Term project

Title
Solvent extraction of lube oil stocks

A
TERM PROJECT
ON

SOLVENT EXTRACTION OF LUBE OIL STOCKS

MASTER OF TECHNOLOGY
IN
CHEMICAL ENGINEERING

SUBMITTED BY

RAKESH BISWAS (22CH60R83)

SATHISH KUMAR C (22CH60R84)

VAIBHAV SANJAY SHIRSATH (22CH60R85)

GROUP NO.: 28

MENTOR

PROF. KOUSTUV RAY

DEPARTMENT OF CHEMICAL ENGINEERING

INDIAN INSTITUTE OF TECHNOLOGY KHARAGPUR

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 Term project
Title
Solvent extraction of lube oil stocks

CONTENTS

S. No. Title Page No.

1. Introduction 3
2. Lubricant base stocks 4
3. Base stock selection 5
4. Lube oil manufacturing 6
5. Extraction of lube oil with phenol 7
6. Extraction of lube oil with furfural 11
7. Summary 15
8. Reference 16

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 Term project
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Solvent extraction of lube oil stocks

1. INTRODUCTION
The basic rudimentary for lube oil started with an application, the engine parts (or motor
bearings) moving with stipulated velocity over a period of time, due to the movement friction is
created between the parts and eventually ended up with large amount of heat generation, which
creates an unnecessary damages to the engine parts, for example engine lifetime will decrease
due to the wear and more fuel consumption will arise.

To overcome the friction, make the system to run smoothly and encounter the other problems
new terminology is introduced that is namely lubricants and also called us lubes/lube oil, it is
divided into;

Three basic categories

Mineral oil Synthetic oil
Semi - synthetic

1.1 Mineral oil

Mineral (conventional oil) which is obtained from petroleum crudes and undergoes several
manufacturing, pre and post treatment techniques, since it is conventional form which is widely
used in many industry with respect to the demand and application.

Major fact about the mineral oil is inexpensive compared to other types, because the source in
which it is produced. When the molecules are examined this depicts different structure and size.

Piston
Different size

Cylinder
Figure 1: Arrangement of the molecules in the typical piston cylinder assembly

This project sole depends on the manufacture of the mineral oil by using solvent extraction
technique from lube oil stock.

1.2 Synthetic oil

The same suggest, it is made by artificially like some chemical compounds blended together to
facilitate the lubrication property.

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 Term project
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Solvent extraction of lube oil stocks

This synthetic molecule depicts same almost the size and structure when examined at micro
level, one more term in the synthetic oil is called us synthetic blend and it is obtained from
various synthetic manufacturing process and the molecules are made unique manner.
Since, it is made synthetically which can handle extreme temperature than conventional oil,
because the way it has been built but it is more expensive one.

Piston
Same size

Cylinder
Figure 2: Arrangement of the molecules in the typical piston cylinder assembly

One of the mostly used synthetic oil is polyalphaolefines (PAO), which is predominantly used in
automotive services.

1.3 Semi - synthetic oil

There some distinct type of synthetic oil, which is chosen as a blending agent to blend with
conventional (mineral) oil, which ultimately increase the performance of the oil, that blend oil is
called semi-synthetic oil.

Piston
Different size

Cylinder
Figure 3: Arrangement of the molecules in the typical piston cylinder assembly

It is used for some special applications and the price of this oil is lies between mineral and
synthetic oil.

2. LUBRICATION BASE STOCKS

Lubricant base stocks are classified by the American Petroleum Institute (API) which is
published in API publication 1509 Annex E.
As classified in the publication which is used as a base for selection of wide range of lubricants;

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 Term project
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Solvent extraction of lube oil stocks

API base stock classification

Group Saturates (%) Sulfur (%) Viscosity Index
I
< 90 > 0.03 80 to < 120
Solvent – refined
II
≥ 90 ≤ 0.03 80 to < 120
Hydro processed
III
≥ 90 ≤ 0.03 ≥ 120
Waxy feeds
IV - - -
V - - -

Inference:
Group I, II and III are conventional oil based stocks and derived from petroleum crude.
Synthetic oils are falls under Group IV and some recent advancement is under progress in
it.
The non-conventional synthetic base stocks and mineral based naphthenic oils are comes
under the Group V and it will undergoes a severe reinforcements to enhance the proper
quality.

3. BASE STOCK SELECTION

Paramount entity in lube oil manufacturing is lube oil base stock selection.
The base stock influences the quality of the finished products, which shall be the properties like,
Property Requirement
Should be in the favorable range and also
Viscosity
vary depends upon the application.
Viscosity Index Possibly high.
Flash point As a matter of fact, it should be low.
Pour point Must be low.
Carbon residues For better workability it should be low.
Main aim is to reduce the friction at higher
Oxidation stability temperature as well, therefore it should be
high.

Foam resistance Considerably, it should be high.

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Solvent extraction of lube oil stocks

With all due requirements, the base oil is also selected with profit balance, hence the optimum
base stock shall be adopted for production of premium lube oil.

4. LUBE OIL MANUFACTURING

From the above the statements, lube oil is proficient and indispensable one, especially for
engineering application, lube oil is manufactured by the following techniques,
1. Refining of crude oil.
2. Re – refining of used lubricants.
3. Synthetic manufacturing (blending).
From the major 3 process refining of crude oil is chosen for this project,
4.1 Lube oil from refining of crude oil:
The product obtained from the Vacuum Distillation Unit (VDU) is used as the major feed stock
for the production of lube oil. In general from VDU we get the lube oil stocks but, that are like
initial components which has required further processing to meet the specific requirement.
From that various techniques has been accommodated to produce the specific grade of crude oil,

Grade Specific process

Group I Solvent extraction
Hydrocracking or hydrotreating
Group II Hydrocracking and solvent
extraction
Group III Hydrocracking or hydrotreating

This project specifically signifies the solvent extraction of lube oil from hydrocarbon fractions
and more importantly two methods (solvent extraction) are chosen for this project namely,

Extraction
By using By using
of
Phenol Furfural
Lube oil

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Solvent extraction of lube oil stocks

5. EXTRACTION OF LUBE OIL WITH PHENOL

A common procedure is to extract the hydrocarbon fractions with phenol to obtain the raffinate
(lube oil product) of high viscosity index (75 or greater).

Why does it seems concentrating on higher viscosity index, because desirable lube oil product is
the one which has a high viscosity index, ultimately resist viscosity changes with temperature
and thus it is used in motors, machines, etc.

In addition to having high viscosity index, lube oil product must satisfy the standard of degrees
of haze formation in lube oil, haze will tend to form due to the precipitation of small quantities of
wax crystals within the lube oil product.

In addition to that, It has been standard practice to set cloud point requirement in accordance
with the ASTM cloud point test, the ASTM cloud point being designed to fix the temperature at
which the wax first starts to precipitate within the lube.
Note: ASTM - American Society for Testing and Materials.
5.1 ASTM cloud point test:

The tube is placed in the

Heating the oil > 25 oF Poured the clear oil in a cooling media and
shall approximate cloud standard glass tube to a media is changed
point. height 2 to 24 inch. intermiitently until
achive the goal.

The goal is inspect the

The final temperature of
oil and stop the process
the experiment termed
until distinct cloud or
as ASTM cloud point.
haziness apperas.

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 EXTRACTION OF LUBE OIL
Title
PROCESS FLOW DIAGRAM

Vent gases

Hydro- Isomerization
Zone

Phenol Blend
Raffinate
Light Naphtha

Other fractions H2
Extraction
Zone
Distillation unit
Distillate

Crude

Extract

Heavy Tar Disposal

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Solvent extraction of lube oil stocks

5.2 Distillation unit:

Subjecting crude e.g. Naphthenic crude to fractional distillation where it undergoes fractional
distillation. Light Naphtha constituents are taken out as overhead and heavy tar withdrawn from
bottom. Other fractions like gas oil withdrawn by another lines, and distillate as shown in the
PFD, that is our lube lies under hydrocarbon fraction boiling range of 700 to 1100 oF and having
properties,
1. Viscosity Index = 35 - 45
2. Pour point = - 10 to + 10 oF
3. ASTM cloud point = -5 to +10 oF
4. Haze point = 40 to 50 oF
5.3 Extraction zone:

Now the distillate is passed to the extraction zone where it is contacted with phenol which
is fed from the top of the extraction zone.
Quantity of phenol to feed is 2 volumes of phenol per volume of distillation feed.
Extraction process is operated at 200 oF with 5% of water in phenol.
Raffinate yield from the extraction zone and having viscosity index within the range of
constant haze point. In addition to phenol, the extract will contain single ring and
condensed ring aromatics and sulfur compounds, which is also removed from the distillate
fraction as part of the extraction.
Partially, extract is used to stabilize final high viscosity index product or may be discarded.

5.4 Hydro Isomerization Zone:

Raffinate which is extracted from the extraction zone is passed to Hydro- Isomerization Zone.
Hydro-isomerization zone contains a fixed bed with isomerization catalyst and shall be adapted
to isomerize the raffinate to more branched molecules.
Following catalytic materials shall be adopted:
 Pt, C1 on alumina, or on silica alumina
 Pd, C1 on alumina, or on silica alumina
 Ru, Cion alumina, or on silica alumina
 Rh, CI on alumina, or on silica alumina

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Solvent extraction of lube oil stocks

 Co, MoC4 on alumina

 Neon silica alumina
Especially for this project they had used 0.6 wt. percent platinum and 0.6 wt. percent chlorine on
an alumina base.

Operating conditions:

• Raffinate • Hydrogen
feed rate feed rate

500 standard
1 vol. liquid cubic feet of
feed/vol. of hydrogen per
catalyst/hr barrel of
feed

700 oF 400 psi

• Temperature • Pressure

Inference:
For further reinforcement with accommodating the above all due requirements, proportion of the
extract mixed with the isomerized product and final blend (product) is removed as shown in the
PFD.
Note: PFD - Process Flow Diagram.

5.5 Conclusion:
1. A high viscosity index lubes having good hazing properties and obtained with efficient and
economically attractive manner.
2. Phenol extraction step has tendency to remove the low viscosity index material. It also helps
to remove the sulfur compounds which promote oxidation stability and serve as a wax
solubilizing agent.
3. Blending of the small portion of extract is done for more stability of lube oil product.

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Solvent extraction of lube oil stocks

5.6 Future aspects:

1. The phenol extraction step shall be batch or continuous having single stage or multiple stages
adopted deemed necessary.
2. Various refining steps may be employed, e.g. raffinate of the phenol extraction zone shall be
clay treated prior to isomerization in order to upgrade the feed.

5.7 Future challenges associated with anomalies:

One method of preventing haze formation in lube is to dewax the lube product by using
appropriate solvent and chilling techniques.
However, this process is expensive and economically impractical as applied to low-price
lube oils.
Need to find the another route for inexpensive process capable of producing a high
viscosity index lube having a low haze - forming tendency, particularly with low pour
point.

6. EXTRACTION OF LUBE OIL WITH FURFURAL

In lubricating oil manufacturing process, aromatic content of vacuum distillates is reduced by
solvent extraction. Furfural is one of the most broadly utilized solvent (because its selectivity
towards aromatic compounds is high enough and decreases gradually with expanding
temperature).
For the refining of lube oil stocks to remove undesirable components of lubricating oil, which are
the potential components, lower the quality and it is naturally present in crude oil distillate and
residual stocks.
The main process variables are the quality of the feedstock, temperature, solvent dosage, purity
of the solvent and the quantity of extract recycled to the feed or below the feed in the extraction
device.
6.1 Key parameter:
The temperatures and solvent dosages used are highly dependent on the quality of the crude
source (feedstock) and the quality level of base stocks being produced.

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 EXTRACTION OF LUBE OIL
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PROCESS FLOW DIAGRAM

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6.2 Initiation zone:

The feed oil is introduced at the lower portion of the extraction tower and solvent furfural is
introduced at the top of the tower. The temperature of the streams is regulated to maintain the
bottom temperature between 80-100 oF and top temperature around 110-150 oF. under this
condition, extract and raffinate phases form. The formed extract phase sends to the extract oil
stripping tower.
The distillate from the raffinate oil and extract strippers, comprises a mixture of furfural, oil and
water vapours are condensed and send to a settling chamber or decanter, where condensate
separates into;

Oil
Water
Solvent rich
layers

The solvent-rich layer is continuously withdrawn from the decanter.

6.3 Extraction zone:

Then the solvent-rich stream is sent to furfural extraction tower, where it moves downward
counter currently, the stream of relatively high boiling paraffinic oil introduced at lower portion
of the tower.
The solvent extraction and purification tower is operated with approximately;

Desirable process conditions

Volume 0.5 - 3.0 volumes of paraffinic oil to one volume of recovered furfural
Temperature 90 - 140 oF

At this condition, the phase is accumulating in the bottom of the tower is composed of furfural of
reduced light aromatic (oil content) and lean solvent. Send to solvent accumulator from again
cycled to charge oil extraction tower.

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6.4 Recovery zone:

The extract phase of paraffinic oil from the top of the solvent extraction purification tower,
which is containing some amount of dissolved light hydrocarbon fractions, therefore sent to
water wash tower for water washing to recover any small amount of dissolved furfural.
The water washed oil is send to a stripping tower where extraction of additional furfural-rich
layer is done.
Oil drawn off from the bottom of the tower is a stripped paraffinic (high molecular weight)
fraction which is passed into the surge drum and from again send to a solvent extraction
purification tower.
The overhead product from the stripping tower is send to a condenser where water and light
hydrocarbons are recovered.
6.5 Layer separation and debris removal:
From the bottom of the water wash tower, wash water is combined with water rich layer from
decanter and send to a solvent recovery fractionator.
1. The overhead product from this fractionator is condensed and sent to a decanter to separate
the lower (solvent-rich) layer from the upper (water-rich) layer.
Water layer
Solvent rich - layer

2. The solvent-rich layer is withdrawn and sent to the solvent accumulator.

3. the water-rich layer is again sent to the fractionator and residual water is discharged from
the fractionator,
By considering all the main and reinforcement process, the required quality of lube oil is
obtained from the extraction process as specified.

6.6 Conclusion:
1. A highly efficient process, which eliminates all the process impurities in each and every path
the way it is build.
2. As far as process is concerned it is little time consuming but, it can rest assure the high
quality lube oil.
3. There are multiple extractions, purification and recovery phenomena are revolved around the
process to ensure the finest separation as much as possible.

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6.7 Future aspects:

This extraction process is preliminary process as far as quality and yield is concerned, based on
the need, and shall be operated as batch or continuous.

6.8 Future challenges associated with anomalies:

The packing extraction tower shall be adopted with enriched packing method to evolve
around the multiple media.
Some extraction process enriched with emulsion formation, to counteract further
improvements shall be made to avoid the emulsion.
The process is seems time consuming, there are some possibilities for intensification like
extractive distillation, in which accommodating the future advancements and optimum
recovery shall be obtained as much as possible.

7. SUMMARY

Solvent extraction of lube oil stocks

It shall be done by some established process however; this project

primarily chooses two techniques; Extraction of lube oil with
1. Phenol
2. Furfural

Extraction by phenol: Distillation, Extraction followed by hydro

isomerization has been done to produce the required quality of lube oil as
described earlier.

Extraction by furfural: Distillation, Extraction followed by recovery has

been done to obtain the required quality of lube oil as specified above.

Considering chemical hazard nature and process

feasibility, furfural is non-hazard chemical and
waste water from solvent recovery fractionator is
the only waste effluent from this unit.

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8. REFERENCE

1. Burke. R.F., Summit, and Sutker B. J., Newark,N.J., “Extraction of lube oil with phenol upto
haze point change” , United states patent office, 769,732 (1958).

2. Baudilio Coto, Rafael van Grieken, Jose L. Pena, Juan J. Espada, “A model to predict
physical properties for light lubricating oils and its application to the extraction process by
furfural”, Chemical Engineering Science, 61,4381 – 4392 (2006).

3. Bruce.C, Benedict, Bartlesville, Okla, “Slovent extraction of lubricating oil with phenol”,
United states patent office, 474,270 (1954).

4. L.Tao, L.Qingjing, X.Zhiming, S.Xuewen, Z.Suoqi, “A noval characterization of furfural-

extract oil from vacuum gas oil and its application in solvent extraction process”, Fuel
processing technology, 152, 356 - 366 (2016).

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