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VIET NAM OIL AND GAS GROUP

PETROVIETNAM UNIVERSITY

Advisor: Le Thanh Thanh, PhD


Presenter: Group 7
MEMBERS

NGUYEN HONG PHUC

DO XUAN QUOC

NGUYEN DUY TAN

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CONTENT

WAX FRACTIONATION
PROCESSES

SOLVENT DEWAXING 03 PROCESS VARIABLES


PROCESSES
02 04
INTRODUCTION SOLVENT RECOVERY
01 05

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01. INTRODUCTION

Purposes and Effects

Feedstocks and Products

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01. INTRODUCTION

Solvent Dewaxing Wax Fractionation


Remove wax from lube Remove oil and low melting
feedstocks and improve of the point waxes to permit
Purposes low temperature properties manufacture of low oil content
waxes with high melting point

✓ Wax content decreases ✓ Oil content of wax decreases


✓ Aromatic content increases ✓ Melting point of wax increases
✓ Pour point decreases
✓ Nitrogen content increases
Effects ✓ API gravity decreases
✓ Sulfur content increases
✓ Viscosity index decreases
✓ Viscosity increases

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01. INTRODUCTION

Solvent Dewaxing and Wax Deoiling Feedstocks and Products

Dewaxing Feedstocks Dewaxing Products


Solvent extracted distillates Solvent neutral oils
Solvent extracted DA oils Bright stocks
Deasphalted (DA) residua Cylinder oils
Hydrocracked distillates Solvent neutral oils
Hydrocracked DA residua Bright stocks and neutrals
Unrefined distillates Paraffin pale oils
Wax deoiling feedstocks Deoiling products

Slack waxes Hard wax and soft wax


Waxy distillates Hard wax and soft wax

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02. SOLVENT DEWAXING PROCESSES

Ketone The Di/Me


Dewaxing Dewaxing
Processes Process

The
The Urea
Propane
Dewaxing
Dewaxing
Processes
Processes

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02. SOLVENT DEWAXING PROCESSES
2.1 Ketone Dewaxing Processes
Solvents used most often are various mixtures of acetone, benzene,
methyl ethyl ketone (MEK), methyl isobutylketone (MIBK), toluene and
other aromatic hydrocarbons.

The solvent mixtures used most often are MEK-tolune and MEK-MIBK.

The most widely used ketone dewaxing processes in use today are:

❖ Texaco Solvent Dewaxing Process

❖ The Exxon Dilchill TM Process

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02. SOLVENT DEWAXING PROCESSES
Texaco Solvent Dewaxing Process

Feedstocks

Crystallization
(Dilution and Chilling)

Filtration Wax

Dewaxed
Solvent Solvent Recovery
oil

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02. SOLVENT DEWAXING PROCESSES

Figure 01. Process flow diagram of Texaco solvent dewaxing process


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02. SOLVENT DEWAXING PROCESSES
The Exxon Dilchill TM Dewaxing Process
❖ Is a modification of the ketone dewaxing process.

❖ Direct chilling of the feedstock in the crystallizer is accomplished


using a cold-solvent multiple-dilution shock-chilling techniques.

❖ A solvent drying step must be added to remove the last traces of


water from the solvent to prevent the icing of the solvent chillers

❖ Filtration and solvent recovery by multiple effect evaporation are


conducted in the usual manner.

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02. SOLVENT DEWAXING PROCESSES
2.2 The Di/Me Dewaxing Process

Dewaxing of lubricating oil


Dichloroethane (Di) and base stocks and the
methylenedichloride (Me) manufacture of low oil
content waxes

60% of cooling is conducted 40% of cooling is conducted


in scraped-surface double- through using ammonia or
pipe exchangers propane refrigeration

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02. SOLVENT DEWAXING PROCESSES

Figure 02. Process flow diagram of Di/Me solvent dewaxing process


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02. SOLVENT DEWAXING PROCESSES
2.3 The Propane Dewaxing Process

Figure 03. Process flow diagram of the propane solvent dewaxing process
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02. SOLVENT DEWAXING PROCESSES
2.3 The Propane Dewaxing Process

✓Cheap and readily ✓ The dewaxing


Advantages

available differential is higher


than other processes
✓Reduce the adhesion ✓ Difficult to control

Disadvantages
of wax batch chilling

✓Wax cloud points of ✓ Require to obtain


propane dewaxed bright good filtration rate
stocks are lower than
ketone’s ones

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02. SOLVENT DEWAXING PROCESSES
2.3 The Urea Dewaxing Process

Figure 04. Process flow diagram of the urea solvent dewaxing process
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3. WAX FRACTIONATION

I. I The Wax Sweating Process​

The Warm-up Deoiling


Wax II
Processes​
Fractionation
The Wax Recrystallization
III
Processes​

IV The Spray Deoiling Process​

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3. WAX FRACTIONATION

Process Main characteristics

I. The ✓ The oldest process.


Wax ✓ The molten wax is solidified by chilling in large pans
Sweating contained in large ovens.
Process ✓ The wax is slowly heated in these ovens.
✓ This process can be used for the deoiling of the
paraffin (macrocrystalline) wax but cannot be used with
the waxes which contain microcrystalline wax
or petrolatums.

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3. WAX FRACTIONATION

Process Main characteristics


II. The ✓ Always operated in conjunction with the solvent dewaxing
Wam-up processes.
Deoiling
Processe ✓ The slack wax from solvent dewaxing is diluted and mixed
s with warm solvent and filter at a temperature which provides
a hard wax of the desired melting point.

✓ The solvent recovered from the low oil content hard wax,
soft wax and dewaxed oil by distillation is recycled in the
process.

✓ The warm-up deoiling procedure is more cost-effective than


the recrystallization procedure for manufacture of low oil
content waxes because capital and energy requirements are
lower.
✓ The warm-up deoiling procedure was used in parallel with
ketone dewaxing.
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3. WAX FRACTIONATION
Process Main characteristics

III. The ✓ Licensed by Texaco and Unocal, used for all types waxes.
Wax ✓ The filtration of the wax in the third stage is conducted at a
recrystall higher temperature than that used in the first or
ization second dewaxing and repulp filtrations.
processe ✓ The temperature used is selected to adjust wax melting
s
point and penetration.

IV. The ✓ The spray deoiling process is a development


pray of Edeleanu which can be used to deoil macrocrystalline
deoiling wax containing up to 15 weight percent oil.
process ✓ This process like the sweating process is not suitable for
the deoiling of malcrystalline wax.

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04. PROCESS VARIABLES

❖ Process variables have a significant effect on the operation and


economics of the dewaxing process.

Process Variables

01 Feedstock – crude source, viscosity, boiling range

02 Solvent and solvent composition

03 Crystallization – dilution and chilling procedure

04 Filtration – filter operation and number of stages

05 Solvent recovery – type and number of stages

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04. PROCESS VARIABLES

Quality of Feedstock

Crystallization
Filtration
method

Properties

Dilution and chilling Solvent and solvent


Rate composition

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04. PROCESS VARIABLES

4.1 Quality of the Feedstock


Feedstock Parameters
Viscosity Product pour
Boiling range Wax type
Wax content Crude source
Prior processing Handling – mixing

➢ The viscosity and wax content of the feed are the key determinants of
solvent dilution ratio and thus have a profound effect on refrigeration
requirements, filtration rates and size of the solvent recovery facilities.
➢ The boiling range and type of wax are related and can significantly affect
filtration rates.
➢ The wax content is generally related to crude source and will affect the
filtration rates as well as dewaxed oil yield.
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04. PROCESS VARIABLES

4.1 Quality of the Feedstock

Figure 05. Ultimate dewaxed oil yield for a light neutral rafinate

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04. PROCESS VARIABLES

4.2 Crystallization method


The crystallization method has a significant effect on the type and filterability
of the wax crystals formed.

Figure 06. Double dilution – single stage filtration procedure

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04. PROCESS VARIABLES
Scraped-surface double-pipe exchangers

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04. PROCESS VARIABLES

4.3 Solvent and solvent composition

The characteristics of an ideal dewaxing solvent


Low solvent power for wax Non – corrosive to conventional metals
High solvent power for oil Easily recoverable by vaporization
Low freeze point Adaptable to all feedstocks
Low viscosity Low dewaxing differential
Low in cost Good chemical stability
Non – toxic Good thermal stability
Table . Characteristics of an ideal dewaxing solvent
➢ Although no single solvent meets above criteria, mixtures of ketone and
aromatic solvents most nearly meet these requirements.

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04. PROCESS VARIABLES

4.3.1 Determination of Solvent Composition

Figure 07. Miscibility diagram of filtrate in toluene/MEK mixtures

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04. PROCESS VARIABLES

4.3.2 Effect of Solvent Composition on Dewaxing Differential

Figure 08. Effect of Solvent Composition on Dewaxing Differential


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04. PROCESS VARIABLES

4.4 Dilution and Chilling Rate


❖ Effect of Dilution Ratio on Filtration Rate

Figure 09. Effect of dilution ratio on filtration rate


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04. PROCESS VARIABLES

4.4 Dilution and Chilling Rate


❖ Effect of Dilution Ratio on Viscosity and Liquid-Solids Ratio
A high viscosity or low liquid-solids ratio may result in high pressure drop
and poor filtration as well as high oil content wax.
Use of high dilution ratios can lead to low viscosity which will result in
poor filtration rates and excessive use of energy for refrigeration and
solvent recovery.
❖ Dilution Procedures
Single dilution – single stage filtration
Double dilution – single stage filtration
Double dilution – two stage filtration
Multiple dilution – single stage filtration
Incremental dilution – two stage filtration

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04. PROCESS VARIABLES

4.4 Dilution and Chilling Rate


❖ Dilution Procedures

Figure 10. Double dilution – two stage filtration procedure

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04. PROCESS VARIABLES

4.5 Filtration
❖ Filtration Variables

Filtration Variables

Filters Filter cloth


Operational mode Filter washing method
Filter speed Filtrate recycle rate
Vacuum (pressure differential) Wax recycle rate
Wash ratio Cake thickness

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04. PROCESS VARIABLES

4.5 Filtration

Figure 11. Pictorial presentation of filter time

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04. PROCESS VARIABLES

4.5 Filtration
❖ Continuous Rotary Vacuum Filter

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04. PROCESS VARIABLES
❖ Continuous Rotary Filter

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05.SOLVENT RECOVERY

5.1 Introduction:
Multiple Effect Evaporation : The number of stages used for
evaporation of the solvent has a significant effect on the energy costs
for these processes.

Inert Gas Stripping : Using inert gas in place of steam for stripping
the last traces of solvent from the dewaxed oil and waxes.

Energy requirements reduced Dilution ratios reduced

Dewaxed oil yield increased Solvent losses reduced

Dewaxing differential decrease Maintenance costs reduced

Table 5.1 - Benefits from Use of Inert Gas Stripping

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05.SOLVENT RECOVERY
5.2 The effect of the number of stages on multistage evaporation :
SIMPLE EFFECTCT:

1. Solvent is vaporized at one pressure level.


2. Energy is wasted in condensation; it is not recovered.
DOUBLE EFFECT:

1. Solvent is vaporized at two pressure levels.


2. One-half of the solvent is vaporized at each pressure level.
3. Condensing vapors are used to operate the first evaporator.
4. Energy requirements are reduced by 45 to 50 percent.
TRIPLE EFFECTCT:

1. Solvent is vaporized at three pressure levels.


2. One-third of the solvent is removed at each pressure level.
3. Condensing vapors are used to operate the first two stages.
4. Energy requirements are reduced by an additional 30-33 percent.
5. Energy requirements are 30 to 33 percent of single effect.

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REFERENCES
❖Lubricant Base Oil and Wax Processing - Avilino Sequeira, Marcel
Dekker

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