 99.985%wt purity can be reached with DRIGAS-3.
Figure VII-B. 21 – Process flow diagram of DRIGAS-2 Figure VII-B. 22 – Process flow diagram of DRIGAS-3
1.3.2.8. ECOTEG
The ECOTEG process is very similar to the Drigas process, and focuses on avoiding BTEX emission to the
atmosphere. It also aims to limiting BTEX absorption by TEG. ECOTEG takes advantage of the fact that BTEX
absorption is inversely proportional to the BTEX concentration of the lean glycol. Thus, the BTEX removed from
the recycled stripping gas are sent back to the lean glycol in the absorber, in order to saturate the lean glycol
in BTEX. Therefore, most BTEX remain in the treated gas.
1.3.2.9. CLEANOL+
The CLEANOL + process also recycles the stripping gas which is composed mainly of aromatics (BTEX) trapped
in the glycol contactor and collected from the overhead vapor from the reboiler/still column. The BTEX and
some water are condensed from the vapor. The liquid BTEX and water are separated, and the required flow of
dry BTEX is vaporized and injected into the stripping column. Any excess BTEX is recovered as condensate
avoiding any discharge to the atmosphere. The condensed water contaminated with BTEX is vaporized and
recycled for recovery of BTEX, and the clean water is discharged for disposal.
CLEANOL+ efficiency
Glycol purity : 99,96 wt%
Water Dew point depression : -50°C
The dehydration process can be selected based on the information summarized on Table VII-B. 5.
Figure VII-B. 24 provides guidance for the selection of the appropriate dehydration method based on the
respective applicability ranges with regard to the contactor temperature, the expected water dew point and
the TEG concentration.
8 th
Further detailed in section 2.2.2. Determining the minimum leaned TEG concentration and flowrate, 5 Step.
This chapter gives a method to estimate the influence of the main parameters (inlet gas temperature, water
dew point required, ...) on the performance of a glycol dehydration process (lean TEG concentration and
flowrate, stripping gas flowrate, reboiler duty, ...). It also illustrates how to check the characteristics of a
vendor's proposal or operations of an existing unit (contactor and still column diameter, ...).
Even small quantities of these materials can result in excessive glycol losses due to foaming, reduced efficiency
and increased maintenance.
For this reason complete scrubbing of the incoming wet gas is absolutely essential for satisfactory
performance. The inlet gas separator scrubber shall have a liquid removal efficiency of at least of 98%. Any
free water that enters the contactor increases the reboiler duty.
To prevent condensate forming in the gas filter/separator-contactor line due to pressure drop and ambient
temperature effect, the scrubbing system must be located close to the absorber, and be line insulated.
Integration of an inlet separator in the bottom part of the contactor instead of a scrubbing system so as to
save place must be prohibited. Separators efficiency cannot be guaranteed.
Note: For any dehydration process, it is important to reduce the amount of liquid droplets and solid particles
as well as to avoid flow maldistribution for any type of scrubber. The following good engineering practice
should apply for any dehydration process.
The inlet scrubber should match the following criteria, so as to obtain a good gas-liquid separation, while
avoiding gas and liquids carry-over:
2.1.1.2. Absorber
As shown in Figure VII-B. 25 below, the absorber (or contactor or dehydration column) consists of a mass
transfer or drying section in the middle, a mist extractor at the top and a liquid surge volume at the bottom.
Drying section
In the past, contactors were usually equipped with bubble cap trays while random packing was used for very
small diameter columns (12 inches or less) although mass transfer efficiency was lower, due to low cost and
easy installation. Sieve or valve trays can be considered only if gas flow is relatively constant.
Nowadays, structured packing is the preferred option instead of bubble cap trays, due to lower height
requirement and higher allowable gas velocity. Moreover, for offshore applications, structured packing
performance is less sensitive to floater motion (FPSO, FPU, barges).
Structured packing
Structured packing was developed as an alternative to random packing to allow improved control of
mass transfer by the use of a fixed orientation of transfer surfaces. Structured packing is the
preferred option for dehydration (high gas/liquid ratio), where as random packing is more frequently
selected for amine units (lower gas/liquid ratio).
Structured packing has been tested and shown to be superior to trayed columns, providing roughly
twice the capacity and up to 50 % greater efficiency. The gas capacity of structured packing is about
150% to 190% greater than that of bubble cap trays. Indeed, the combination of high gas capacity
and reduced height equivalent theoretical plates (HETP) in comparison with trayed contactors makes
the application of structured packing desirable for new contactor designs and existing trayed
contactor capacity upgrades.
Structured packing is essentially a series of closely spaced corrugated sheet metal plates stacked
vertically on edge with corrugations at a 45° angle from horizontal. Flow passages direct the gas and
liquid countercurrent to each other. Packing sections are usually less than 12 in. high and are stacked
so the corrugations run at 90° orientation from the layers above and below.
The packing is generally of the same geometry but each vendor has a different type of surface
treatment intended to enhance vapour-liquid contact.
At low gas rates the packing efficiency decreases because of a gas bypassing effect. 1 to 5 wt %
bypass has been observed, significantly reducing structured-packing efficiency. The bypassing is
caused by low liquid hold-up which reduces the contact surface available between liquid and gas.
However in dehydration service, the required number of theoretical contact stages tends to decrease
with increasing glycol flow rate. This phenomenon offsets efficiency loss and provides liberal
turndown.
Good distribution of gas in glycol should be insured through the packing in order to avoid
channelling. Thus:
o An inlet diverter and a tray shall be provided at the gas inlet section for gas distribution
o A glycol distributor tray at the top of the drying section shall be installed for good glycol
distribution. A density of 80 drip points per square meter is a common standard. Higher drip
points density will increase the contactor efficiency for small packing height but since
distributor orifices size is decreased, they will be sensitive to fouling.
Height of packing equivalent to a theoretical plate (HETP) varies with TEG circulation rate, gas rate,
and gas density. Usually, 1.5 meters height of packing for one theoretical plate is, with a minimum
height of 3 meters recommended by the GS ECP 101.
However, when the gas density exceeds about 100 kg/m3 (generally at very high pressures), the
above conversion may not provide sufficient packing height. When the contactor temperature is less
than about 16°C, the increased viscosity of the TEG can reduce mass transfer efficiency, and
temperatures in this range should be avoided. Such criteria will require supplier/manufacturer
expertise10.
A second generation of structured packing (like SULZER Mellapak Plus) is available on the market
since the end of 90s. The difference between the first and the second generations is the modification
of the corrugation angle at the lower and upper end of each packing element: bottom and top ends
corrugated sheets are bent smoothly to be vertical. Therefore, there is no abrupt change of gas
direction and leads to lower the local pressure drop and shorten the transition zone. Flooding at the
interface of packing elements is also reduced. On the overall performance, experimental pilot tests
report that these modified packings achieve capacity increase but lead to a certain deterioration of
mass transfer efficiency.
Figure VII-B. 26 – Mellapack (1st generation – Sulzer) Figure VII-B. 27 – Mellapack Plus (2nd generation –
Sulzer)
10
The diameter of the column and the height of structured packing are calculated and guaranteed by the Supplier/ Manufacturer of
structured packing.
If structured packing is selected for a new design, provision should be incorporated for the future
debottlenecking by retrofitting swirl tube trays. This requires that the column support rings should be
designed for swirl deck trays, which are heavier.
The gas handling capacity of swirltube trays is about 160% of structured packing. Swirl tube trays
require special provision for turndown; each tray has a glycol level of 250-300 mm on it during
normal operation. If the gas flow drops below the threshold the glycol inventory will run to the
bottom of the contactor. The control system of the contactor must be able to cope with this glycol
surge, for example by allocating a volume for it between NLL and LAH.
Source: [10]
Liquid distributor
A liquid distributor is required when packing or swirltube trays are used. Packing is very sensitive to liquid
maldistribution. Correct design and installation of liquid distributor are essential for the performance of a
packing column. It is then recommended that packing and liquid distributor be supplied by the same vendor.
L V
Vc 0.048 Eqn 6
V
Superficial velocity usually adopted to size the equipment is
- 1.7 times the critical velocity for the mist eliminator meshpad (Kvalue =1.7);
- 3.3 times the critical velocity for the vane pack (Kvalue = 3.3).
The distance between the top of the structured packing and the mist eliminator must be at least 1 200 mm.
(See the GS ECP 101 for arrangements of mist eliminator and vane pack at the top of the contactor).
If a natural gas liquid extraction unit is installed downstream of the dehydration unit, it is recommended to
install a three phase separator as a cold separator. It would enable the separation of liquid glycol carried by
the gas, or resulting from the condensation of vapour glycol contained in the gas (condensation occurring in
the NGL extraction unit).
Swirltube deck (Shell patent): the deck is composed of swirltubes of 0.11m ID. Swirltubes are axial
cyclones with a swirler at the inlet and longitudinal slits in the tube wall. Separation is done by impact of
droplets on the vanes of the swirler and by centrifugal forces on the tube wall. Liquid films from the slits
are drained to a liquid collection chamber to avoid re-entrainment. As some gas is also bled through the
slits with liquid droplets, secondary outlets at the top (see Figure VII-B. 33 below) are provided in the
liquid collection chamber for gas evacuation. This bleeded gas goes eventually through a second
demister pad.
Swirldeck are suitable when swirl tube trays are used as mass transfer internals for high gas velocity. A
wire mesh pre-conditionner is recommended upstream the deck. Swirltube deck is suitable for high
pressure contactor (above 70 barabs).
Different configurations for the installation of swirl tube deck with pre-conditionning exist, as shown on Figure
VII-B. 34 for separators.
Scaling-up of a separator equipped with a swirldeck is done simply by increasing the number of swirltubes
proportionally to the gas flow in the separator.
Cyclone mist eliminator (CDS patent): The principle is similar to Shell swirltube deck
Chimney Tray
A chimney tray is required immediately below the contacting section for all configurations where condensate
skimming is incorporated. The function of a chimney tray is to enable the rich glycol to go down and to be sent
to the skimmer.
The minimum surge volume required in the bottom of the absorber is fixed by GS ECP 101: it corresponds to a
normal volume flow rate of glycol during ten minutes, and enables the height between the low liquid alarm
level (LAL) and the normal liquid level (NLL) to be determined.
A skimming device must be installed in the bottom of the absorber to remove possible liquid hydrocarbons
from any of the following sources:
carry over from the upstream equipment (by pass of the inlet gas filter/separator)
liquid condensing in the glycol contactor, by retrograde condensation of the gas due to the pressure loss
in the absorber
Temperature drop of the gas in the column
To prevent the last event particularly during cold season, especially in hot countries, or in countries with heavy
rain, it is recommended to insulate the dehydration section.
Absorber specificities
Besides the above characteristics, the glycol absorber (or contactor) shall also match the following design
constraints:
Gas inlet distributor
o A Schoepentoeter type inlet distributor (or similar) is required
This induces a more efficient repartition of gas/liquid (avoiding liquid jets) in the absorber, and is
required for an efficient operation of the absorber’s internals. Chimneys are not recommended.
Strutured packing (Figure VII-B. 36)
o A Sulzer Mellapak 250 Plus or 350 Plus, or the equivalent equipment provided by another
supplier, shall be selected
o Sharps edges shall be avoided
o The maximum bed height shall be limited to 5 meters (an additional bed can be added if
necessary)
Internals (Refer to chapter XVII. Separators for further details regarding the internals)
o Two different internals shall be selected among: Mist extractor, cyclone, coalescer.
Vane packs are not recommended. The two internals are complementary, the first one improving the
efficiency of the second one. The internals aim at preventing glycol carry-over.
Liquid distributor
o A very high efficiency distributor is required
INTALOX random packing INTALOX structured packing Mellapak Plus strutured packing
TEG absorbs 7.5 10-³ Sm³ of natural gas per litre at 71 bar abs and 35°C. Most of this gas appears when the
glycol flashes at 6 bar abs. The amount of flash gas is less than 15 10-³ Sm³ per litre of TEG. However, the
majority of aromatic compounds and heavier hydrocarbons remain in solution in rich glycol.
Heavy hydrocarbons form stable emulsions and foams. These are broken at 65°C and a retention time of
20 minutes.
To remove the heavy hydrocarbons, the rich glycol must be pre-heated before flashing. Heating reduces the
viscosity and accelerates glycol-H.C. liquid separation. However, increased temperatures increase the solubility
of liquid hydrocarbons in the glycol (glycol should not be heated over 90°C).
Before flashing, rich glycol may be heated in the integrated condenser of the still column, or otherwise in a rich
glycol/lean glycol plate fin heat exchanger. In the case where condenser is external, heating is carried out in a
rich glycol/lean glycol plate fin heat exchanger.
The pressure in the flash separator must be sufficient to allow the exit glycol stream to flow through all
downstream equipment, i.e. the heat exchangers and the filters.
Because better hydrocarbon-glycol separation is obtained with a horizontal flash drum, the horizontal flash
drum is usually a horizontal three-phase separator with a 30 minutes liquid retention time operating at 3 to 6
bar abs.
When feed gas to absorber contains high concentration of CO2, a simple flash tank may not be adequate for
removing dissolved CO2 due to its high solubility in glycols. It is wise to remove dissolved CO2 prior entering
regeneration still column in order to minimize corrosion issue, reduce reboiler heat load and vapour traffic in
the still. An intermediate pressure stripper (with stripping gas) may be required prior entering regeneration
column.
2.1.1.4. Filters
Filtration includes the removal of solid particles and dissolved impurities. In especially dirty glycol systems,
filters are often bypassed to avoid frequent filter change-out. This approach will ultimately lead to
operational problems downstream.
If solid particle filter plugging is excessive, a larger filter size should be trialled and the source of the problem
investigated (e.g. poor inlet separation, degradation, corrosion products, etc...).
Note that judging the filtration effectiveness solely on the basis of glycol colour is difficult, even well filtered
glycol is black.
Paper and fiberglass elements have generally been proven unsatisfactory. A cloth fabric element that is
capable of reducing solids to about 100 ppm wt is preferred.
Filter size in a properly operated glycol system should be 5-10 µm. A larger size of 25-50 µm may be required
during start-up and in dirty services.
Ideally two identical cartridge filters, designed to handle 125 vol % of the total flow of rich glycol, are installed
in parallel with no by-pass line: one in operation, one in stand-by. Minimum filtration area is 0.2 m2 per m3 of
TEG.
Coal-based activated carbon should be used because wood-based charcoal tends to break up in use. This
carbon can be placed in a metal canister or fill a vessel. In either case, good screens are needed to prevent
carbon loss into the system. Said carbon particles, much like iron sulfide, tend to promote a stable foam.
The use of a carbon purifier downstream of the solid particle filter is recommended. This will produce
essentially water-white glycol, a colour that has proven to be desirable. Indeed, it tends to increase
dehydration efficiency and minimise foaming, a major source of glycol loss.
A carbon filter vessel handling at minimum 10 -15 vol % of the rich glycol flow rate is used downstream of solid
particle filters (supplementary rich glycol flow rate flows through the by-pass). The length to diameter ratio
should be at least five. Granular, 8 to 30 mesh, 480 kg/m³ (30 lb/cuft), coal-based carbon is recommended. The
flowrate should be 4.9 to 7 m³/(h.m²), (2 to 3 gpm/ft²), of bed area. A retention time of 15 to 20 minutes is
recommended to obtain the full carbon capacity. The carbon should be replaced when it no longer removes
colour from the glycol. New carbon should reduce foaming and hydrocarbon content. The carbon should be
replaced on a regular planned maintenance schedule.
Still column
The still column is insulated and fitted with two beds of one meter high minimum of 316 stainless steel
random packing (PALL rings or equivalent) per bed.
Ceramic saddles are prohibited.
Trays are sometimes used in very large units.
Reflux should be controlled by installing a condenser in the top of the still column. Wet glycol flows through
the condenser and controls the temperature at the top of the still: 100°C. Glycol losses in the water vapour
leaving the still are minimal with a reflux equal to 30 % of effluent water vapour.
The still column condenser may be an integrated condenser for low capacity units, or an external condenser
for larger capacity units. The condenser types are described further on this section (Refer to Heat exchangers
description).
Advantage of external condenser use, is the limitation of water condensation in low pressure flaring system.
Reboiler
The reboiler provides the heat necessary to boil the water out of the glycol.
Direct-fired heaters are often used, but they constitute an open flame hazard. In some locations, such as
offshore platforms, indirect heating with oil, steam or electrical resistance is required by fire code and prudent
practice.
TEG does not undergo significant thermal decomposition if the bulk glycol temperature is kept at maximum
204°C, and the maximum outside fire-tube skin temperature does not exceed 221°C.
To maintain proper skin temperature, prevent "hot spots" and obtain satisfactory fire-tube life, the reboiler
must have sufficient area. The following are recommended:
2
Maximum heat flux across fire-tube wall : 23 kW/m ,
2
Recommended heat flux for maximum life : 20 kW/m ,
2
Burner capacity : 30 kW/m .
Notice that the burner possesses extra capacity to obtain firing flexibility. Experience has shown that extra
heating capacity is desirable (20 % for electrical heaters, 10 % for hot oil or fire tube reboiler).
Extra capacity should be considered to take into account the vaporization of aromatics (BTEX) absorbed by
TEG. The same remark applies to the regeneration system (still column, reflux system, ...).
The typical heat balance will indicate a reboiler heat load of 390-450 kJ/litre of TEG circulated.
Glycol level in the reboiler is controlled by a weir, or the height of the downcomer. In all cases, the glycol level
should be 15 cm over the top heat source (i.e. top tube).
Reboiler selection between electrical or any other heater is basically based on the following aspects:
1. Required duty for the reboiler: Some vendors (like EXHEAT) talk about 1000 kW as maximum power
duty for a single shield, it may be possible to get more power by combination of several enclosures, but
then the lay out required will be much bigger.
2. Heating medium availability: When waste heat recovery is not practical, electrical heating
implementation is often a very attractive option.
3. Available lay out versus required lay out.
Others characteristics such as temperature control efficiency, response time, cost effectiveness, compactness
(…), have to be taken into account in the selection of the heating device.
More information on heaters can be found in section XIX-E.
Note: The reboiler shall match the following criteria (good engineering practice):
3*50% duty electrical heaters are required, with the availability to run in parallel and to be replaced
online if necessary.
A minimum clearance is required between the liquid level in the reboiler and the bottom of the still
column, so as to avoid flooding within the latter.
During normal operation, the surge tank should be half full. A gas blanket (fuel gas may be used) is
recommended to prevent air contamination. The surge tank should have a level indicator, a low level
shutdown and insulation to protect operators and conserve heat.
In some cases condensate is accumulated on the glycol surface in the surge tank. A draining facility for the
accumulated condensate must be provided.
A first solution consists in installing a dry gas/lean glycol heat–exchanger vertically on the dehydration column
(absorber). This heat exchanger is of shell and tube type.
This solution is technically acceptable if there are no limitations on the gas pressure and the gas temperature
since through this heat exchanger dry gas temperature rises and dry gas pressure drops.
A drawback of this approach is that the temperature of lean glycol leaving the heat exchanger is gas flow
dependent. It is not possible to accurately control this temperature.
An alternative consists in installing a forced-draft air heat exchanger (i.e. an aircooler) or a water-cooler of
shell and tube type11.
An automatic control system of lean glycol temperature is installed with an air or water-cooled heat exchanger
to take into account temperature value of the gas entering the absorber.
11
Because of the high pressure of the regeneration, the use a plate exchanger is not recommended.
Temperature control of the stream leaving the top of the still column is achieved with a manual by-pass
valve on the rich glycol stream.
2nd solution: external condenser with reflux drum and reflux pumps
This solution is used for units of large capacity or if condensation of water is required. The heat
exchanger may be an aircooler or a water cooler. The reflux drum is usually a horizontal three phase
separator. The gas is sent to a LP flare.
Recovered liquid hydrocarbon should be pumped or sent by gravity to the oily water treatment
production system
Part of the condensed oily water (30 % of water flow) is pumped through a flow control valve to the still
column to assure the reflux. The remaining oily water passes through a level control valve to the oily
water treatment.
Two pumps must be installed: one running, one in stand-by.
In this option, rich glycol leaving absorber must be heated by lean glycol in a plate fin exchanger, before
entering the still column.
An approach of 25-40°C at the hot end is desirable in the rich/lean-glycol heat exchanger.
This exchanger has a large temperature cross ; that means the temperature of the exit lean glycol is much
lower than that of the exit rich glycol. This type of service requires true counter-current flow. Two exchangers
in series are often used in larger units to control the temperature at which the rich glycol enters the flash
drum.
These heat exchangers are welded stainless steel plate fin heat exchangers.
Plate and gasket heat exchangers are prohibited due to leaks during transitory periods.
An over design of 25 % extra heat transfer area is adopted. These heat exchangers and the heat exchanger
used to heat rich glycol upstream flash drum when an external condenser is installed may be located between
the stripping column and the surge drum, or between the surge drum and the injection pumps.
2.1.1.8. Pumps
Reciprocating pumps are generally used.
A full-flow standby pump minimizes downtime due to pump failure.
An in-line strainer should be included on the pump suction.
Good flow control is desirable because excessive glycol circulation increases the reboiler duty.
Flow control is done either by varying the pump speed or with a bypass around the pump. The bypass valve
around the pump should discharge to the surge tank. Full flow around the pump cools the pump packing and
reduce leaks.
The installation of a stripping column must be recommended even if the purity of the lean glycol does not
require it (refer to GS ECP 101). At minimum, provision for direct stripping gas injection into the reboiler must
be provided (applicable for small units only).
This method is based on the principle of reducing the effective partial pressure of H2O in the vapor section of
the glycol reboiler, and hence obtaining a higher glycol concentration at the same temperature. The process is
illustrated on Figure VII-B. 37.
Stripping gas must have at least the minimum quality characteristics required for a fuel gas in order to prevent
glycol pollution by heavy hydrocarbons.
In addition to the usual equipments, the stripping gas process uses specific components such as:
A stripping gas scrubber to remove condensed liquid droplet that can lead to foaming (free water, oils,
entrained brine…). A recommended scrubbing system is composed of:
o A knock-out drum to separate the liquid slugs carried by the stripping gas.
o A gas filter/separator (mist extractor with coalescing cartridge) to remove the liquid droplets and
dust particles carried over from the knock-out drum.
For further information, refer to the description given in GS ECP 101 [1].
A downcomer between the reboiler and the surge tank packed with 1 bed of 1.2 meter high minimum
of 316 Stainless Steel random Pall rings or equivalent.
An heating coil inserted in the reboiler (reboiler target temperature: 204°C)
A sparging pipe installed at the bottom of the reboiler: Stripping gas is admitted to the reboiler through
a sparging pipe extending longitudinally of the tank from near the back end of the fire tube. Sparging
pipe may also be installed at the bottom of the stripper.
A dedicated stripper: Table VII-B. 7 gives some TEG regeneration efficiency in function of the stripping
rate at 760 mm Hg pressure and a reboiler temperature of 204°C.
Stripping rate Wt% TEG in rich glycol Wt% TEG in lean glycol
Scf/U.S. gal m3/liter of glycol
6 0,05 96,84 98,9
4 0,03 96,84 99,15
2 0,02 96,84 99,25
Source [2] – Gas processing - P357
Table VII-B. 7 – TEG regeneration efficiency in function of stripping rate (at 760 mm Hg and 204°C)
Source: Prosernat
In addition to the usual equipments, the DRIZO process uses specific components such as:
solvent preheater,
solvent/water separator,
solvent /water condenser,
solvent pumps,
Water coalesce in solvent loop,
Solvent dehydrator
The solvent/water condenser is designed so as to lessen light ends degassing, which would induce BTEX carry-
over.
An oily water treatment is required because of the glycol and dissolved BTEX present in the water outlet.
A coalescer or a molecular sieve can be added in between the solvent pump and the lean glycol/solvent heat
exchanger, so as to remove more water from the solvent, as shown on Figure VII-B. 46. It is feasible to then
reach 100 wt ppm water content in solvent.
Advantages
Azeotropic distillation of the solvent and glycol
Low water dewpoint Technology enhancements
Very high water removal efficiency
Contamination of the condensates tolerance better with DRIZO than
Condensate contamination
other dehydration processes
High glycol concentration obtained in DRIZO
Low glycol rate
Low energy
Decrease of total energy consumption (no gas flaring)
Comment ECP: including solvent heater consumption?
No stripping gas
Higher recovery of BTEX
“Zero” vapour emissions Avoids disposal of vent vapour from the solvent-water separator to
atmosphere but a dedicated water treatment is required for oily
water (steam stripping or membrane treatment)
High glycol purity
Low height of contactor
Reduced height of contactor unit (less stages required)
Temperature of the reboiler can be maintained at around 193°C (TEG
degradation temperature: 207°C)
Minimum degradation of TEG
Minimum TEG degradation
No carbon bed required; carbon beds are anyway not recommended
in case of high BTEX presence in lean or rich glycol because of the
preferential adsorption of aromatics.
Table VII-B. 8 – DRIZO advantages
Table VII-B. 9 lists the required data for calculation procedure, and the main resulting output data.
The procedure below is straightforward and can be performed manually or with the dedicated Excel
calculation tool. In all but a few exceptional applications, it will give results as reliable as more complex
(appearing) methods.
The calculation procedure may be summarized as follows:
12
Bukacek correlation defines the water content w of a gas at saturation as a function of gas maximum temperature T and minimum
pressure P. Bukacek is applicable for temperature from -40°C to 130°C, and for pressures from 1 bar abs to around 690 bar abs.
A(T)
w = B(T )
P
The A and B factors are temperature functions, depending on temperature value:
A(T)
73.7433 * T 0.30673912 * T 2
-40°C < T <40°C 4926.5573 * exp( )
1000
62.00686*T 0.13096345*T 2
40°C< T <90°C 6156,9611* exp ( )
1000
62.00686*T 0.13096345*T 2
90°C< T <130°C 6156,9611* exp ( )
1000
B(T)
53.5703 * 87 * T 0.19866041* T 2
-40°C < T <40°C 44.8739 * exp( )
1000
55.042799 * T 0.16553793 * T 2
40°C< T <90°C 40.5058 * exp( )
1000
23.2637894 * T
90°C< T <130°C 70.0737 * exp( )
1000
13
Correction factors
Source: [5]
Figure VII-B. 39 – Equilibrium water vapour content of sweet natural gas (Wichert Chart) 13
13
The resulting water dew point shall be adjusted using correction factors related to gas density and salinity. Once the water vapour
content is estimated from the graph, multiply it by the correcting factors.
(Wi - Wo ) Q
Wr = * 1.1 Eqn 7
24
It includes 10% overdesign (1.1 factor). Indeed to design glycol dehydration unit, the GS ECP 101
recommends to adopt a safety margin of 10 % to take into account gas flow fluctuations.
Source: [5]
Figure VII-B. 40 – Equilibrium H2O Dewpoint vs. Temperature at Various TEG Concentrations 14
(10bara < Contactor Pressure <140bara)
As illustrated by the dashed line on Figure VII-B. 40, 98.5 wt % must be considered as a minimum value
for lean glycol concentration C 14. Furthermore, it should not exceed:
98.8 % wt in case of regeneration without stripping gas15;
99.5 % wt in case of regeneration with stripping gas but without stripping column;
99.9 % wt in case of regeneration with stripping gas injected in a stripping column.
Note that the minimum lean TEG concentration may not be the one used. A higher concentration may
be specified to minimize the circulation rate and optimize cost.
14
The dashed line in Figure VII-B. 40 at about 98.5 wt % represents the concentration of lean TEG that can be produced routinely in a
regenerator operating at standard atmospheric pressure and 204°C. If the concentration obtained with Figure VII-B. 40 is less than
98.5 wt %, use 98.5 wt % for the calculation.
15
Concentrations of 98.7-98.8 wt % are common without stripping gas. Concentrations of 99.9 wt % have been reported but it
corresponded to a case where incoming hydrocarbons provided natural stripping and/or the pressure was lower than standard
atmospheric. Note that since the capital cost of ordinary gas stripping accessories is trivial, they always should be included.
- the amount of lean TEG circulation rate per unit of removed water r = 27
- lean TEG concentration C = Cmin
A
18 r
1 Wo Wi r 1 132.2 C 15 020 * 1 Wo Wi Eqn 8
M
With glycol activity coefficient given in Figure VII-B. 41 below, versus gas inlet temperature and
lean TEG concentration.
Source: [2]
Step 6.b: Calculate the lean glycol concentration required with the number of theoretical trays adopted.
In a first approach:
n = 1.5 for 6 bubbles caps trays,
n = 2 for 3 meters of structured packing
100 R
C Eqn 9
1 R
With:
150.2
R 1 Eqn 10
18 1 Wo Wi
1 n 1
A A A n 1 1
Figure VII-B. 42, adapt the values of C, r, n, until the value of C found in step 6.b is equal to the value
introduced in Step 6.a
From
Step 5
j0
Aj
rj
1 132.2 * Cj 15 020* 1 Wo Wi
j
j j 1
150.2 j
Rj 1
18 1 Wo Wi
1 n 1
A A A 1
n 1
No Yes To
Ccalc, j C j
Step 7
Q
m MAWi * * Eqn 12
18 * 24
mC
c=
Q Eqn 13
m + (W i - Wo )
24
With the lean TEG density d given in Figure VII-B. 43 and plotted against various concentrations of
several aqueous TEG solution, the TEG volumetric rate LVOL is given by the following relation:
m
LVOL = Eqn 14
d
Source: [5]
Figure VII-B. 43 – Densities of aqueous TEG solutions
Source: [5]
Figure VII-B. 44 – Effect of Stripping Gas on TEG Concentration
Note that a reboiler heat load of 450 kJ/litre of TEG of TEG is often adopted by providers.
The absorber diameter D with bubble caps trays can be obtained from manufacturers' charts or
from equation as follows for 24 inch tray spacing :
M G x QS
DBubblecap = 37.79 Eqn 15
G 1/4 ( L - G )1 / 4
Note: This equation is obtained assuming that gas velocity between two bubble cap trays is equal
to critical velocity16 given by:
L V
48 Eqn 16
V
An overdesign of 10 % on the maximum operating gas flow rate shall be used to take account of
gas flow fluctuations, as recommended by the GS ECP 101.
The absorber diameter D with structured packing can be obtained from equation as follows :
D 0,77 * DBubblecap Eqn 17
16
See PRODEM Chapter XVII – Gas/Liquid separators for further information.
2.2.3. Example
j - 0 1 2 3
Cj (wt %) Cmin = 99.65 % 99,67 99,69 99.70
γj - γ (Cmin )= 0.617 0.617 0,616 0,616
rj - 27.00 27.00 27.00 27.00
Aj
rj
1 132.2 Cj 15 020* 1 Wo Wi - 5.18 5.17 5.17 5.17
j
150.2 j
Rj 1
18 1 Wo Wi - 757.44 444.71 326.87 327.56
1 nj1
nj1
Aj Aj Aj 1
The following economical indications should be kept in mind when sizing a TEG dehydration unit:
In a first approach glycol OPEX and CAPEX are functions of the reboiler heat duty design, which is itself a
function of the glycol flow rate (Reboiler installed heat duty is 450 kJ/litre of glycol).
Glycol flow rate depends on the amount of water removed from the gas. Therefore it is most
economical to "dry" a cooled gas at high pressure than a hot gas a low pressure.
Water dew point value of the "dry" gas leaving the absorber is controlled by lean TEG concentration. An
economical way to increase lean TEG concentration is to install a stripping column with 1 bed of 1.2
meter high minimum of packing, between the reboiler and the surge tank. The investment required for a
stripping column is low, but main advantages of this equipment are obvious. It enables to obtain a
higher concentration of lean glycol and a lower consumption of stripping gas to be reached compared to
the solution consisting in injecting stripping gas into the reboiler (See Figure VII-B. 44)
In conclusion from an economical point of view it is more interesting to increase, within certain limits, the
glycol concentration than the glycol flow rate.
The Figure VII-B. 45 below illustrates the results obtained with the previously described procedure. The example
introduced corresponds to the Yadana project.
The following Excel Data Sheet is obtained using the Wichert chart (See Figure VII-B. 39) to determine the
maximum water-content of gases.
Da ta to be fi l l ed-i n
Da ta ba s ed on corres pondi ng cha rts
Da ta a utoma ti ca l l y ca l cul a ted
First of all, macros should be activated when opening Excel, so as to allow their use. The calculation sheet can
be used without macros, but would be less user-friendly.
The calculation sheet can then be used as follows:
1. Two sets of units can be selected in the calculation sheet. According to the choices made, the equations
will be automatically updated, so as to reflect the conversion factors between metric and imperial units.
2. In order to complete the definition of the inputs of the calculation, the user can fill in
the green boxes. Note that some boxes shall be filled-in in an iterative procedure as explained
below.
the orange boxes on the basis of several charts given in the corresponding excel sheet.
3. Based on the first inputs provided by the user such as inlet gas properties and the water dew point
required, the user shall fill in the following orange boxes:
Select a water content calculation option on the top of the tool in order to define the dry gas
water content and minimum water content, and the maximum water-vapour content of the wet
gas:
- “Wichert Chart” option (Figure VII-B. 39): Water contents will be defined by the user with
the use of the Wicher Chart on the correspond sheet of the calculation tool.
- Bukacek correlation option: Water contents will be automatically calculated.
Using the “TEG concentration” graph (Figure VII-B. 43): the minimum / Design lean TEG
concentration Cmin
4. Next, the following boxes shall be filled by the user on the iterative procedure described in 6th step:
green boxes: the lean concentration C, the lean TEG/removed water ratio r, and the number of
theoretical plates in the absorber
orange boxes: the activity coefficient corresponding to C on the basis of the “Activity” graph
(Figure VII-B. 41).
5. Then, once the lean TEG concentration is calculated, the following data shall be provided for the next
steps:
7th step: lean TEG density shall be stipulated, using the “TEG density” chart (Figure VII-B. 43) to
calculate the minimum rich TEG concentration
8th step: the number of theoretical plates of the stripping column and the stripping gas flowrate
(based on the “Stripping gas flowrate” chart in Figure VII-B. 44) shall be filled-in
9th step: the reboiler type selected shall be specified in order to calculate its duty.
6. Finally, the absorber diameter will require such data as the tray type, the dry gas density and the dry gas
molar mass.
The results – intermediate and final – can be found in the blue boxes (light blue for intermediate, dark blue for
final results). These cells cannot be modified.
At this point, the design calculation is finished. However, the user has the ability to check whether this design
is correct. The “Input and output data verification” button checks whether the values provided as inputs to the
calculation and the results obtained match the minimum and maximum values criteria defined along this
chapter. For invalid data, a message will appear explaining the reason why it is incorrect and how it should be
modified. The corresponding cell will become red. The user is informed when all inputs and outputs are valid.
A final sheet is provided, corresponding to the example previously described. The “Contact” button indicates
who to contact within EP/DEV/ED/ECP for further assistance on this calculation sheet.
Table VII-B. 11 below lists the main process design parameters of TEG dehydration designs performed by ECP.
The Girassol dehydration PFD is presented in Appendix 5.
17
The dew point was only specified for the gas after compression.
18
The water dew point was defined for dehydration pressure and for gas after compression, in a LNG train.
19
The design flowrate was initially 340 m3/h, but the test run figured out that a rate of 110 Sm3/h was sufficient.
20
Design data, different from installed performance. Refer to feedback documents for operational data.
3. OPERATIONAL DATA
The pressure and temperature of the inlet gas control the water content and condition the water amount to
be removed.
High pressures and low temperatures are preferred for operating conditions because they reduce water
content, equipment size and fabrication costs.
Glycol losses can be defined as mechanical carry over from the contactor plus vaporization from the contactor
and regenerator and spillage.
Normal process glycol losses is
10 litres/106 Sm3 (0.07 US GAL/106 Scf) for the contactor
4.1 litres/106 Sm3 (0.03 US GAL/106 Scf) for the regeneration skid
Total = 14.1 litres/106 Sm3
However TEG losses may range from 7 litres/106 Sm3 for high pressure, low temperature gases to 40 litres/106
Sm3 for low pressure, high temperature gases.
This excludes leakage at valve and pump packing and spillage to drain system.
Excessive losses result from foaming in the absorber and/or regenerator (Anti-foam agents are sometimes
used), carry over at the top of contactor, losses at the top of the still column due to too low reflux, leakage at
valves and pumps gaskets and spillage to drain system.
For ordinary pipeline water dewpoint control, the glycol circulation rate usually will be 15 to 35 litres per kg
water absorbed from gas (mean value is 27.4 litres/kg of absorbed water).
A circulation rate above this range can only be justified economically in special applications due to utility
consumption.
Refer to Figure VII-B. 10, Figure VII-B. 11 and Figure VII-B. 12 for main control loops to be set up for TEG or
DRIZO units.
Gas pre-treatment
- Level control of liquid KO drum
- Pressure drop of filter separators
Absorption
- Pressure control of the absorber on dry gas outlet
- Temperature control of lean glycol entering the absorber
- Rich glycol level control at bottom of contactor
- On line analyzer for water dew point measurement on gas outlet
Note: A manual bypass around the absorber is desirable to aid in the start-up and shutdown of the unit.
Flash drum
- Pressure control via PCV on gas line to flare
- Rich glycol inlet temperature control
- Level controls on glycol and liquid hydrocarbons sides
Regeneration:
- Feed to still column is under level control of glycol in the flash drum
- Pressure control of still column via PCV on vented gas to flare
- Reboiler temperature control
- Stripping gas rate control
- Reflux control if external condenser
- Indirect still column top temperature control via manual bypass on rich glycol for integrated condenser
case or by reflux for external condenser
As previously noted (See paragraph 2.1.1.1), about half of all gas dehydration problems are caused by
inadequate scrubbing of the inlet gas, allowing several contaminants to impair the performance of the TEG
such as:
3. Entrained brine
The salts, dissolved in the glycol, are corrosive to steels, especially stainless, and can deposit on the
fire tubes in the reboiler, causing hot spots and fire-tube burnout.
Even small quantities of these materials can result in excessive glycol losses due to foaming, reduced efficiency
and increased maintenance.
Complete scrubbing of the incoming wet gas is absolutely essential for satisfactory performance.
Consequently, significant attention should be paid to the proper sizing of the inlet scrubber and filter.
3.3.2. Absorption
While TEG can dehydrate natural gas at operating temperatures from 20°C to 70°C, the preferred temperature
range is 20-30°C. Below 15°C, the glycol is too viscous. This reduces tray efficiency, promotes foaming, and
increases glycol losses. Above 30°C, the inlet gas contains much water and the drying ability of the glycol is
reduced.
The inlet glycol temperature should be 5°C - 10°C higher than the inlet gas temperature.
If the glycol enters cooler than gas, the resulting chilling condenses hydrocarbons which, in turn, promote
foaming.
If the glycol enters more than 10°C above the effluent gas temperature, TEG vaporization losses are increased
unnecessarily.
In very cold climates, heat losses through the contactor walls can lead to HC condensation. Insulating and/or
housing the contactor may be justified.
Many operating and corrosion problems are avoided when glycol is kept clean.
Hot spots are observed at night ; if the flame is shut off, they continue to glow bright red.
3.3.3.3. Low pH
Solutions in a glycol unit that is not downstream of an amine unit become acidic and corrosive, especially
when the inlet gas contains H2S or CO2.
The optimum glycol pH is 7.0 - 8.5. A pH above 9 promotes foaming and emulsion formation.
Corrosive acids formed by glycol decomposition or oxidation or dissolved H2S or CO2 can be neutralized by
bases such as triethanol amine. These bases should be added slowly and in small amounts, e.g. 1 kg of
triethanol amine per 2 800 litres of glycol, because excess base can precipitate sludge.
Take care, adjustment of pH must be correctly implemented. The cure can be worse than the disease if it is
overdone.
Special equipment, such as a separate glycol reclaimer or ion-exchange resin bed, is required for removing salt
from TEG. Produced water should be prevented from entering the absorber by use of an upstream filter
separator.
Hydrocarbon contamination should be minimized by scrubbing the inlet gas, keeping the lean glycol 5°C to
10°C warmer than the wet gas, adequately sizing the three-phase flash drum and using activated carbon
purification. Liquid hydrocarbons, if permitted to enter the still column, flow down this one and flash rapidly in
the reboiler. This can blow liquid out of the still column.
Proper filtration of both the rich and lean glycol streams should keep the solids concentration below 0.01 wt%.
3.3.3.7. Foaming
Foaming may be mechanical or chemical. Mechanical foaming is caused by excessively high gas flowrates in
the absorber. Contaminants such as solid particles, salts, corrosion inhibitors and liquid hydrocarbons cause
chemical foaming.
Foaming is best detected by monitoring the pressure drop across the contactor. Erratic readings followed by a
rapid increase of 0.2 to 0.3 bar are symptoms of foaming. Chemical foaming can be detected by bubbling air
through a sample of the glycol for five minutes and observing the resulting foam height and stability.
If the pressure drop across the absorber suddenly increases by 0.3 to 0.6 bar and the chemical foam test is
negative, then suspect mechanical foaming or some other problem.
Foaming should be prevented by good front-end separation of contaminants, proper solution filtration and by
raising the temperature of gas and glycol above the dew point of the condensed hydrocarbons.
Use of defoamers merely treats the symptom; eliminating the cause is far better.
Careful monitoring, elimination of contaminants, carbon filtration, use of a three-phase flash drum and
maintenance of pH between 7 and 8 can extend glycol life to 5-10 years.
Vacuum distillation can recover up to 90 % of the remaining glycol from contaminated glycol. One approach is
to use a portable unit on a 200 to 600 litres per hour sidestream.
Aromatic removal
The affinity for aromatics by TEG has long been recognized. The UDEX process was used for many years in
refineries and chemical plants to extract aromatic hydrocarbons from paraffins with TEG.
In gas dehydration service, TEG will absorb limited quantities of aromatic hydrocarbons (benzene, toluene,
ethylbenzene and xylene) from gas. These components are often abbreviated as BTEX.
Quantifying the absorption levels has become more important in recent years due to increased restrictions
on aromatic emissions from glycol units.
Predicted adsorption levels for BTEX components vary from 5-10 % mol for benzene to 20-30 % mol for
ethylbenzene and xylene. Absorption is favoured at
higher pressures
lower temperatures
higher TEG concentration and circulation rate
The bulk of absorbed aromatics leaves the top of the regenerator with the water vapour. In some cases, these
aromatics can be condensed and recovered ; however the effectiveness of condensation declines rapidly with
increasing stripping gas rates.
If aromatics content in TEG is high, their recovery with a DRIZO gas dehydration process should be considered.
Published data on hydrocarbon absorption are inappropriate for high concentrated glycols. Attention should
be paid to such data in light of the aromatic emission toxic qualities of the regenerator vent gas.
This preferential absorption for aromatics in glycol has a curious property of being either good or bad. A
conventional regeneration unit will exhaust all of the absorbed BTEX components with the water vapour as a
vent. If condensation of the vapours is attempted, BTEX components will condense with the water vapour.
However, if stripping gas is used, then the "sweeping" effect of the imposed stripping gas will inhibit BTEX
condensation and recovery.
Operational experience reflects this observation, confirmed by Hysim simulator runs.
Several other qualitative observations can be made about rich BTEX inlet gas systems.
The lean glycol-retained heavy hydrocarbons would be preferentially absorbed on the carbon bed,
rendering an adsorptive carbon filtration bed ineffective to remove glycol reboiler degradation
products. In that case the carbon bed filter is normally eliminated. It is a waste of funds when BTEX
components are present in the inlet gas.
Condensed water disposal from any regenerator overhead needs attention. A level of BTEX components
from 90 to 900 ppm may be present in the liquid water of a DRIZO unit.
Associated with BTEX components are heavy components (> 204 °C boiling point), which accumulate in
the glycol. These heavy components may be removed by a trap in the solvent line or manually by a
series of drawoffs on the glycol surge drum.
BTEX components may cause unstable operation of the glycol reboiler due to flooding of the reflux/rich
still column.
o The DRIZO system eliminates this operational concern.
Regarding the temperature control scheme of the DRIZO loop (Figure VII-B. 46), an excessive temperature
would induce risks of thermal cracking. Consequently, the temperature downstream the vaporizer must
remain below 160°C, while the temperature downstream the superheater can reach up to 220-240 °C.
The presence of BTEX allows benefiting from the positive azeotrope regarding the vaporization temperature.
Besides, such a temperature control scheme allows the heavy ends to return to the main process treatment,
thereby minimizing the presence of heavy ends in the solvent loop.
VAPORIZER
LIQUID
SEPARATION POT
To production
Two DRIZO units are being operated by TOTAL E&P, respectively on Nkossa (Congo) and K5CC (Netherlands).
The purpose of this paragraph is to present the lessons learnt through the operation of these DRIZO units,
enabling a better design for future installations.
The good performances of both DRIZO units, despite design or operational issues, highlight the robustness of
the DRIZO technology.
General view of Nkossa DRIZO skid Nkossa DRIZO glycol reboiler electrical heaters
Item
Equipment Design inadequacy / Operational issue Suggested design improvement
n°
The inlet gas cooler is underperforming The inlet cooler duty shall be carefully
1 Inlet cooler when seawater is too warm (summer), designed to ensure sufficient duty.
because of an insufficient duty.
Compact design, No compact design allowed,
Vane packs implemented, No vane pack allowed as internal,
Inlet
2 No inlet distributor, Vane type inlet distributor
scrubber
contrary to the design recommendations in (“Schoepentoeter” like)
case of a DRIZO. recommended.
Random packing installed, instead of a Efficient structured packing to be selected.
3 Contactor
structured packing.
Heavy hydrocarbons sent to reboiler Install of 3-phase separator preferably.
where they may form polymers, Ensure a sufficient temperature for
4 Flash drum
because the separator is 2-phase. efficient separation, and select a
A poor separation is observed. minimum 20 minutes retention time.
Recovery The pure glycol is sent to the still column, The pure glycol shall be sent directly to the
5
glycol drum implying quality loss. solvent/water separator.
The flash in the still column induces Sending the pure glycol directly to the
instabilities, which the packing is solvent/water separator would solve
suffering from. the instability problem.
6 Still column An inadequate packing has been SS316 structured packing shall be
installed (random packing originally, selected.
poor material of structured packing
then).
Solvent/water condenser may be blocked 3 times 50% electrical heaters, with the
(fouling inducing an excessive pressure at ability to run simultaneously, shall be
the top of the still column (1.7 bar abs). installed to reduce the occurrence of that
The temperature then seems too high in problem.
7 Reboiler
the reboiler, and reboiler duty is then The fired heaters should be installed as
reduced, where as it is actually shown in (b) rather than the existing
underperforming (2 heaters running, position illustrated on (a) in Figure VII-B.
insufficient duty)). 48.
Stripping The original random packing has been Structured packing required
8
column changed to a structured packing
Table VII-B. 13 – Nkossa DRIZO design drawbacks
(*) Usually a minimum height of liquid (around 0.2 to 0.5m) is required in order to immerge the electrical
bundle for energy efficiency purpose and also to avoid thermal degradation of thin glycol film deposit on non
immerged side of bundle
3
4
7
1
2
Glycol The configuration of electric bundles and logic The change of control logic can solve this
reboiler of power supply was not adequate, leading to issue.
electric hot spots, glycol overheating and
bundles degradation.
Reboiler Corrosion issue has been observed as a result Select an adequate material.
corrosion of high temperature, CO2 and salt presence,
and inadequate material selection.
High glycol Due to formation water carry-over at A regular change-out of glycol solves this
salinity satellite(s), glycol salinity increases up to issue.
solubility level. Salt deposition as a result of
high temperature in HEXs and reboiler has
been observed.
Lean DEG O2 ingress into lean DEG storage tank as a Reverse Vacuum Pressure Valve and a
storage tank result of a wrongly installed Vacuum Pressure proper blanketing can solve this issue.
Valve and no sweeping gas has been
observed, leading to accelerating glycol
degradation.
PT 410
to LP
vent
TIC 440
TT 435
TIC 424
LIC 420
DS 420
Solvent
drum M
M EB 440 Solvant /
EB 420 Solvant water condenser
solvent make-up
1 DS 410
DEG
recovery condenser
to vent
LIC 410
Flash DS 440 LIC 441
Drum Solvent LIC 440
CA 435
Water
DS640A
PDT 435
DS640B
from
FIC 435 4 Water
Condensate
Treatment
DS 400 DEG
FILTER
1 CA 460
stripper
PDT 460
HA 430 Glycol reboiler GX 440
treatment
IF 470 rich
DS300 COALESCER DEG filters
TT 430
LDC 400
LIC 430
to DS 330 PT 430
DS 490 LIC 460
DEG
from DS feed EC 455 Solvent
300 LDC 303 tank super heater DA 460 Glycol surge
TIC 455
drum Excess
FC 490 GX 420 Solvent
LC 490 EC 470 FT
EC 470
DEG/ 470
LIC 430 to glycol
TIC 471
2 DEG /
solvent
solvent
exchanger
slop drum exchanger
1
GX 470
EC 420
EC 420
K5A DA460 DEG to FIC 420 IF 420 DEG
filters
DEG/DEG
DEG / DEG
exchanger
exchanger
2 Liquid
trap
storage DA
GX 490
471
LT 473
Rich DEG
EC 450
3 from
Contactor
EC 450
DEG/DEG
DEG / DEG
exchanger
2
CA 230 exchanger
Signal from
TT 445
dry gas
TT 447
Lean DEG
to contactor
M
Dehydration DEG
FT 445 EB 445 lean glycol
pump GX450
coolerr
Preventive maintenance reduces operating costs. It aims to carry out maintenance regularly in order to avoid
unplanned repairs: early diagnosis of troubles is the best approach. Such diagnoses require thorough online
inspections, careful downtime inspections and servicing, and diligent record keeping.
In addition, if required:
1. Add glycol to surge tank. Note time and amount added,
2. Replace filters when pressure differential reaches 0.7 bar for soft cartridges and 1.7 bar for rigid
cartridges,
3. Replace strainers when plugged,
4. Repair leaks.
At least once a week, fill a quart jar with glycol from the drain top on the storage tank. Hold the jar up to a
light and check carefully for the following:
1. Fine black particles which settle when shaken, this FeS and/or Fe3O4 precipitate indicates ongoing
corrosion and potential failure of the filters,
2. Sniff sample carefully. A sweet, aromatic odour like burnt sugar or overripe bananas suggests thermal
degradation,
3. Check the flow characteristics of the sample. A black, thick viscous solution indicates that heavy
hydrocarbons are being absorbed from the gas,.
4. Check for an oily layer floating on the glycol, which also indicates that heavy, non-volatile hydrocarbons
are being condensed. Such evidence of glycol contamination should be confirmed by a complete glycol
analysis.
5. Estimate glycol loss (should be < 14.1 l/106 Sm3 gas treated).
Every month, or sooner if contamination is suspected, the glycol should be sampled and analyzed for
hydrocarbons, water, solids, iron, chlorides, specific gravity, pH, if deemed appropriate, glycol component
analysis.
Sample both the lean and rich glycol streams and compare with the optimum values in Table VII-B. 16 as
follows:
Remarks:
pH usually lower on rich glycol due to acid-gas content ;
Hydrocarbon, iron and suspended solids may be different for lean and rich glycols, depending on filter
placement ;
Difference between lean and rich glycol water contents should be 2 to 6 %.
Temperature of 60-65°C and high circulation rates improve the cleaning process.
Hot spots and subsequent burnout of reboiler fire tubes are caused by improper firing and/or deposits on the
outside of the tubes (often salt). Adjust burner controls monthly and clean the reboiler thoroughly once a year.
Appendix
Material Safety datasheet is intended to provide workers and emergency personnel with procedures for handling or
working with that substance in a safe manner, and includes information such as physical data (melting point, boiling
point, flash point, etc.), toxicity, health effects, first aid, reactivity, storage, disposal, protective equipment, and spill-
handling procedures.
MSDS formats can vary from source to source within a country depending on national requirements.
Appendix gives preliminary safety consideration of TEG, DEG, Benzene. MSDS are provided by Vendor.
Thanks to refer at the latest issue, each MSDS be regularly updated usually every three to five years.
Product
Product Name Triethylene glycol
Synomyns, Trade names Glycol-bis(Hydroxyethyl)Ether, , TEG,
CAS Number 112-27-6
Physical and chemical properties
Apperance Liquid Odour Mild
Colour Colourless Solubility Solube in water
Relative density 1.126 at 20°C Melting Point (°C) -4,3
Boiling Point (°C) 282-291 Flash point (°C) 177
Auto ignition Temperature (°C) 370
Stability and Reactivity
Stability Stable under normal Material to avoid Strong acids – Strong alkilis
temperatures conditions Strong oxidising substances
Conditions to avoid Avoid excessive heat for Hazardous decomposition CO – CO2
prolonged periods times products
Toxicological and Ecological Information
Inhalation In high concentration, vapours Ingestion May cause discomfort if
may irritate throast and swallowed
respiratory system and cause
coughing
Skin contact Liquid may irritate skin Eye contact Spray and vapour in eyes may
cause irritation and smarting
Ecotoxicity Not regarded as dangerous for Mobility The product is miscible with
environment water.
Handling and Storage
Usage precautions Avoid spilling, skin and eye contact.
Storage precautions Store in tightly closed original container in a dry, cool and well-ventilated place. Keep in original
container.
Exposure controls/Personnal Protection
Engineering measures Provide adequate ventilation. Observe Workplace Exposure Limits and minimise the risk of
inhalation of vapours.
Respiratory equipment No specific recommendation made, but respiratory protection may still be required under
exceptional circumstances when excessive air contamination exists.
Hand protection Use suitable protective gloves if risk of skin contact.
Eye protection If risk of splashing, wear safety goggles or face shield.
Fire fighting measures
Extinguishing media This product is not flammable. Use fire-extinguishing media appropriate for surrounding materials.
Specific Hazards Oxides of: Carbon.
Protective measures in fire Self contained breathing apparatus and full protective clothing must be worn in case of fire.
First aid measures
Inhalation Move the exposed person to fresh air at once. Rinse nose and mouth with water. Get medical
attention if any discomfort continues.
Ingestion NEVER MAKE AN UNCONSCIOUS PERSON VOMIT OR DRINK FLUIDS! Rinse mouth thoroughly. Get
medical attention if any discomfort continues.
Skin contact Remove affected person from source of contamination. Remove contaminated clothing. Wash the
skin immediately with soap and water. Get medical attention if any discomfort continues.
Eye contact Make sure to remove any contact lenses from the eyes before rinsing. Promptly wash eyes with
plenty of water while lifting the eye lids. Continue to rinse for at least 15 minutes. Get medical
attention if any discomfort continues.
Product
Product Name Diethylene glycol
Synomyns, Trade names DEG
CAS Number 111-46-6
Physical and chemical properties
Apperance Liquid Odour Odourless
Colour Colourless Solubility Solube in water
Relative density 1.118 at 20°C Melting Point (°C) -9
Boiling Point (°C) 245 Flash point (°C) 145
Auto ignition Temperature (°C) 364
Stability and Reactivity
Stability Stable under normal Material to avoid Strong acids – Strong alkilis
temperatures conditions Strong oxidising substances
Conditions to avoid Hazardous decomposition CO – CO2 – Alcohol ether -
products Aldhehydes
Toxicological and Ecological Information
Inhalation In high concentration, vapours Ingestion Harmfull if swallowed. Irriting.
may irritate respiratory system May cause nausea, stomach
or lungs pain and vomiting
Skin contact Liquid may irritate skin Eye contact May cause temporary eye
irritation
Ecotoxicity Not regarded as dangerous for Mobility The product is miscible with
environment water.
Handling and Storage
Usage precautions Avoid spilling, skin and eye contact.
Storage precautions Keep separate from food, feedstuffs, fertilisers and other sensitive material. Store in thihtly closed
original container in a dry, cool and well-ventillated place.
Exposure controls/Personnal Protection
Engineering measures Provide adequate ventilation, including appropriate local extraction, to ensure that the defined
workplace exposure limit is not exceeded.
Respiratory equipment In case of inadequate ventilation use suitable respirator. Use respiratory equipment with
combination filter,
Hand protection Use suitable protective gloves if risk of skin contact. Use protective gloves made of: Butyl rubber.
Neoprene. Rubber (natural, latex). Nitrile. Polyvinyl chloride (PVC).
Eye protection Wear approved safety goggles.
Fire fighting measures
Extinguishing media Extinguish with alcohol-resistant foam, carbon dioxide, dry powder or water fog. Do not use water
jet as an extinguisher, as this will spread the fire.
Specific Hazards By heating and fire, toxic vapours/gases may be formed. Carbon monoxide (CO). Carbon dioxide
(CO2).
Protective measures in fire Self contained breathing apparatus and full protective clothing must be worn in case of fire.
First aid measures
Inhalation Move into fresh air and keep at rest. When breathing is difficult, properly trained personnel may
assist affected person by administering oxygen. Get medical attention.
Ingestion Do not induce vomiting. Get medical attention immediately! Immediately rinse mouth and drink
plenty of water (200-300 ml).
Never give liquid to an unconscious person.
Skin contact Rinse immediately with plenty of water. Immediately remove contaminated clothing. Wash
contaminated clothing before reuse.
Get medical attention if any discomfort continues.
Eye contact Immediately flush with plenty of water for up to 15 minutes. Remove any contact lenses and open
eyes wide apart. Rinse with water. Contact physician if discomfort continues.
Product
Product Name Benzene
Synomyns, Trade names Benzol - Cyclohexatriene - Phenyl Hydride.
CAS Number 71-43-2
Physical and chemical properties
Apperance Liquid. Odour Characteristic aromatic odour.
Colour Clear Colourless Solubility In most organic solvent
Relative density 0,879 at 20°C Melting Point (°C) 5,5
Boiling Point (°C) 80,1 Flash point (°C) -11
Auto ignition Temperature (°C) 560
Stability and Reactivity
Stability Stable at ambient Material to avoid Inorganic Acids, Oxidizing
temperature. agents
Conditions to avoid Source of ignition Hazardous decomposition Oxides of Carbon
products
Toxicological and Ecological Information
Inhalation Benzene vapour will irritate Ingestion Ingestion will irritate the
the respiratory tract and be digestive tract and be
absorbed in the lungs causing absorbed into the body.
systemic effects. Ingestion can cause severe
pulmonary oedema.
Skin contact Benzene is toxic and irritating Eye contact Benzene is irritating to eyes
to skin. It can be absorbed and may be absorbed into the
through the skin which may body if allowed to splash
lead to irreversible effects. around the eye.
Ecotoxicity Not regarded as dangerous for Mobility Mobile between phases,
environment volatility ensures rapid
evaporation from water
bodies.
Handling and Storage
Usage precautions Benzene should only be handled by persons who are trained in its hazardous properties and are
adequately protected
Storage precautions Cool and well ventilated local. Storage media : Mild steel, stainless steel, copper
Exposure controls/Personnal Protection
Engineering measures Ventilation and Equipment should be earthed and bonded.
Respiratory equipment Self contained breathing apparatus.
Hand protection PVC or rubber gloves.
Eye protection Safety goggles
Fire fighting measures
Extinguishing media Extinguish with alcohol-resistant foam, carbon dioxide, dry powder or water fog. Do not use water
jet as an extinguisher, as this will spread the fire.
Specific Hazards By heating and fire, toxic vapours/gases may be formed. CO, CO2
Protective measures in fire Self contained breathing apparatus and full protective clothing must be worn in case of fire.
First aid measures
Inhalation Move into fresh air and keep at rest. When breathing is difficult, properly trained personnel may
assist affected person by administering oxygen. Get medical attention.
Ingestion Do not induce vomiting. Get medical attention immediately! Immediately rinse mouth and drink
plenty of water (200-300 ml).
Never give liquid to an unconscious person.
Skin contact Rinse immediately with plenty of water. Immediately remove contaminated clothing. Wash
contaminated clothing before reuse.
Get medical attention if any discomfort continues.
Eye contact Immediately flush with plenty of water for up to 15 minutes. Remove any contact lenses and open
eyes wide apart. Rinse with water. Contact physician if discomfort continues.
1
xw =
18 C Eqn 19
1+
150.2 100 - C
With Water-vapour content of gas in equilibrium We with the lean glycol entering the absorber:
In general, correlations used today agree reasonably well with the measurements and are adequate for
most TEG system designs. All are limited by the ability to measure accurately the equilibrium
concentration of water in the vapour phase above TEG solutions. The Parrish correlation (1986) has
been used to establish Figures VII-B.3 and VII-B.4, because equilibrium water concentrations in the
vapour phase were determined at infinite dilution (essentially 100 % TEG). The other correlations, like
Worley, use extrapolations of data at lower concentrations to estimate equilibrium in the infinite dilute
region.
Obviously, any uncertainty in the vapour liquid equilibrium data produces an equal uncertainty in the
computer simulation21.
Generally, a tray efficiency equal to 25 % for bubble cap trays is used, and the figure for the actual
number of trays is rounded off to the next higher integer value.
For the structured packing-type contactor, a minimum of 1.2 m height of packing must be used for one
theoretical plate. 1.5 m height is a mean value.
The minimum number of bubble cap trays to be installed is 6. It corresponds to 1.5 theoretical trays
(average value).
The absorption factor value by the following basic absorption equation (Kremser-Brown
approach):
W i - Wo A n + 1 - A
Eqn 23
W i - We A n+1 - 1
Figure VII-B. 51 represents on the ordinate the ratio, on the abscissa the absorption factor. To
obtain the A value
W i - Wo
1. Enter the righthand ordinate at the value
W i - We
2. Read horizontally to the number of theoretical plates selected
Then the Glycol circulation molar rate per unit of gas volume L:
The glycol circulation rate is given by the following expression of the Absorption factor:
L
A Eqn 24
Kvs * V
Calculate the lean glycol molecular weight with the following equation:
100
M
C 100 C Eqn 25
150.2 18
The Amount of lean TEG circulation rate per unit of removed water
24 m
r Eqn 27
(Wi Wo ) Q
For economic reasons the recommended lean glycol circulation rate to be used is in the range
15 to 35 kg per kg of removed water in the gas by time unit.
A good average value is around 27.4 kg of lean TEG per kg of water removed (3 gallons of lean
TEG per pound of removed water).
Increasing the glycol flowrate and purity may reduce the structured packing height. But the
gain obtained by the reduction of the glycol contactor height is counter balanced by the
increase of the regeneration unit size since more glycol have to be treated.
The GS ECP 101 gives the minimum of lean TEG circulation rate per unit of removed water,
versus the water – vapour content of the gas at the absorber inlet.
Furthermore, to insure a good wetting of the structured packing, a minimum glycol flowrate of
one cubic meter per hour per square meter of dehydration column area section is required.
Glycol Dehydration unit - Technical information to include in a feedback document Glycol Dehydration unit - Technical information to include in a feedback document
EQUIPMENT DATA (1/3) : HEAT EXCHANGERS
PROCESS DATA
PFD
GAS COMPOSITION
Join a glycol dehydration PFD Yes
N2 % mol
C02 % mol Reboiler
H2S % mol Heating Medium : -
Maximum flowrate 106 Sm3/da y or 106 Std cuft/da y Lean glycol Inlet temperature °C or °F
Outlet temperature °C or °F
Operating flowrate 106 Sm3/da y or 106 Std cuft/da y
Maximum pressure ba r a bs or ps i a Lean Glycol Cooler
Operating pressure ba r a bs or ps i a Cold side fluid Dry Ga s /Wa ter /Ai r Air
Maximum temperature °C or °F Heat transfer area m2 or ft2
or water content required kg/106 Sm3 or l b/Std cuft Atmospheric Inlet temperature °C or °F
cooler Outlet temperature °C or °F
ABSORBANT
Glycol type TEG, DEG, TREG
lean absorbant flowrate kg/106 Sm3 or l b/106 Std cuft
lean absorbant concentration wei ght %
absorbant losses kg/106 Sm3 or l b/Std cuft
or kg/da y or l b/da y
PRODEM
SECTION N° VII-C
REVISIONS
T.BRENAS
P. CHILLEMI
8 12/2011 Major Revision G. DELANNAY A. GERVAIS A. ROCHER
L. PAGNON
ENEA Consulting
CONTENTS
REVISIONS........................................................................................................................................................... 0
Contents........................................................................................................................................................... 1
Figures.............................................................................................................................................................. 2
Tables............................................................................................................................................................... 2
References ....................................................................................................................................................... 3
Glossary ........................................................................................................................................................... 3
OVERVIEW .......................................................................................................................................................... 4
1. General Information regarding gas refrigeration and hydrate inhibition processes .................................. 5
1.1. Gas Refrigeration ................................................................................................................................ 5
1.2. IFPEXOL – IFP Gas Dehydration Process............................................................................................... 8
1.2.1. IFPEXOL process ........................................................................................................................... 8
1.2.2. IFPEX-1 ........................................................................................................................................ 8
1.2.3. Installed IFPEXOL processes ....................................................................................................... 10
1.3. Twister process ................................................................................................................................. 11
1.3.1. Process purposes ....................................................................................................................... 11
1.3.2. Process description .................................................................................................................... 12
1.3.3. Installations ............................................................................................................................... 14
2. Design ..................................................................................................................................................... 15
3. Operational feedback.............................................................................................................................. 15
3.1. IFPEXOL process................................................................................................................................ 15
FIGURES
Figure VII-C. 1 – Typical process of gas cooling – Low Temperature Separation ............................................... 5
Figure VII-C. 2 – Diagram of typical gas cooling processes................................................................................ 6
Figure VII-C. 3 – Gas cooling by Joule-Thompson Expansion ............................................................................ 6
Figure VII-C. 4 – Gas cooling by Turbo-Expander .............................................................................................. 7
Figure VII-C. 5 – Gas cooling by External Refrigeration ..................................................................................... 7
Figure VII-C. 6 – Typical Schematic Flow Diagram of IFPEX 1 ............................................................................ 9
Figure VII-C. 7 – Twister schematic ................................................................................................................. 12
Figure VII-C. 8 – Twister scheme .................................................................................................................... 13
Figure VII-C. 9 – Twister application decision tree.......................................................................................... 13
TABLES
REFERENCES
GLOSSARY
SYMBOL DEFINITION
IFP Institut Français du Pétrole
LPG Liquefied Petroleum Gas
NGL Natural Gas Liquids
Table VII-C. 1 – Glossary
OVERVIEW
Introduction
• As part of the TOTAL PRODEM manual this chapter provides a reference tool for TOTAL process
engineers. PRODEM aims to provide the user with technical information and a standard set of tools to
facilitate process design. The contents of this chapter are relevant to all TOTAL process engineers and
aimed specifically at junior process engineers in ECP and process design engineers in TOTAL affiliates.
• This particular section is dedicated to gas refrigeration and hydrate inhibition processes.
General content
General information regarding the gas refrigeration “Low Temperature Separation Process” is provided.
Water vapor (moisture) shall be removed from sales gas to lower the temperature at which water will
condense (called the "water dew point" of gas), in order to prevent hydrate or ice from appearing into the
stream at a given pressure. Most gas sales contracts specify a maximum value for the amount of water vapor
allowable in gas. For instance, in the European Consortium the water dew point for gas shall be - 15°C at 70
bara. More information in that respect is provided in PRODEM chapter VI dedicated to products Specifications.
Gas dehydration can be achieved by refrigeration in presence of hydrate inhibitor and freeze protection.
Mono-ethylene glycol (MEG), Di-ethylene glycol (DEG), methanol and kinetic hydrate inhibitor (KHI) are the
most commonly used hydrate inhibitors. The process of cooling the gas to condensate the heavy ends and
water is known as the Low Temperature Separation (LTS) process as shown on the Figure VII-C. 1.
WET
DRY
WET
The Figure VII-C. 2 illustrates on a PT diagram the two typical gas cooling cycles:
• JT valve process : the link between the thermodynamic states (ABCD) and the process steams is shown
on the Figure VII-C. 3
• Turboexpander process : the link between the thermodynamic states (AB’C’D’) and the process
steams is shown on Figure VII-C. 4
B’ B A
Pressure
C D
C’ D’
Cricondenbar
Phase envelope of
Liquid natural gas
Turboexpander process
Cricondentherm Temperature
Several processes can be applied to refrigerate the gas; among them the following technologies can be
mentioned:
- Isenthalpic expansion through a Joule-Thompson valve (J.T. valve), appropriate to relatively high
pressure feed gas (70 bara and higher) (state A). Typically, the temperature decrease due to the
expansion is in the order of magnitude 0.30 to 0.45 °C/bar (from B to C). Finally, a heat recovery
between feed gas (from A to B) and NGL free gas (from C to D) is commonly realised.
B C
- Polytrophic Expansion through a turbo expander, appropriate to relatively high pressure feed gas (70
bara and higher) (state A). In this process, the feed gas provides energy to the turbine (which drives a
compressor in most cases to recompress the condensate free gas: from D’ to D), resulting in a decrease
in the enthalpy of the gas (from B to C), and hence in a temperature decrease. The order of magnitude
of temperature fall with the pressure reduction is 0.8 to 1.0 °C/bar.
D’ D
C’
B’
A
- External Refrigeration source such as a propane loop: It is broadly appropriate when relatively low
pressure process is at stake (over 30 bara).
DRY
WET
WET
The related principles of condensation, hydrate formation and hydrate inhibition are further developed in
PRODEM chapters:
• PRODEM Chapter IV – Fluid behaviour, which deals with hydrates, formation and inhibition
• PRODEM Chapter IX – Natural gas liquids recovery, which deals with condensation, and cooling cycles
Patented by IFP (Institut Français du Pétrole), the IFPEXOL process is a cryogenic liquid separation that uses
methanol for water dew pointing remediation instead of glycols. This process becomes even more interesting
when water dewpointing and hydrocarbon dewpointing are both required.
The IFPEXOL process is based on two independent steps, with no heat requirement nor atmospheric venting.
Each step can be used independently or both steps can be combined together:
• IFPEX-1: Simultaneous water and hydrocarbon dew pointing.
• IFPEX-2: Acid gas and sulfur compounds removal to achieve sales specifications.
IFPEX-2 is further developed in PRODEM Chapter XI.B – Gas Sweetening (External hyperlink).
1.2.2. IFPEX-1
Figure VII-C. 5 represents the process scheme of IFPEX treatment. The natural gas inlet is split into two
streams. The stream (1), representing 50% of the total flowrate, passes through the IFFEX-1 contactor tower,
while the stream (9) bypasses the tower.
The gas rises in the contactor tower (3) while methanol is vaporized from the top (2) and is stripped from the
rich aqueous phase by the gas so that almost pure water is collected from the bottom of the IFPEX-1 contactor
(4).
Afterwards the bypass stream (9) and the IFPEX-1 contactor gas outlet (5) are recombined and a makeup of
methanol (10) is provided before feeding a cold process (JT valve, Turbo expander, Propane Loop, etc), and
then the cold separator (8). The cold process (7) aims to reduce the gas temperature to the point at which the
water or hydrocarbon dew point specification is reached.
The water/methanol blend recovered in the cold separator (2) is recycled to the contact tower (3). The liquid
hydrocarbon condensed in the cold separator (11) can be further treated to enhance the methanol recovery
rate [3].
According to IFP and Prosernat, IFPEX-1 can usually reach hydrocarbon and water dew points between -80°C
and -100°C (at 80 bar abs), which can represent dew point depressions beyond 140°C depending on the gas
temperature.
• Advantages:
The IFPEX-1 process employs methanol instead of triethylene glycol (TEG) to dehydrate the gas. No thermal
regeneration of the solvent is consequently required.
In addition it offers a number of benefits with regards to glycol technologies, including more compact design
with only one contactor tower (of a special interest for offshore locations), no required heating, no foaming in
contactors, reduced corrosion and solvent degradation, and the ability to locate the cold section at a separate
treating position.
• Disadvantages:
The IFPEX 1 process induces methanol losses mainly in the outlet gas and condensate streams. As a
consequence, attention should be paid to downstream products specifications regarding the maximum
methanol content allowable (for further information on products specifications, refer to PRODEM Chapter VI).
Considering the low interfacial tension between the water-methanol mixture and hydrocarbons, there is a risk
of emulsion in the cold separator, which would lead to higher methanol losses in the hydrocarbon stream
(refer to PRODEM Chapter IV-D – Crude emulsion). Besides affecting the cost-effectiveness of the dehydration
process, higher methanol losses due to emulsion may require a treatment of the condensates downstream the
dehydration unit in order to reach the condensate methanol specification.
The Twister technology is based on condensation and separation at supersonic velocity. It relies on a static
device hence its stability: avoiding the use of any rotating part nor chemicals, it ensures a rather simple facility
with a high availability. This technology presents other advantages like no environmental emissions, a compact
design, a low weight, an unmanned operation, and a nearly instantaneous start-up.
The Twister Supersonic Separator combines adiabatic cooling and cyclonic separation in a single compact
device. Adiabatic cooling is achieved in a Laval nozzle—an aerodynamically shaped venturi tube— which
achieves an adiabatic and isentropic expansion efficiency of typically 80%. The swirling motion is generated by
a vane ring at the entrance of the Laval nozzle. The swirl strength increases strongly, due to contraction in the
nozzle, resulting in a centrifugal field of about 500,000 g. The fine dispersed liquids formed during the
adiabatic expansion are separated as a result of the centrifugal forces exerted by the strong swirling flow, and
removed from the dry flow at minimum temperature and pressure with a separation efficiency of typically
95%. At the point where liquid/gas separation takes place, the total fluid velocity is around 400 m/s. The
remaining kinetic energy in the separated flowstreams within the tube is transformed to increased static
pressure in the diffuser section.
The Figure VII-C. 7 represents the Twister dehydration process. Cold gas is fed into the inlet separator (3). Then
the gas feeds the Twister tubes (4), where an isentropic gas expansion occurs at supersonic velocity; the gas
cools down to cryogenic temperatures and water and NGLs condense. Afterwards the condensed liquids are
separated in the liquid degassing vessel (5). The separated product streams are recompressed using a diffuser,
reducing the velocity.
The stream separated from the main gas stream thanks to centrifugal forces is a mix of liquids (water and
condensate), which also contains slip gas. Slip gas is removed in either a two- or three-phase liquid degassing
vessel (5) and recombined with the dry gas stream. Dry export gas is directed through the exchanger (2) to
cool the feed stream.
The following flow sheet represents a decision tree which helps to determine whether the Twister technology
can be applicable or not as according to operating conditions:
Y
Flow rate
>200 act.m3/hr
Y
N
C3+ mole Y N
Water spec
fraction
> 3lbs/mmscf
>1%?
N
N
N Y
HC spec
Y N Y >25% free Y Remove location or
HC dew point > -3°C? Glycol usage
pressure drop Offshore or Hardly
required? @circondenther allowable? Y
available? accessible?
m
Y N N
N
N
N
C3+ recovery Y
<95 mole%?
• Advantages:
Twister technology presents some cost reductions, on both CAPEX and OPEX:
- Simultaneous hydrocarbon and water dewpointing, avoiding multiple processes
- A compact and low weight design enables offshore structure cost reduction
- A claimed high availability, with thus less equipment sparing
- The absence of moving parts induces less maintenance
- Being chemical-free, the process relies on reduced supply and logistic costs
- The operation is unnamed
As previously mentioned, the additional advantages are:
- Environmental (no emissions)
- Ease of use (nearly instantaneous start-up)
• Disadvantages:
- A flowrate of at least 200 Am3/d is required to ensure a suitable pressure drop
- The process applicability is strongly dependent on gas compositions: If C3+ mole% is lower than
1%, the Twister process can’t be selected. Indeed, if the C3+ fraction in feed becomes too low, the
condensed fraction of the stream diminishes so that liquid droplets diameter becomes smaller
than 0.5 micron, hence not anymore separable in a cyclonic separation device.
1.3.3. Installations
No Twister unit is operated within TOTAL. Table VII-C. 3 lists the installations referenced in 2007:
2. DESIGN
3. OPERATIONAL FEEDBACK
• Inhibitor losses
As previously mentioned, inhibitor losses in hydrocarbon can be experienced in the IFPEXOL process due to
methanol volatility, and emulsion issues. High concentration of methanol in the export hydrocarbon streams
(gas and condensate) could consequently lead to disrespect products specifications.
Although there are generally no specifications on sales gas methanol content, in the case of Elgin PUQ in UK,
sales gas specifications limit the methanol concentration to 5 mg / Sm³ on normal operating conditions (for
treatment stability issues). Similarly, the methanol content of LPG is usually limited to 500 ppmv if the LPG is
meant to feed an isomerisation or an alkylation plant (see PRODEM Chapter VI – Products Specifications).
As a consequence, the operating conditions of the IFPEXOL process shall be defined so as to limit methanol
losses in hydrocarbon streams. Inhibitor losses depend on the inlet raw gas composition. But as a general rule,
Prosernat recommends not to operate the IFPEXOL dehydration process (IFPEX-1) above -20°C.
PRODEM
SECTION N° VII-D
GAS DEHYDRATION
MOLECULAR SIEVE DEHYDRATION UNIT
Date Author
SCOPE 4
REFERENCES 4
RECOMMENDATIONS 4
GENERAL 5
DESIGN CONSIDERATIONS 7
1. TEMPERATURE 7
2. PRESSURE 8
3. CYCLE TIME 8
4. GAS VELOCITIES 8
5. BED HEIGHT TO DIAMETER RATIO 9
6. PRESSURE DROP 9
7. MOISTURE CONTENT OF INLET GAS 9
8. DESICCANT SELECTION 10
EQUIPMENT CHARACTERISTICS 12
1. INLET SEPARATOR 12
2. ADSORPTION TOWER 12
3. REGENERATION HEATER 13
4. REGENERATION COOLER 13
5. REGENERATION SEPARATOR 13
6. SWITCHING VALVES 13
7. PIPING 13
8. DRY GAS FILTERS 13
APPENDIX
Figure VII-D1 - Gas dehydration by solid desiccant dehydrator twin tower system - Typical
schematic flow diagram
Figure VII-D2 - Absorbent bed support
Figure VII-D3 - Mole sieve capacity corrections
Figure VII-D4 - Gas treatment - Typical total cycle
Figure VII-D5 - Inlet and outlet regeneration gas temperatures during typical solid desiccant
bed regeneration cycle
SCOPE
Adsorption (or solid bed) dehydration is the process where a solid desiccant is used for the removal of
water vapour from a gas stream. The solid desiccants commonly used for gas dehydration are those
that can be regenerated and, consequently, used over several adsorption-desorption cycles.
Some solid desiccants, such as molecular sieves, can dehydrate gas to 1 ppm or less; these
desiccants are widely used on feed streams for cryogenic processing.
This section introduces several aspects of the basic adsorption dehydration unit processing.
REFERENCES
RECOMMENDATIONS
Most adsorbents tend to adsorb heavy hydrocarbons, glycols and methanol, resulting in
contamination and a reduction in capacity. These components are difficult to remove during
regeneration. Therefore, for efficient desiccant performance and for a longer desiccant life, the inlet
gas stream must be thoroughly cleaned to remove all liquids and solids.
GENERAL
Adsorption is a surface phenomenon. All solid surfaces have some ability to adsorb, i.e., capture and
hold molecules from gases or liquids on their surfaces. Two types of gas (or liquid) adsorption occur :
chemical adsorption and physical adsorption. Physical adsorption is caused by Van der Waals forces
between the gas or liquid molecules and the surface thus forming multilayer of adsorbate on the
surface.
The desiccant is a solid, granulated drying or dehydrating medium with an extremely large effective
surface area per unit weight because of a multitude of microscopic pores and capillary openings. A
typical desiccant might have as much as 800 square meter of surface area per gram.
The initial cost for a solid bed dehydration unit generally exceeds that of a glycol unit. However, the
dry bed has the advantage of producing very low dew points, which are required for a cryogenic plant,
and is adaptable to very large changes in flow rates.
Disadvantages are that it is a batch process, there is a relatively high pressure drop through the
system, and desiccants are sensitive to poisoning with liquids or other impurities in the gas.
Multiple desiccant beds are used in cyclic operation to dry the gas on a continuous basis. The number
and arrangement of the desiccant beds may vary from two towers, adsorbing alternatively, to many
towers.
Three separate functions or cycles must alternatively be performed in each tower. They are: an
adsorbing or gas drying cycle, a heating or regeneration cycle, and a cooling cycle.
Figure VII-D1 is a flow diagram for a typical two-tower solid desiccant dehydration unit.
• a high-temperature heater to provide hot regeneration gas to reactivate the desiccant in the
towers,
• a regeneration gas cooler to condense water from the hot regeneration gas,
• a regeneration gas separator to remove the condensed water from the regeneration gas,
• piping, manifolds, switching valves and controls to direct and control the flow of gases
according to the process requirements.
In the drying cycle, the wet inlet gas first passes through an inlet separator where free liquids,
entrained mist, and solid particles are removed. Most adsorbents tend to adsorb heavy hydrocarbons,
glycols and methanol, resulting in contamination and a reduction in desiccant capacity. These
components are difficult to remove during regeneration. Therefore, for efficient desiccant performance
and for a longer desiccant life, the inlet gas stream has to be thoroughly cleaned to remove all liquids
and solids.
In the drying cycle, the wet inlet gas flows downward through the tower. The adsorbable components
are adsorbed at rates dependent on their chemical nature, the size of their molecules, and the size of
the pores. The water molecules are adsorbed first in the top layers of the desiccant bed. Dry
hydrocarbon gases are adsorbed throughout the bed. As the upper layers of desiccant become
saturated with water, the water in the wet gas stream begins displacing the previously adsorbed
hydrocarbons in the lower desiccant layers. Liquid hydrocarbons will also be adsorbed and will fill
pore spaces that would otherwise be available for water molecules.
For each component in the inlet gas stream, there will be a section of bed depth, from top to bottom,
where the desiccant is saturated with that component and where the desiccant below is just starting to
adsorb that component. The depth of bed from saturation to initial adsorption is known as the mass
transfer zone. This is simply a zone or sections of the bed where a component is transferring its mass
from the gas stream to the desiccant's surface.
As the flow of gas continues, the mass transfer zones (M.T.Z.) move downward through the bed and
water displaces the previously adsorbed gases until finally the entire bed is saturated with water
vapour. If the entire bed becomes completely saturated with water vapour, the outlet gas is just as wet
as the inlet gas. Obviously, the towers must be switched from the adsorption cycle to the regeneration
cycle (heating and cooling), before the desiccant bed is completely saturated with water.
At any given time, at least one of the towers will be adsorbing while the other towers will be in the
process of being heated or cooled to regenerate the desiccant.
When a tower is switched to the regeneration cycle, some dry gas (that is, the outlet gas downstream
of the adsorbing tower) is heated to temperatures of 230°C to 315°C in the high-temperature heater
and routed to the tower to remove the previously adsorbed water. As the temperature within the tower
is increased, the water captured within the pores of the desiccant turns to stream and is adsorbed by
the natural gas. This gas leaves the top of the tower and is cooled by the regeneration gas cooler.
When the gas is cooled, the saturation level of water vapour is lowered significantly and water is
condensed.
The water is separated in the regeneration gas separator and the cool, saturated regeneration gas is
very often recycled to be dehydrated. This is done by recompressing the regeneration gas.
In some gas liquefaction plants the regeneration gas used is not outlet gas downstream of the
adsorbing tower but recompressed boil off produced in flash separator located just before liquefied
natural gas (LNG) storage tank.
This gas leaving the tower in regeneration is used as fuel gas.
In this case the regeneration cycle is performed at lower pressure (fuel gas pressure). This scheme
corresponds to an optimization of the power consumption of a liquefaction plant.
Once the bed has been "dried" in this manner, it is necessary to flow cool gas through the tower to
return it to normal operating temperatures (about 35°C to 50°C), before putting it back in service to
dehydrate gas. It is the cooling cycle.
The cooling gas is gas that has already been dehydrated. A hot tower will not sufficiently dehydrate
the gas because desiccant efficiency is temperature depending: cold temperature favours adsorption,
hot temperature favours desorption.
The beds switching is controlled by a time controller that performs switching operations at specified
times in the cycle. The length of the different phases can vary considerably. Longer cycle times will
require larger beds, but will increase the bed life. A typical two-bed cycle might have an eight-hour
adsorption period with six hours of heating and two hours of cooling for regeneration. Adsorption units
with three beds typically have one bed being regenerated, on fresh bed adsorbing, and one bed in the
middle of the drying cycle.
Internal or external insulation for the adsorbers may be used. The main purpose of internal insulation
is to reduce the total regeneration gas requirements and costs. Internal insulation eliminates the need
to heat and cool the steel walls of the adsorber vessel (Saving up to 30 % of the total regeneration
heat). Normally, a cast-able refractory lining is used for internal insulation. The refractory must be
applied and properly cured to prevent liner cracks. Liner cracks will permit some of the wet gas to
bypass the desiccant bed. Only a small amount of wet, bypassed gas is needed to cause freeze-ups
in cryogenic plants. Ledges installed every few feet along the vessel wall can help eliminate this
problem. To eliminate this kind of problem, the best is to apply an external insulation.
DESIGN CONSIDERATIONS
1. TEMPERATURE
Adsorption plant operation is very sensitive to the temperature of the incoming gas. Generally, the
adsorption efficiency decreases as the temperature increases.
If regeneration gas is recycled, i.e. mixed with the wet inlet gas, condensed liquids can appear when
the hotter gas stream is saturated with water and/or hydrocarbon during its cooling by the colder
stream, or when the gas mixture reaches its water and/or hydrocarbon dew point.
The temperature of the hot gas entering and leaving a desiccant tower during the heating cycle
affects both the dehydration unit efficiency and the desiccant life. To assure good removal of the
water and other contaminants from the bed, a high regeneration gas temperature is needed. The
maximum hot gas temperature depends on the type of contaminants and the "holding power" or
affinity of the desiccant for the contaminants. A temperature of 230°C to 315°C is normally used.
The desiccant bed temperature reached during the cooling cycle is important. The use of dry gas for
cooling, allows to cool the desiccant bed within a differential temperature of 5°C to 10°C of the
incoming gas temperature during the adsorption cycle. This maximizes the adsorption capacity of the
bed.
The temperature of the regeneration gas in the regeneration gas scrubber should be low enough to
condense and remove the water and hydrocarbons from the regeneration gas without causing hydrate
problems.
2. PRESSURE
Generally, the adsorption capacity of a dry bed unit decreases as the pressure is lowered. If the
towers are operated well below the design operating pressure, the desiccant will have to work harder
to remove the water and to maintain the desired effluent dew point. With the same volume of
incoming gas, the increased gas velocity, occurring at the lower pressure, could also affect the
effluent moisture content and damage the desiccant.
3. CYCLE TIME
Most adsorbers operate on a fixed drying cycle time and, frequently the cycle time is set for the worst
conditions. However, the adsorbent capacity is not a fixed value; it declines with usage. A new
desiccant has a very high capacity for water removal for the first few months of operation. A moisture
analyser is installed on the effluent gas, a much longer initial drying cycle can be achieved. As the
desiccant ages, the cycle time will be automatically shortened. This will save regeneration fuel costs
and improve the desiccant life, because fuel consumption and desiccant ageing are also depending of
the number of regeneration cycles.
The water content monitoring of each tower is recommended.
An example of cycle time is given in figure VII-D4.
The heating time is usually 50 % to 60 % of the total regeneration time which must include a cooling
period. Figure VII-D.5 – Inlet and outlet regeneration gas temperatures during typical solid desiccant
bed regeneration cycle-shows a typical temperature profile for a regeneration cycle (heating and
cooling). For 8 hours adsorption cycles, the regeneration normally consists of around 4 ½ hours of
heating, around 3 hours of cooling and around ½ hour for standby and switching.
4. GAS VELOCITIES
Generally, as the gas velocity during the drying cycle decreases, the ability of the desiccant to
dehydrate the gas increases.
At lower actual velocities, drier effluent gases will be obtained. Consequently, it would seem desirable
to operate at minimum velocities to fully use the desiccant.
However, low velocities require towers with large cross-sectional areas to handle a given gas flow,
and allow the wet gas to channel through the desiccant bed and not be properly dehydrated.
In selecting the design velocity therefore, a compromise must be made between the tower diameter
and the maximum use of the desiccant. The table as follows, shows a maximum design velocity.
Smaller velocities may be required due to pressure drop considerations.
Pressure (bar g) 10 20 30 40 50 60 70
maximum superficial velocity 26.8 20.7 17.7 15.2 13.4 12.5 12.2
(m/min)
In its simplest form, a tower is normally a cylindrical tower filled with a solid desiccant. The depth of
the desiccant may vary from a 1 to 10 meters or more. The vessel diameter may be from a few
decimetres to 4.5 meters.
Ratios as low as 1:1 are sometimes used ; however, poor gas dehydration, caused by non-uniform
flow, channelling and an inadequate contact time between the wet gas and the desiccant sometimes
result.
6. PRESSURE DROP
Towers are sized for a design pressure drop about 0.35 bar through the desiccant. A design pressure
drop higher than 0.55 bar is not recommended.
∆P 2
= Bµvs + CρvS
L
where :
An important variable that determines the size of a given desiccant bed is the relative saturation of the
inlet gas. This variable is the driving force that affects the transfer of water to the absorbent. If
saturated gas is being dried, higher useful capacities can be expected for most desiccants than when
drying partially saturated gases. However, in most field gas dehydration installations the inlet gas is
saturated with water vapour and this is not a variable that must be considered.
8. DESICCANT SELECTION
No desiccant is perfect or best for all applications. In some applications, the desiccant choice is
determined primarily by economics. Sometimes the process conditions control the desiccant choice.
Many times the desiccants are interchangeable and the equipment designed for one desiccant can
often be operated effectively with another product. Table, as follows, illustrates the most common
desiccants used for gas dehydration and some conservative parameters to use for initial design.
All desiccants exhibit a decrease in capacity (design loading) with increase in temperature. Molecular
sieves tend to be the less severely affected and aluminas the most affected by temperature. Aluminas
and molecular sieves act as a catalyst with H2S and CO2 to form COS. When the bed is regenerated,
sulfur remains and plugs up the spaces.
Liquid hydrocarbons also present a plugging problem to all desiccants but molecular sieves are less
susceptible to contamination with liquid hydrocarbons.
Silica gels will shatter in the presence of free water and are chemically attacked by many corrosion
inhibitors. The chemical attack permanently destroys the silica gels. The other desiccants are not as
sensitive to free water and are not chemically attacked by most corrosion inhibitors. However, unless
the regeneration temperature is high enough to desorb the inhibitor, the inhibitor may adhere to the
desiccants and possibly cause coking. The same phenomenon appears with the C6+ hydrocarbons
fractions.
The activated aluminas, and molecular sieves are all chemically attacked by strong mineral acids and
their adsorptive capacity will quickly decline. Special acid resistant molecular sieve desiccants are
available.
Molecular sieves possess the highest water capacity, will produce the lowest water dew points. They
also are usually much more expensive.
Molecular sieves are commonly used ahead of LNG cryogenic section and NGL recovery plants
where extremely dry gas is required. Cryogenic NGL plants designed to recover ethane produce very
cold temperatures and require very dry feed gas to prevent formation of hydrates. Dehydration to
approximately 1 ppmw (water dew points around – 100°C at gas pressure) is possible with molecular
sieves.
Molecular sieves are crystalline zeolites or metal alumino-silicates having a uniform, three-
dimensional interconnecting structure of alumina and silica tetrahedra.
These synthetic zeolite crystals are manufactured to contain interconnecting cavities of uniform size,
separated by equally uniform pores or narrower openings. The silica and alumina tetrahedra form a
sodalite cage or truncated octahedron having a silica or alumina tetrahedron each point. Different
crystal structures are obtained by varying the metal cation (Na, K or Ca) and the alumina to silica
ratio.
Two types of structures are commonly used in gas processing. In type A, the sodalite cages form a
simple cubic structure. When the metal cation is sodium, the pores are 4.2 angstroms (Å) in diameter,
and the mole sieve is called 4A. Replacing Na with K results in type 3A (pore size about 3 Å) and
substituing Ca for Na yields type 5A (or 5 Å pores).
In type X, the sodalites cages are arranged in a tetrahedral structure. The sodium form, type 13 X has
a pore size of 10 Å.
LNG plant feed pretreatment 4A, 5A, 13X Choice of system would depend on
specifics.
A typical system could be a main 4A or
5A bed for H20, C02 and H2S removal
A 13X trimmer bed for mercaptan
removal.
In some plants the towers are filled with tow layers of molecular sieves of different type to eliminate in
the same tower the water and the sulphur compounds contained in the gas.
At the top a first layer is devoted to the water removal. Below, in the bottom part a second layer with
an other molecular sieve type allows the mercaptans and other sulphur compounds removal.
To have a good running of this layer below, it is necessary to have a very good water content
monitoring. If water reach this layer, sulphur compounds yet adsorbed by molecular sieves are
displaced by the water, and carried out the tower with the gas. In that case sulphur content
specification of the gas cannot be satisfied.
Other consequence is the deterioration of this layer, due to the water, during the regeneration cycle.
Therefore efficiency of this layer downs.
EQUIPMENT CHARACTERISTICS
1. INLET SEPARATOR
A separator is absolutely necessary to protect the desiccant from impurities such as free water, salt
water, compressor oils, adsorption oil, liquid hydrocarbons, paraffins, corrosion inhibitors, glycol,
amines, pipelines rouges (rust), iron sulfide, iron oxide, frac sands, drilling muds, pipeline scale,
element sulphur, etc... Water and other free liquids will "hammer" the desiccant and cause breaking
and powdering. Non-volatile liquids coat the desiccant and/or block pores, thus reducing capacity.
Solids can plug the bed, and the resulting increased pressure drop can crush the desiccant particles.
The separator should be large enough to handle the most demanding conditions and should have
adequate surge capacity for free liquids and solids.
A high liquid level alarm and a high liquid level shutdown are desirable.
A filter-type separator or coalescer should be used when downstream of an amine unit or compressor.
All droplets larger than 10 µm and 99 % of droplets 0.5 to 10 µm should be removed.
2. ADSORPTION TOWER
As shown in figure VII-D2, the adsorption tower consists of a bed support, gas stream distributors at
both ends, adsorbent loading and removal connections, and a sample/moisture probe. The bed
support must withstand both dead load (weight of desiccant) and live load (flowing pressure drop).
One type of bed support is a stainless steel or monel screen (with openings 10 meshes smaller than
the desiccant particles) supported horizontally by I-beams and a welded ring. The screen should be
securely fastened while allowing for thermal expansion and contraction.
The annular space between screen and vessel wall should be sealed to prevent desiccant loss.
Bed support balls normally consist of a 2 to 3 in layer of ¼ in. balls on top of a 2 to 3 in. lower layer of
½ in. balls.
At the tower top, the inlet gas should be introduced radially at low velocity. A screen-wrapped slotted
pipe or perforated basket is recommended.
Also at the top, the desiccant bed should be protected by a 4 to 6 in. layer of ½ to 2 in. balls resting on
a retainer screen with ½ in. openings. This improves distribution of the inlet gas and prevents
desiccant damage due to swirling.
3. REGENERATION HEATER
Any type of heating (hot oil, steam, furnaces, gas turbine exhaust gases) is acceptable. Under-sizing
the heater results in incomplete regeneration and thus reduces the performance of the entire unit.
4. REGENERATION COOLER
While water can be used, ambient air is generally used to cool the regeneration stream (temperature
approach shall be optimised but it shall not be smaller than 10°C for air coolers. See Total General
Specification GS ECP 103).
5. REGENERATION SEPARATOR
6. SWITCHING VALVES
Good quality valves will minimize operating problems. The most difficult service occurs where the
valves "see" hot (315°C) regeneration gas on one side and ambient (35°C) inlet gas on the other.
Usually three-way valves have more problems than two-way valves. Because low leakage is
mandatory, ball valves with metal seats are recommended.
7. PIPING
Regeneration piping is subjected to severe temperature cycle service. Follow ANSI B 31.3 Piping
Code when designing expansion loops and anchors (fixed and "floating").
Insulate any hot piping for personnel protection and heat conservation.
Dry gas filters (cartridge type) are installed downstream the dehydration towers to eliminate the
molecular sieve powder generated by the molecular sieve erosion produced by the gas flow through
the molecular sieve bed.
These filters must be correctly sized and operated to prevent the plugging of the heat exchangers,
installed downstream, by the molecular sieve powder or the filter material due to cartridge destruction.
(1 µ m filters are frequently installed).
The detailed design of solid bed towers should be done to desiccant vendors (e.g. Grace Davison,
Union Carbide, Zeochem, CECA). The general "rules of thumb" presented in this chapter can be used
for preliminary design, or to check some characteristics of a vendor's proposal or a running of an
installation.
• Utilities available :
Electricity,
Instrumentation air.
2. CALCULATION PROCEDURE
1st Step: Determine the gas characteristics at the adsorber tower inlet.
∆P
= Bµvs + CρvS
2
∆P
- (Bµ ) + (Bµ )2 + 4Cρ
v = L
s 2Cρ
where :
Particle type B C
∆P
For a first estimation of vs, adopt = 8.5 kPa / m
L
5th Step: Calculate the total water load per cycle per tower.
The amount of water to be removed from the gas, per cycle, per tower, is given by the
following equation:
M = WQT
H2 O i
where :
MH2O : total water load per cycle per tower, (kg),
Wi : water vapour content of inlet gas, (kg/106 Sm3),
Q : standard gas flow rate per adsorbing tower, (106 Sm3/hr),
T : cycle time, (hr).
Note: It is a good practice to adopt for water content of inlet gas, leaving an amine
sweetening unit, the maximum water-vapour content of the inlet gas multiplied by 1.1 to
take into account gas flow fluctuations and entrainment of small water droplets.
6th Step: Find the total mass of desiccant per tower MDES and the bed height L
a) Quick estimation
For a quick estimation of mass of desiccant per tower previous values can be
adopted.
In that case:
MH2O
M DES =
weight water/wei ght bed
4M DES
Bed height: L=
πD 2ρ
Where :
L : bed height, (m),
MDES : total mass of desiccant per tower, (kg),
D : bed diameter, (m),
ρ : desiccant bulk density (kg/m3):
For mol sieves, GPSA engineering data book propose a more precise estimation
by method as follows:
During the adsorption cycle, the bed can be thought as operating with three zones.
The top zone is called the saturation zone. The molecular sieves in this zone are in
equilibrium with the wet inlet gas. The middle or mass transfer zone (MTS) is
where the vapour content of the gas is reduced from saturation to < 1 ppm. The
bottom zone is unused sieve. If the bed operates too long, the mass transfer zone
begins to move out the bottom of the bed causing a "breakthrough".
Unfortunately, both the water capacity and the rate at which the molecular sieves
adsorb water change as the molecular sieves age. The object of the design is to
install enough so that three to five years into life of the sieves, the mass transfer
zone will be at the bottom of the bed at the end of the adsorption cycle.
In the saturation zone, the molecular sieves are expected to hold approximately 13
kg of water per 100 kg of sieves (for 3 to 5 year old sieves). This capacity needs to
be adjusted when the gas is not water saturated or the temperature is above 24°C.
See figure VII-D3 for the correction factors.
• The total bed height is the summation of the saturation zone and the mass
transfer zone heights.
L = HS + HMTZ,
L : bed height, (m).
∆P (kPa) = 8.5L(m)
If the pressure drop is higher than 55 kPa adopt a lower value for vs.
If the pressure drop is lower than 30 kPa adopt a higher value for vs.
For these cases do again a calculation run.
To prevent molecular sieve crushing during gas drying cycle (gas flows downward
through the tower) it is recommended to limit the total pressure exerted on the
molecular sieve bottom layer up to a maximum of 70 kPa (10 psi) for 3A, 5A, 13X
molecular sieve type, up to a maximum of 100 kPa (15 psi) for 4A molecular sieve type
(UOP recommendation).
8th Step: Total heat required to desorb the water and heat the sieves and vessel for one
tower.
where :
PD
e =
2S
where :
The mass of the shell and hemispherical heads in carbon steel (density = 7800
kg/m3) may be estimated when, h = 2.5D, by equation as follows:
m = 0.0347 hDe
where:
• Heating requirements to desorbs the water and heat the sieve and vessel per cycle.
Qtr = mCp(Trg-Ti)t
Where:
Qtr : heat load of the regeneration heater (kJ),
m : mass regeneration gas flowrate, (kg/h),
Cp : regeneration gas specific heat, (kJ/(kg.°C)) at average temperature,
t : heating time to reach the regeneration temperature Trg (hr).
• Heat load of the regeneration gas leaving the bed during heating time :
(T - Ti ) dτ
Trg
mC p ∫
Ti
Assuming gas temperature T of gas leaving the bed linear versus time τ
with 0 ≤ τ ≤ t
Trg −Ti
mC p rg (T-Ti )dτ = mC p
T
Ti ∫ 2
t
Trg −Ti
( )
mC p Trg - Ti t = Q hr + mC p t
2
Trg - Ti
Rearrangement gives: mCp t = Qhr and Qtr = 2 Qhr
2
Where: Qhr = total heat required to desorb water, heat the sieve, heat the steel vessel.
• Conclusion: For the entire regeneration cycle, only about ½ of the heat put into the
regeneration gas is utilized.
The heating time is usually 1/2 to 5/8 of the total regeneration time which must include
a cooling period. For 8 hours adsorption cycles, the regeneration normally consists of
4 ½ hours of heating, 3 hours of cooling and ½ hour for stand-by and switching.
For longer cycles, the heating time can be lengthened as long as a minimum pressure
2.3 kPa/m is maintained.
2.75 (Q w + Q si + Q st )
Q gh =
t
where :
In this equation, a safety factor of 25 % is included to take into account the heat
losses and the non-uniform flow through the tower and other equipments.
Coefficient 2.75 is equal to 2 + 2 x 25% times the factor 1.1 to take account of heat
losses through the tower.
Q gh
R g (kg/hr) =
(
C p Trg - Ti )
where :
300
Tpc = 214 K; Tpr = = 1.4 Z= 0.83
214
ρ=
( )
(65.9 ) 10 5 (21.04 ) = 67 kg/m 3
(0.83 )(8314.5)(300 )
∆P
• Extrudate : 1/8" ; B = 5.36 ; C = 0.00189 ; = 8.5 kPa/m.
L
• Allowable superficial velocity :
ρs =
(21.04 ) (10 5 ) = 0.890 kg/m 3
(0.987 )(8 314.5)(288 )
D = 145.67
(
(3 434) 10 - 6 )
= 3.02 m
7.97
Value indicated in the FLUOR Process Flow Diagram (Feed gas dehydration):
Feed Gas dehydrator inside diameter: 3 048 mm.
MH2O =
(0.627) (6.204) 10 3 (8) ( )
= 1 296.6kg
24
• Bed height :
4 (16207)
L= = 3.535 m
π(3.02) 2 (640)
1 296.6
M sz = = 10 177kg
0.13 × 1.0 × 0.98
4 (10177)
HS = = 2.220 m
π (3.02) 2 (640)
Value indicated in the FLUOR Process Flow Diagram (Feed gas dehydration):
7 620 mm T.T.
πD 2 π
M DES = Lρ = (3.83) 2 (3.8)(640) = 17 558 kg
4 4
8th Step: Total heat required to desorb the water and heat the sieve and vessel for one
tower.
• Heating requirements to desorb the water and heat the sieve and vessel per cycle :
Q gh =
2.75 (Q w + Q si + Q st )
=
2.75 (5.432 + 4.618 + 10.320) 10 6 ( ) kJ
t 4.5
= 12.448 x106 kJ/hr
= 2.973 x106 kcal/hr
Value indicated in the FLUOR Process Flow Diagram (Feed gas dehydration) :
( )
4.16 10 6 kcal/hr.
This value is 40 % higher than the calculated required minimum duty. This is a safe
value for a heater design.
R g (kg/hr) =
Q gh
=
( )
12.448 10 6 kJ/hr
= 20 445 kg/hr
(C p ) (Trg - Ti ) 2.315 (290 - 27)
where :
Cp = 2.315 kJ/(kg.°C).
Value indicated in the FLUOR Process Flow Diagram (Process Flow Diagram -
Material Balance): 26 202 kg/hr.
This value is 22 % higher than the calculated required minimum gas flow rate.
This is a safe value for a regeneration gas flow rate design.
Excel data sheet with procedure calculation previously described: in yellow input data, in blue
calculated results.
4th step - Choice of the cycle time: Common choice is between 8 or 12 hours hr 8.0 hr
5th step - Calculation of total water load per cycle per tower
kg 1319
6th step - Calculation of total mass of dessicant per tower M DES
a) Quick estimation
Design molecular sieves capacity (weight water / weigt bed) 0.08
Mass of desiccant per tower kg 16488
Dessicant bulk density (for spherical particles 670 kg/m3, for extruded cylinders=640) kg/m3 640
Bed height L = 4 x MDES / (πD²ρ) m 3.59 m
HEIGHT OF TOWER A free space above and below the bed is needed
h = L + 3.6 m 7.5
h=L+D m 6.9
h = 2.5 D m 7.6
Recommended heigh tower h in metres: h = L + 3.6 for D < 3.6m; h = L + D for D > 3.6
Rule: adopt h > or = 2.5 x D
Adopted heigh of tower h m 7.6
Heat required to desorb the water: QW (kJ) = 4 190 kJ/kg x kg of water on bed kJ 5.527E+06
Heat required to heat the sieves: QSI (kJ) = sieve mass (kg) x 1.00 kJ/kg.°C x (TRG-Ti) kJ 4.659E+06
Approximate thickness of shell e =PxD / (2S (S=allowable stress intensity in barg) mm 92.5
Adopted standard thickness of shell mm 93.0
Calculated external diameter mm 3208
Adopted standard external diameter mm 3200.00
Estimated mass of shell and heads m = 0.0347 hDe kg 78483
Heat required to heat the steel vessel: Qst (kJ) = vessel mass x 0.50 kJ/kg.°C x (TRG-Ti) kJ 1.032E+07
Total heat required for one tower with 10% of heat loss through the tower 2.2557E+07
Contamination of the bed is the most frequent problem encountered and the single most important
cause of premature bed aging. This is usually caused by the entry, and adsorption of materials which
have a residual effect on the adsorbent even after normal regeneration.
This includes all material that comes from compressor lube leakages, from the wells. It enters a bed in
a form of droplets or aerosol. At best, it will be adsorbed by the binder, or in the macropores of the
molecular sieves. It is not completely removed during regeneration, and eventually cracks,
polymerizes, and otherwise goes through any number of reactions which result in "coke" formation. If
its molecules are such that they can enter the micropores of the sieves, the coke is on the actual
adsorption surface, blocking access to those materials the sieves is supposed to adsorb. If the
molecules are excluded from the pores, the "coke" forms on the external surface of the molecular
sieve particles or in the macropores of the particles. There, it blocks diffusion to the actual adsorption
sites, or so impedes molecular diffusion within the macropores that the kinetics of the system are
slowed and the mass transfer zone becomes enormous. In either case, a decrease in dynamic
capacity results and the sieves exhibit premature breakthrough of the "designed for" adsorbate.
These materials, which frequently come from carry over from prior processing steps, behave as heavy
oils. They are quite readily adsorbed in the macropores, or even micropores of some sieves. During
normal regeneration cycles, they decompose and eventually go through various condensation or
polymerization reactions which result in the deposit of heavy coke on the sieve surfaces, macropore
blockage and in severe cases the cementing of molecular sieve particles together to form large
chunks.
In mild cases the result is loss of access to adsorptive surface, and in the case of chunk formation,
channelling of gas flow results. This can lead to very early breakthrough. The prevention of gross
carryover is usually achieved by optimizing the operation of the processing step which introduces the
contaminants to the stream. When this is not possible, the use of filters or even water scrubbers may
be indicated.
3. AMINES
Amines themselves, when adsorbed by the sieves, will decompose during regeneration and
contribute some hydrocarbons to produce coke. In addition, the ammonia formed will chemically
attack the silica in the most commonly used molecular sieve "binder systems" and weaken the
physical structure of the particles. When water is also present, the ammonia may affect an ion
exchange with the cation in the molecular sieves to form an unstable sieve crystal structure. The
displaced cation may actually be washed from the system by subsequent liquid carryover, or it may
migrate to the pore openings and block access to the pores by the normal adsorbates of the system.
The hydrogen form of the sieves being quite unstable will shortly collapse leaving a mass of
amorphous "clay" in place of the molecular sieves.
When amines are used for gas sweetening precautions may be adopted to minimize amine carryover
into molecular sieves.
Many molecular sieve adsorbers are designed to remove sulfur compounds from hydrocarbon
streams. Unfortunately, all sulfur compounds are not designed for easy removal from the sieves.
Heavy mercaptans and other large molecule, high boiling, sulfur compounds, are not efficiently
removed during routine molecular sieve regeneration cycles. As a result, they tend to build in
concentration as a bed ages and produce a capacity reduction much as do the previously mentioned
heavy oils.
They may be acids, amines, phosphates... Their effect on the adsorbent is as varied as their lot. The
end result is loss of capacity.
Some efficient scrubbers or coalescers will get them...
6. PARTICULAR MATTER
In new plants, this type of contaminant may be mill scale, rust or other debris from the construction,
new pipes, or equipment upstream. It is a good idea to blow all this accumulation out of the system
before the final flanging of an adsorber.
7. SALT
Salt usually enters a desiccant bed dissolved in entrained water. Unfortunately, it does not leave
when the water is vaporized and removed from the bed during regeneration. Thus, the solid
accumulates and blocks pores, macropores, and in some extreme cases, all the voids between the
molecular sieve beds. Once sufficient salt has accumulated to reduce adsorbent capacity below the
minimum level required to maintain cycle times, it is usually necessary to replace the adsorbent.
In installations subject to such contamination, the design of inlet scrubbers, separators, coalescers,
etc,... is extremely critical to satisfactory adsorber service and adsorbent life.
8. WATER
Water can be a serious contaminant in an adsorber, either because of the quantity present, or
because of any quantity present. The overload situation occurs when the feed carries more water
than it is anticipated under design conditions. In a closely designed system, the problem is in almost
direct proportion to the "excess". However, even systems that are designed for water saturated feed
will be severely overloaded if some liquid water, mist or droplets, enters the bed. The result will be a
premature breakthrough water, and possibly an incompletely regenerated bed on the next cycle. This
latter is the likely consequence of the regeneration system providing loss energy than is required.
The answer to this "liquid invasion" may be as simple as bigger and better separator-scrubbers ahead
of the adsorber.
FLOATING SCREEN
ADSORBENT
ADSORBENT
3" 3"
3" CERAMIC BALLS 3" CERAMIC BALLS
8 4 4
OR
8 5 3
Figure VII_D5 - INLET and OUTLET REGENERATION GAS TEMPERATURES DURING TYPICAL
SOLID DESICCANT BED REGENERATION CYCLE
DGEP Job : Unit :
Service : Date : Rev.:
MOLECULAR SIEVE DEHYDRATION UNIT CHARACTERISTICS
Unit
1st step - GAS CHARACTERISTICS at adsorber tower inlet
Minimum operating pressure (! the lower, the more conservative! ) bar abs 65.9
Design pressure barg 76.5
Maximum operating temperature (! the higher, the more conservative! ) °C 27.0
10^6 Sm3/day 6.2
Maximum standard gas flowrate
10^6 SCFD 219.515
Gas molecular weight kg/kmol 21.04
Gas density at standard conditions: kg/Sm3 0.89
Gas density at actual conditions: kg/Am3 67.00
Maximum actual gas flowrate 10^6 Am3/hr 0.003
Maximum vapour-water content of inlet gas at saturated conditions (Bukacek correlation) kg/10^3 Sm3 0.580
Water content of inlet gas to be removed at design conditions (safety margin of 10%) kg/10^3 Sm3 0.638
Gas viscosity (1 mPa.s=1 cP) cP 0.0104
DESICCANT & PARTICLES SELECTION - cf. PRODEM VII-D
Type of desiccant Molecular sieves
Particle type: 1/8"(3 mm) or 1/16"(1.5 mm) bead or extrudate 1/8" extrudate
4th step - Choice of the cycle time: Common choice is between 8 or 12 hours hr 8.0 hr
5th step - Calculation of total water load per cycle per tower
kg 1319
6th step - Calculation of total mass of dessicant per tower MDES
a) Quick estimation
Design molecular sieves capacity (weight water / weigt bed) 0.08
Mass of desiccant per tower kg 16488
Dessicant bulk density (for spherical particles 670 kg/m3, for extruded cylinders=640) kg/m3 640
Bed height L = 4 x MDES / (πD²ρ) m 3.59 m
b) GPSA precise estimation
Estimation of the mass of molecular sieves required in the saturation zone:
Correction factor for unsaturated inlet gas Css 1.0
Correction factor for inlet gas temperatuire Ct 0.986
Mass of mole sieves in saturation zone MSZ = MH2O / (0.13 x CSS x Ct) kg 10311
Height of saturation zone: HS = 4 MSZ / (πD²ρ) m 2.25
Coefficient function of mole sieve size z = 0.52 for 1/8" sieves, z = 0.26 for 1/16" sieves 0.52
Length of mass transfer zone: HMTZ = (Vs/11)^0.3 x z m 1.61
TOTAL BED HEIGHT L = HS + HMTZ m 3.86
TOTAL MOLECULAR SIEVE MASS INSTALLED PER TOWER kg 17715
HEIGHT OF TOWER A free space above and below the bed is needed
h = L + 3.6 m 7.5
h=L+D m 6.9
h = 2.5 D m 7.6
Recommended heigh tower h in metres: h = L + 3.6 for D < 3.6m; h = L + D for D > 3.6
Rule: adopt h > or = 2.5 x D
Adopted heigh of tower h m 7.6
Heat required to desorb the water: QW (kJ) = 4 190 kJ/kg x kg of water on bed kJ 5.527E+06
Heat required to heat the sieves: QSI (kJ) = sieve mass (kg) x 1.00 kJ/kg.°C x (TRG-Ti) kJ 4.659E+06
Approximate thickness of shell e =PxD / (2S (S=allowable stress intensity in barg) mm 92.5
Adopted standard thickness of shell mm 93.0
Calculated external diameter mm 3208
Adopted standard external diameter mm 3200.00
Estimated mass of shell and heads m = 0.0347 hDe kg 78483
Heat required to heat the steel vessel: Qst (kJ) = vessel mass x 0.50 kJ/kg.°C x (TRG-Ti) kJ 1.032E+07
Total heat required for one tower with 10% of heat loss through the tower 2.2557E+07