CHAPTER 1

INTRODUCTION

1. INTRODUCTION
The constant demand for products such as liquid fuels is the main driving force behind the
petroleum industry. Indeed, fuel products, for example, gasoline, kerosene, and diesel fuel, are
the prime products of the current era. In addition, other products, such as lubricating oils, waxes,
and asphalt, have also added to the popularity of petroleum as an important resource. Petroleum
products are the basic materials used for the manufacture of synthetic fibers for clothing and in
plastics, paints, fertilizers, insecticides, soaps, and synthetic rubber. In fact, the use of petroleum
as a source of raw material in manufacturing is central to the functioning of modern industry
Base oil is the base stock or blend of base stocks used in American Petroleum Institute (API)licensed oil and a base stock slate is a product line of base stocks that have different viscosities
but are in the same base stock grouping and are from the same manufacturer. Base oil (the raw
material for lubricants) is the name given to lubrication grade oils initially produced from
refining crude oil (mineral base oil) or through chemical synthesis (synthetic base oil). Base oil is
typically defined as oil with a boiling point range between 300C (550F) and 565C (1050F),
consisting of hydrocarbons with 18 to 40 carbon atoms. This oil can be either paraffinic or
naphthenic in nature depending on the chemical structure of the constituent molecules. Like
many petroleum products, there are no longer many (if any) processes that are responsible for the
direct manufacture of base oil. The base oil is typically a blend of products from several streams
to which additives are added to adjust the properties to meet specifications and desired service
life.

1.1 HISTORY
Lubricating oil manufacture was well established by 1880, and the method depended on whether
the crude petroleum was processed primarily for kerosene or for lubricating oils. Usually, the
crude oil was processed for kerosene, and primary distillation separated the crude into three
fractions, naphtha, kerosene, and residuum. To Manufacture of Lubricating Oil WE increase the
production of kerosene, the cracking distillation technique was used, and this converted a large
part of the gas oils and lubricating oils into kerosene. The cracking reactions also produced coke
products and asphalt-like materials, which gave the residuum a black color and, hence, it was
2

often referred to as. The rapid evolution of lubricating oil manufacture and use occurred during
the early decades of the twentieth century. Petroleum-based oils first became available and as the
demand for automobiles grew, so did the demand for better lubricants. By 1923, the U.S. Society
of Automotive Engineers (SAE) classified engine oils by viscosity as light, medium, and heavy
lubricating oils. However, engine oil contained no additives and had to be replaced every 800 to
1000 miles. In the 1920s, more lubrication manufacturers started processing base oils to
improve their performance. Three popular processing routes were:

clay treatment

acid treatment

sulfur dioxide treatment

Clay treatment was used to soak up and remove some of the worst undesirable components in the
petroleum base oil. These compounds were usually aromatic and highly polar compounds
containing sulfur and nitrogen. Acid treatment with concentrated sulfuric acid was used to react
with the worst components in the base oil and convert them into a sludge that could be removed.
Although this process effectively cleaned up the oil, it was expensive and the technology is no
longer used in many refineries due to environmental concerns about the acid and the acid sludge
(a thick viscous material that separates when petroleum or petroleum products are treated with
sulfuric acid) formed in the process.
Continuous acid treatment involves the same steps as batch refining with the exception that

the acid and feedstock oil and neutralizing agent are mixed with pumps or static mixers

excess acid and sludge and excess neutralizing agent and soaps are removed using

centrifuges or centrifugal extractors

Water washing is conducted using centrifugal extractors, and

Drying of the oil is conducted in continuous strippers.

The advantages for the continuous process over the batch process are higher yields of oil, lower
chemical consumption, and a reduction in air and water pollution. Sulfur dioxide treatment was a
primitive extraction process to remove the worst components in the lubricating oil using a
3

recyclable solvent which, unfortunately, was highly toxic. Although it also has been virtually
phased out, it was a useful stepping stone to conventional solvent extraction. Currently, catalytic
de-waxing and solvent de-waxing are processes commonly in use, older technologies include
cold settling, pressure filtration, and centrifuge de-waxing .
1.2 Used Lube Oil Re Refining Processes

Re-refining removes all the contaminants from used lube oil to recover base lube oil

product. During the last years many factors have obliged rerefiners to look for alternative Rerefining process, such as:

Increased use of additive packages in the formulation of finished lube oil and by

consequence higher level of contaminants in the used oil.

Increased amount of thermal degradation products due to longer mileage of the

lubricants.

Pollution problems related to the disposal of acid sludges and spent clay from the

traditional acid/clay re-refining.

Among the available today processes, STP Re-refining offers a low energy high yield operation,
high quality products and absence of noxious wastes or by products
1.3 STP Re-refining Process

High flexibility towards feedstock quality and composition

High process yield with recovery more than 72%.

High separation selectivity, removal of contaminants and production of high quality base

oils.

Low energy and low utility consumption.

High on stream efficiency without corrosion, fouling, coking.

Environment safeguarding operation.

Management of all odorous compounds to eliminate malodorous and toxic emissions.

Capital investment and operating cost highly competitive.

Re-refining process removes all the contaminants from the used lube oil and recovers a distillate
product as high quality base oil either API Group I by chemical finishing or API Group II by
hydro finishing. It does not release harmful or pollutant wastes to be disposed and is therefore
environment friend. Process water sent to treatment before disposal and process off gas sent to
thermal oxidizer for combustion and destruction according to environmental law and regulations.
1.4 DEMAND AND SUPPLY DATA
The generation of Waste Oils in some of the major regions/countries of the world is reported
as under.
(a) United States
The demand for lubricants was forecast to expand 1.3 percent annually to 7.66 MMT in
2014. However, with the present sluggishness in market, this may not be realized.
(b) European Union
Waste oil generated in selected European countries (Collectable and collected portions of
the lube oils in EU) has been reported by U. S. Department of Energy. According to EC
resources about 5 MMT base oils are consumed in Europe annually, automotive and
Industrial sectors accounting for 65% and 35% respectively.
(c) Asia
Asian region is the largest lube oil market with 30 % of the global demand; automotive
grades have largest segment. The EPA reports that used motor oil alone accounts for 0.67
MMT of waste oil per year. Used motor oil can be recycled to create virgin lubricating oil at a
much more efficient rate than production from crude oil, claims the EPA.
The Lube oil growth potential 2005-10 for Asian countries was projected to be in the range of
0.5% to 4.8%, with Japan at the lowest level with 0.5% and China at 4.8% followed by India
at 4.6%. Also, in Group II base oils, Asia is moving to Group II / II+. Asias strong lube oil
demand growth is driven by China. Strong growth rates were reflected in projections for
2010, where lube demand in China were estimated to reach 5.5 MMT which was close to 40
% of the Asian lube market.
5

Economic growth has led to grassroots refining investments in Asia. Many blenders in China
used Group II / III base oils initially because of better regional availability. Higher quality
requirements for automotive lubricants in these markets are driven by original equipment
manufacturers for Japanese/US and European automotive brands. India is also a large base
oils market - albeit with slightly different characteristics to the Chinese market. Nearly a third
of Indian base oils demand comes from specialty oils, such as white oil, transformer oils and
petroleum jelly. This makes India a big market for Group II/III oils, particularly of South
Korean origin.
China remains the engine of growth in the Asian base oils market. The burgeoning Chinese
car sales overtaking that of the US has boosted Chinese base oil demand for automotive
lubricants, which are estimated to account for over 50% of base oils consumption.
Additionally, the impressive industrial production recovery in China in 2009 has kept growth
in industrial lubes strong. Automotive and marine applications in India are lesser than in
China. The regional sales of automotive lubes in the total base oils demand, however, are
estimated to be 40%. This means that there will be a big scope for Waste Oils recycling
facilities in Asia, too.
(d) Latin America
Brazil consumed more than 1.122 MMT of base oils in 2008. Brazil's largest re-refiner of
used lubricating oils collects more than 50% of the waste lubricants collected under current
environmental standards in the country. Using 15 collection centers located across Brazil
and a fleet of more than 200 trucks, the collection touches 0.106 MMT/year of used
lubricants from service stations, oil change centers, car repair shops and industries.
Mexico produced about 0.247 MMT of base oils in 2008, supplying about 40% of Mexican
demand. The remainder was imported totaling to approx. 0.605 MMT per annum. Assuming
that only 50% of virgin lube oil is collectible as used oil out of which only around 70% is
actually collected, the amount of collected used oil in Mexico can be estimated to be 0.210
MMT per annum. Argentina's lube market is 0.350 MMT per year. Venezuela also consumes
about 0.350
MMT / year of base oils. For these two countries, the amount of collected used oil can be
estimated by the same process used for Mexico above, giving an estimate of approx.
0.122MMT per annum each.
6

(e) Australia:
Around 0.45 MMT of lubricating oil is sold in Australia each year. While some engines, such
as two-stroke lawn mower engines burn oil completely, others like motor vehicle engines and
machinery produce large volumes of waste oil that can be reclaimed and reused. Industry
and the community generate at least 0.225 MMT of waste oil in Australia each year.
Supported by the Australian Government's Product Stewardship for Oil Program, Australia
recycled approximately 0.194 MMT of their waste oil in 200405. Even though this rate is
high, 0.05 to 0.09 MMT of waste oil remains unaccounted for. During 2008-09 about 0.27
MMT of waste oil was generated by industry and the community and was available for
recycling but about 0.24 MMT of waste oil only was collected and recycled in.
#Researchwikies, Lubricants Marketing Research ( http://researchwikis.com/Lubricants_Marketing_Research, 21.06.2011)
# Freedonia Industry Study. World Lubricants, Industry study with forecasts for 2012 to 2017, Study #2454, February 2009

(f) New Zealand :

Used oil is the single largest non-watery liquid waste stream in New Zealand. An estimated
26,460 MT are generated each year. (Approximately 52,920 MT of lubricating oil are sold
each year. About 50% is leaked, burned or otherwise lost during use.)
Used oil recovery programmes have been in place for some years. The major oil companies
operate nationwide collection networks and supply waste oil to Milburn, New Zealand's
Westport cement kiln, where it is burned at high temperatures. The burning of waste oil in
high temperature kilns is good practice environmentally because it deals effectively with
contaminants. In some areas, local operators collect oil for low temperature burners (which
often do not require resource consents), burning in asphalt plants and road oiling. An
unknown but possibly small quantity of waste oil is land filled or dumped in the environment.
(g) South Africa:
An estimated 0,106 MT of waste oil is generated in South Africa in a year. In 2008,
successful recovery of over 70% of waste oil was reported.
(h) Turkey
Turkey generates around 0.32 MMT of Waste Oils per year. Highest generators are trucks
and buses due to their high share in transportation and high engine oil requirement.
Currently, most waste lubricating oils are recycled for use as heating fuels rather than being
7

converted back into base oil that can be sold back into the lubricants industry.
Recovery to base oil is energy intensive and so is not necessarily the best option. However,
concerns over depleting oil reserves, ever increasing carbon emissions and climate change,
are now driving re-assessment of best practice in waste oil industry.
(i) Nigeria25
Nigeria imported a total of 0.332 MMT per annum of base oils (year 2004) into the country.
Assuming that at least 80% of these base oils are blended into different grades of virgin oils,
the virgin oil market is estimated at about 0.260 MMT per annum. Assuming that used oil
generation could be estimated at 50% of virgin oil while the collectible used oil could
be as low as 30%, the volume of used oils in Nigeria is estimated at about 0.130 MMT. Thus,
collected oil could be is as low as 0.078 MMT for re-processing or re-refining.
(Researchwikies, Lubricants Marketing Research ( http://researchwikis.com/Lubricants_Marketing_Research, 21.06.2011)
# Freedonia Industry Study. World Lubricants, Industry study with forecasts for 2012 to 2017, Study #2454, February 2009)

CHAPTER 2
LITERATURE REVIEW

CHAPTER 2 LITERATURE REVIEW

2.1 MEINKEN PROCESS: A Standard Process Involving Sulphuric Acid and Clay
Considered for a long time as the standard process, it remains the most globally applied.
However, its application is on the decline, and is even prohibited in industrialized countries,
for ecological reasons.
2.1.1Process description
After a coarse filtration to eliminate particles, for example, >3 mm, the oil is processed
as follows:
2.1.1.1 Dehydration
Dehydration is almost always the first step. The temperature is of the order of 160-180Cat
atmospheric pressure. Heat is supplied by steam or heated fluid through a heat exchanger. The
dehydration column is in two sections: in the lower section, oil is pumped at a high flow rate to
avoid formation of deposits and oil cracking by ensuring a good heat transfer. A part of the oil is
injected at the top of the upper section where dehydration is achieved. This column helps to
eliminate variable amounts of water in the lower section and, finally, dehydrate the oil in the
upper section. The lighter fractions removed at the top are used as fuels (fig. A).
2.1.1.2 Acid treatment and clay adsorption
Dehydrated oil is cooled to about 30C before reacting with sulphuric acid. Settling time is of the
order of 24 h. Decanted oil is mixed with clay before injection into the high temperature vessel,
(high-speed flash boiler), heated at 270C by a heated fluid to avoid superheating of the oil.
During clay treatment, small acid droplets as well as sulphonic acids and oxidized or sulphurized
products resulting from acid action in suspension are coalesced and adsorbed. Diesel and spindle
oils are removed at the top and the oil at the bottom is cooled to a maximum of 120C before
filtration. The pressure in the vessel is 80 mmHg. According to this process, clay consumption is
of the order of 3.5 wt% of the settled oil (fig. B).

10

2.1.2 Waste production

The nature and amount of waste produced by the Meinken process are as follows:
Process water rejected: about 130 kg/t of waste oil.
Gas production (gas recovered in vacuum circuits): about 40 Nm^/t.
Acid sludge: about 170 kg/t.
Used clay (oil retention 100%): 31 kg/t.
Waste water and gas are fed into a furnace heated to 1,000C, which ensures the
notabledestruction of phenols. Acid sludge and used clay are burned in a furnace equipped witha
dust removal system and Hme washing. Storage and elimination of calcium sulphite andsulphate
resulting from the previous treatments must be properly done.Several solutions were proposed.
In Sweden, acid sludge was neutralized with a 50% soda solution, and then channelled to a
sulphate production plant where it was incineratedwith paper mill black liquor. The sodium
sulphate formed was transformedinto sodium sulphide used in the manufacture of cellulose in the
firing reactor. Anotherapplication consisted of introducing acid sludge into pyrite roasting
furnace for theproduction of sulphuric acid. Finally, application in the cement industry is often
mentioned.To conclude, the Meinken process was and remains a widely used process. It is an
optimizedversion of the standard acid and clay process. The acid withdrawal, because ofthe acid
sludge production and the cost of used clay elimination, has led to the installationof a vacuum
tower upstream and the use of catalytic hydrogenation of distillates, andpossibly of deasphalted
vacuum residue in the most complete rerefining scheme[2].

Fig1.1

11

Fig1.2
2.2 ECOHUILE PROCESS
The information reported here results from the different contacts established in the pastwith this
company and also from the data supplied to Ecobilan for a study based on thelife cycle analysis
carried out in 1997-1998 at the request of ADEME. More recent informationis not available.
However, this company has realized an important investmentin the vacuum distillation column
and stopped clay treatment[2].
2.2.1 History
On Lillebonne's site (Rouen), currently operated by Ecohuile, several companies havebeen active
in the field of regeneration. In the 1960s, the Matthys-Garap collaborationworked on a process,
the essential characteristics of which are described in Section 4.2.The site was then operated by
CBL: the principal shareholders were Burma (34 %),Condat (14 %), Elf (10 %), Total (10 %),
Motul (10 %), and Scori (10 %). In the 1980sthe technical collaboration of CBL with Total and
CEA aimed at developing UF (see the Regelub process - Section 4.12) followed by catalytic
hydrotreatment. This process couldnot be industrially applied and was practically abandoned in
1986, owing to the declines in the price of crude petroleum and the dollar, with a
correspondingly marked decline inthe selling price of rerefined base oils. At the same time, the

12

parafiscal tax on new oil was implemented in order to finance the collection of waste oil. In
1992, after SOPALUNA, IMPERATOR, and UFP closed down, CBL was the only company still
operating apartially obsolete rerefining plant, with a vacuum distillation producing a bottom
residue representing 40 % of the feed to the column. Soon, CBL went bankrupt as well [2].
Then,Lillebonne's site was taken over by a holding company (Financiere 97). In 1994-1995,this
new company proceeded to update the vacuum column to improve the quality of distillates and
reduce the column bottom residue from 40 to 15-20%. In addition, the following technical and
environmental improvements were made:
Prohibition of the use of sulphuric acid, which eliminates the problem of combustionof sludge
containing on average 14 wt% sulphur.
Energy recovery from various effluents (used clay, waste water, and vacuum residueas
supplement) by combustion in a rotating furnace and effluent gas cleaning in electrofilters.
Development of instrumentation and automation of various equipments.
Clay adsorption was banned on 1 January 2001; this simultaneously increased the oilyield and
made the treatment of the corresponding oil waste unnecessary
2.2.2 Process flow sheet (updated in 2001)
A simplified process diagram is shown in 4.3 and includes the following sequences:
Waste oil settling and emulsion treatment.
Mixing with an additive before treatment in the dehydration column (or preflash).
Light hydrocarbon and water elimination (preflash column).
Vacuum distillation feed heated by the rotating furnace effluent coming from the
combustion of wastes[2]

13

Fig 1.3 Simplified production scheme of the Ecohuile plant.

2.3 CHEMICAL ENGINEERING PARTNERS (CEP) - MOHAWK PROCESS
CEP, an affiliate of Evergreen Oil Inc., supplies technology and equipment for the rerefining of
lubricating oils. Mohawk first developed a pre-treatment step. CEP licensed the Mohawk pretreatment step in 1989. Later, CEP and Mohawk collaborated on processes to reduce catalyst
poisons and addressed the problems of short hydrotreatment catalyst life. After the CEP-Mohawk
collaboration ended in 1994-1995,CEP abandoned the Mohawk pre-treatment process and
adopted a simplified approach to address fouling and corrosion problems in rerefining. Efforts
were made by companies to improve regeneration processes; indeed, the direct combustion route
was no longer authorized in the State of California and the province of British Columbia in
14

Canada. Direct combustion of used oil is still possible in the state of California but only in
certain permitted heaters and furnaces, which have been in existence for a long period of time
(old permits). The oil that was burned met a certain standard, calledSB-86, for concentrations of
halogens, metals, and PCBs. It is true that a permit for even the controlled burning of used oil in
California would be very difficult to obtain for a new operation. This situation explains why the
Mohawk process was first operated in these two regions[2].
First version of the Mohawk process

15

The Mohawk Oil Company (MOC) Ltd. of Vancouver, Canada, has been involved inwaste oil
collection and rerefining since 1978. In the oil rerefining, Mohawk researchers had noticed that
some organometallic additives were thermally unstable and formed polymers leading to frequent
plugging and corrosion of equipment, detrimental to reliable operation. Application of a chemical
treatment to the oil, developed by MOC, seemed tosolve such problems well.Its position so
reinforced, MOC licensed the Mohawk process to Evergreen Oil inNewark, CA, USA, and to
Breslube (acquired by Safety Kleen in 1987) near Toronto, Canada. In 1991, the Mohawk plant
in Vancouver and the plants of Evergreen Oil in California and Safety Kleen in Chicago,
produced 18,000, 30,000, and 50,000 t of baseoil, respectively. Two-large capacity plants
(80,000-150,000 t/year) were planned in the USA (Evergreen considered building a plant in
Southern California in the early 1990s,but did not actually do so) and Breslube near Toronto.
shows the steps involved in the process. An antideposit agent is added to the oil before preflash.
A second flash under vacuum eliminates diesel oil at the top of the column. To get better product
separation, a TFE is coupled to the vacuum distillation unit. Notably, hydrotreatment is applied
to the bulk oil, which requires suitable operating conditions in order to ensure quality for the
different fractions at the final separation. Another way to proceed is to first separate the oil
fractions and to apply a hydrotreatment adjusting the conditions for each fraction. This solution
necessitates, however, the installation of intermediate storage between vacuum distillation and
hydrotreatment. In the following section an improvement of the Mohawk process applied at
Evergreen Oil and consisting of a simplification of the process is described[2].

16

Fig1.4 Mohawk process - first version (including an additional vessel for diesel oil separation2.4

COMPARISON OF VARIOUS RE-REFINING TECHNIQUES

Process /Technology

Waste produced

By-products
utilization

Waste disposal

Acid- Clay re-refining

Residue from
settling & course
filtration of waste
oil, Acid Sludge
and spent clay

Fuel products
( utilized in the
plant itself as
fuel)

Acid activated clay

treating process

Residue from
settling & course
filtration of waste
oil , large quantities
of spent clay
Residue from
settling & course
filtration of waste
oil, Distillation

Fuel products
( utilized in the
plant itself as
fuel)

Major problem is of acid

sludge which is to be
neutralized with lime before
disposal , spent clay is
disposed to brick kilns ,
cement plants
Spent clay ( increased
amount) is disposed to
brick kilns, cement plants

Vacuum distillation
based

Fuel products
( utilized in the
plant itself as
fuel)
17

Distillation residue may be

disposed to cement plants
or mixed with asphalt for
road construction,

residues

Extraction Based

Residue from
settling
& course filtration
of
waste oil,
extraction
residues

Fuel products
( utilized in the
plant itself as
fuel)

Membrane based

Residue from
centrifugation,
concentrate from
membranes

Fuel products
( utilized in the
plant itself as
fuel)

Spent clay disposed to

brick kilns
Regeneration of clays is
also an option and is
started now
Extraction residue to
cement plants / mixed with
asphalt for road
construction,
Spent clay - disposed to
brick kilns or regeneration[5]
Concentrate from the
process may be disposed
to cement plants

2.5 A COMPARATIVE STATEMENT OF VARIOUS GENERIC TECHNOLOGIES FOR

WASTE OIL RECYCLING
1.

Technologies
Acid - Clay Process
(Typical
consumption:
Bentonite 1 to 2%:
However, in some
cases up 5%

Features
Acid-Clay Process for used oil
recycling / reprocessing is Old
and popular.

Drawbacks
Causes Environmental
pollution due to generation
of acid sludge and acid gas
emission. Disposal of acid
sludge is a problem.

This is a Proven technology

worked for many years
worldwide. Can be set-up for
very small
capacity.
Low Capital investment. Makes
it most cost effective for small
and
tiny scale plants.
Non sophisticated, Very simple
process. Simple to operate, No
advanced instruments, No

Causes corrosion of
equipments reducing its life.

18

Gives Lower yield. Due to

loss of oil in sludge as well
as clay since higher dosage
of clay is required.
As most of the government
has adopted
stringent pollution control

skilled operators required.

No acid is required

2.

Acid Activated Clay

Process
It is simple process
Suitable for small capacity plant

regulations, this process is

on its way out.
Very high clay consumption,
low yield, inconsistent
quality.
Disposal of large quantity of
spent clay is an
environmental problem[5].
Suitable only for very small
capacity plants.
Process is dependent on a
particular type of clay which
may not be available from
all the sources[5].

Suitable for high capacity plants. Operates at high

temperature & very high
Vacuum. Require
special/expensive thermic
fluids & heating system.
High cost of heating fluid
and
High operational costs.
Vacuum Distillation
(a)Thin/Wiped Film
Evaporator

Thin film evaporator is capable

Requires high capital
of
investment.
Operating at high vacuum and
normally used for high value and
heat sensitive products.
Does not cause pollution.
Sophisticated Equipments &
Process

Produces good quality Base Oils

3.
Simple pipe furnace, convection
heating at low heat flux by
recirculating flue gases.
19

Plant has to be of a higher

capacity to make it
economically viable.
Require highly skilled &
Operational Maintenance
Staff. As it has very
sophisticated equipments.
Higher Fuel
Cost.
Due to multiple stage of
distillation involving
heating & cooling.

No moving part on process side.

Vacuum Distillation
(b) Pipe Furnace
Vaporizer

No prior removal of gas oil is

required.
Simple instrumentation.

In this process propane is used

as
solvent to remove bitumen,
additives, metals and tar etc.
Solvent is recyclable.

4.

Solvent Extraction
Process

Does not cause pollution.

Produce Good quality Base Oils.

20

Has to operate at higher

pressure ( 10 atm. ) at
ambient temperature (27C )
require high pressure sealing
systems.(making system
expensive and complicated)
Involves operational solvent
losses and highly skilled
operating and maintenance
personnel and system is
required.
Economical only for high
capacity plants.
Propane being very
hazardous, Fire &
explosion hazard is
associated with this
process [5].

2.6 PROCESS DISCRIPTION:

The KTI process (Kinetics Technology International), also known as KTI Relube Technology,
combines vacuum distillation and the hydrogenation treatment to eliminate most of the
polluting substances in used oil.

2.6.1 BASIC STEPS OF THE PROCESS:

Waste oil collected is first fed to the heater where its temperature is raised. After that the stream
is sent to the pre flash column here light hydrocarbons and water is removed. Spent lube oil freed
from sludge-forming impurities and from water and light components is fed to a pre-distillation
column, together with an amount of the bottoms from this pre-distillation column which is
recycled. In the pre-distillation column, under reduced pressure, a gasoil of low grade is
separated by fractionation from the lube oil. The gasoil vapors escape through conduit are
condensed in heat exchanger and are partly recycled as a reflux through conduit , the rest being
discharged via line by means of pump and further used as described below. Spent lube oil freed
from gasoil leaves column as a bottoms stream through conduit, and is pressed through a heat
exchanger by means of a pump, where this stream is preheated. Part of the preheated bottoms
stream is recycled through conduit and mixed with the dry spent lube oil in conduit as previously
described. The remainder of the pre-heated bottoms stream flows through conduit to a wiped film
evaporator. The bottoms stream before arriving in the lm evaporator is mixed with part of the
bottom product coming from the film evaporator which is cycled in conduit by means of pump.
The remainder of the bottom product from the film evaporator is discharged through conduit. A
21

heavy fraction, described below, is mixed with the bottoms stream in conduit which is fed as a
blow-off (drain) stream from a hot-soak via conduit. In the film evaporator, which operates under
vaccum, light lube oil components are evaporated. These vapors escape through conduit and are
condensed in the heat exchanger, the temperature being maintained as high as possible. The
condensate is pumped by pump into a vessel, where this condensate under goes a hot-soak. In
this hot-soak treatment impurities present in the condensate are separated as a heavy fraction;
this heavy fraction is recycled as a blow off (drain) stream via conduit and as previously
described, is mixed with the preheated bottoms stream in conduit. The condensate in vessel from
which impurities have been separated as a heavy fraction, is discharged after the hot-soak via
conduit and pump, is mixed with the gasoil fraction which was formed in the pre distillation
(column 2) and discharged by means of pump as described above, and, after having been mixed
with hydrogen, is passed via conduit and heat exchanger to a reactor filled with hydro generation
catalyst, where the mixture is hydrogenated. The product stream from the hydrogenation reactor
is passed through conduit to a separator in which the residual hydrogen is separated and is
discharged through conduit in order that after increasing the pressure in compressor and mixing
with replenishing (make up) hydrogen which is fed through conduit, it is recycled via conduit
and is mixed with the mixture of hydrocarbons fed through conduit. The hydrogenated
hydrocarbon mixture is discharged from the bottom of the separator and is passed via conduit to
a fractionation column , in which this mixture of hydrocarbons is separated into a diesel oil
fraction which leaves the column at the top, a light lubricating base oil fraction leaving the
column as a middle fraction and a heavy lubricating base oil fraction.

22

Fee
d

Vacuum distillation

Prefash

Condensor

Pum
p

mixer

Heat
Exchanger
Hot
soak
vess
el

TF
E

Reboile
r

Fuel Gas

H2 Makeup

Diesel oil

Compres
sor
High
Pressur
e
Vessel

Light Oil

Heavy Oil

Fig1.5 Process flowsheet of KTI Process

23

Fixed
Bed
Reactor

CHAPTER 3
MATERIAL BALANCE

24

3. MATERIAL BALANCE

Capacity Of Plant = 36,000 TPA

Number Of Days For Which The Plants Operates = 330 Days

Total Waste Lube Oil Refined = 4580 Kg/hr

1. PREFLASH:

Waste Lube Oil

Preflash
Column
Input

Water

Output

200

Light Hcs

Output

100

Lube Oil

Output

5000

Components

(Kg/hr)

%Water

Water+ Light HCs

5300

25

0.037735849

%Light HCs
0.018867925

Waste Lube Oil

=5300 kg/ hr

148.8 OC PREFLASH (I)

=5300 kg/ hr

Fig. 2.1 : Prefash

=5000
Kg/hr

Material balance of Preflash

26

Table 1
:

2. VACUUM DISTILLATION:

VACUUM DISTILLATION

= 410 Kg/hr

27

Lube Oil

Diesel oil (8.2%)

(From Condenser)

= 5046
Kg/hr
Fig 2. 3 : Vacuum
Distillation

Lube Oil (From Reboiler)

28

Lube Oil
(From VDU)

Table 2 : Material Balance of Vacuum Distillation

Vacuum
Distillation Unit

(Kg/hr)

Lube Oil

Lube Oil (To SettlingVessel)

Residues(6.2%)
InputAsphaltenes5046.36
%Diesel=0.082

Overhead (Lube Oil+ Gas Oil)

Output

2460

Gas Oil

Output

410

Reflux Stream (Condenser)

Input

2050

Lube Oil

Output

4636.36

Recycled Stream (Reboiler)

Input

46.36

Components

Reflux Ratio=5:1

3. THIN FILM EVAPORATOR:

= 4590 Kg/hr
Lube Oil (From SettlingVessel)
= 5289 Kg/hr
Thin Film Evaporator

(Kg/hr)

Input

209

Lube Oil

Input

4590

Bottom Stream (TFE)

Input

800

Asphaltenes (Residues)

Output

310

Lube Oil(From TFE)

Output

(Recycled

N FILM EVAPORATOR

Bottom Stream (Impurities)

5289

29

Table 3Stream)
: Material Balance of Thin Film

Fig 2. 4: Thin Film

= 310 Kg/hr
Evaporator

4. SETTLING VESSEL:

Lube Oil
= 4389 Kg/hr

= 4180
Kg/hr
5-30% of
Overhead Product
Settling
Vessel
Components
Lube Oil

180 oC

TFE Input
(lll)

(Kg/hr)
4389
Fig 2.5 : Settling

Bottom stream (Impurities)

Output

Vessel
209

Lube Oil

Output

4180

Bottom stream (Impurities)

= 4180 kg/hr
SETTLING VESSEL (lV)
Table 4: Material Balance of Settling Vessel

Lu

30

5. HYDROFINISHING REACTOR:
Assumptions1) Fixed bed reactor
2) Co/Mo or Co/Al Catalyst
Diesel Oil
(From Settling Vessel)
Lube Oil
Hydrofinishing Reactor
Make
Up Up
H2 H2 + Diesel Oil
Lube Oi
l+ Make
HYDRO FINISHING REACTOR

Lube Oil

Lube Oil

(Kg/hr)

Input

4930

Output

4930

= 4930
kg/hr

Fig 2.6 :
Hydrofinishing
Reactor

=4930
Kg/hr
Table 5: Material Balance of Hydrofinishing Reactor

31

6. HIGH PRESSURE SEPARATOR:

= 4880 Kg/hr

HIGH PRESSURE SEPARATOR

=
300Kg/hr

Fig 2.7 : High

Pressure Separator

Separator

(Kg/hr)

Naphtha

Input

4880

Make Up H2

Output

Naphtha

Output

Components

Table 6 : Material Balance of High

Pressure Separator

32

Naphtha
(From Hydro finishing)

Naphtha

300

=
4580 Kg/hr
(To
Fractionation
Coloum)
4580

Diesel Oil
7. FRACTIONATION COLUMN:

Fuel Gas

Heavy Oil

= 4580
Kg/hr

Components

Naphtha Fraction
Heavy Oil + Light Oil

FRACTIONATION COLUMN

= 40 Kg/hr

Fractionation Column
Input

= 520

= 4020 Kg/hr
(Kg/hr)
4580

Fig 2. 8:

Output

4020
Fractionation Column

Table 7: Material Balance of Fractionation Column

Diesel Oil
Output

520

Output

40

Fuel Gas

33

CHAPTER 4
ENERGY BALANCE

34

4. ENERGY BALANCE
1. HEATER:

Water+
Light HCs
Lube Oil
= (200+100) Kg/hr

Table 8: Energy balance of

Heat duty across Heater

Cp

5300

T
3.096

Tr
148.8

T
25

Q=CpT(Kwatt)

123.8

564.2804

Waste Lube Oil

=5300 kg/ hr

148.8 OC PREFLASH (I)

2. PREFLASH:

=5000
Kg/hr

Table 9 : Energy
Preflash

balance of

Energy Balance across Preflash

Input StreamWasteLube Oil
(Kg/hr)
5300

Cp(KJ.Kg-1.C-1)
3.096

T (oC)
148.8

Tr (oC)
25

T (oC)
123.8

Q=CpT(Kwatt)
564.2804

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

Output StreamWater
(Kg/hr)

35

200
Output StreamLHCs
(Kg/hr)
100

4.32

148.8

25

123.8

8.253333

Cp(KJ.Kg-1.C-1)

T (oC)

Tr (oC)

T (oC)

Q=CpT(Kwatt)

1.931
Cp(KJ.Kg-1.C-1)

(Kg/hr)
5000

3.23

148.8
T(oC)
148.8

36

25
Tr(oC)
25

123.8
T

1.844582
Q=CpT(Kwatt)

123.8

555.3806

37

38

39

40

41

42

3. HEATER:

43

44

Table 10 : Energy Balance of Heater 2

45

Heat Duty Of Heater

2
(Kg/hr)
5000

Cp(KJ.Kg-1.C-1)
3.23

T (oC)
220

46

Tr (oC)
25

T (oC)
195

Q=CpT(Kwatt)
874.7917

47

48

Lube Oil

4. VACUUM DISTILLATION:
Table 11 : Energy Balance of Vacuum Distillation
Energy Balance across Vacuum Distillation Unit:
Input Stream-Waste Lube
Oil
(Kg/hr)

Diesel oil (8.2%)

(From Condenser)
-1 -1
o
Cp(KJ.Kg . C )

T( C)

Tr (oC)

T(oC)

5000

3.23

220

25

195

(Kg/hr)

Cp(KJ.Kg-1.C-1)

T (oC) Tr(oC)

T(oC)

2460

2.497216

220

195

(Kg/hr)

Cp(KJ.Kg-1.C-1)

T (oC) Tr(oC)

T(oC)

2460

3.27

180

25

155

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

2050

3.27

Q=CpT(K
watt)
874.7917

Qv

25

Q=CpT(K
watt)
332.754

Qd
Q=CpT(K
watt)
308.035

Ql

VACUUM DISTILLATION

Qc

180 41025Kg/hr155
=

Q=CpT(K
watt)
288.6229

Qv-Qd-Ql
-263.9039

Qw

= 5046

Kg/hr
(Kg/hr)
4590

Qb

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

6.217

320

25

T(o

Q=CpT(Kwatt)

C)

Qf-Qd-Qw-Qc
-1507.71

49

295

2338.3691

Lube Oil (From Reboiler)

Lube Oil
(From VDU)
= 5599Kg/hr

Table 12 : Energy Balance of Thin Film Evaporator

Energy Balance TFE

Lube Oil (To SettlingVessel)

Asphaltenes Residue (6.2%)

Input

(Kg/hr)

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

5599

4.7385

320

25

295

2174.0567

(Kg/hr)

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4389

4.7835

320

25

295

1720.4057

Output
(Kg/hr)

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

1210

4.2845

180

25

155

223.21055

Output

5.THIN FILM EVAPORATOR:

= 4590 Kg/hr
= 5289 Kg/hr

(Recycled
Stream)

148.8 OC PREFLASH (I)

Lube Oil (From SettlingVessel)

50

= 310 Kg/hr

6. MIXER:

Table 13: Energy balance of Mixer

Heat Duty of Mixer
(Kg/hr
)
5599

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4.7385

314.7

25

289.7

2134.9974

7. SETTLING VESSEL:
Lube Oil
= 4389 Kg/hr

TFE (lll)

= 4180
SETTLING VESSEL (l
Kg/hr
5-30% of
Overhead Product
180 oC

Bottom stream (Impurities)

= 4180 kg/hr

51

Energy Balance Across Hot Soak Vessel

Input stream
(Kg/hr)

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4389

4.7835

180

25

155

903.94198

(Kg/hr)

Cp(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4180

4.7835

180

25

155

860.89713

CP(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

155

37.479215

Output stream

Output stream
(Kg/hr)

Table
14: Energy
Balance of
Settling
209
4.165
180
25
Vessel

8. HEATER

Table 15: Energy balance of Heater 3

Heat Duty Of Heater 3
(Kg/hr) CP(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4389

180

25

155

903.94198

4.7835

52

9. HYDROFINISHING REACTOR:
Diesel Oil
(From Settling Vessel)
Lube Oil
Make Up H2
HYDRO FINISHING REACTOR

Lube Oil

= 4930
kg/hr

=4880
Kg/hr
Table 16: Energy Balance of Hydrofinishing
Reactor
Energy Balance Across Reactor
(Kg/hr)

CP(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4930

4.735

320

25

295

1912.8742

10. HEATER

Table 17 : Energy Balance of Heater 4

Heat Duty of Heater 4
(Kg/hr)

Cp CP(KJ.Kg-1.C-1)

4930

4.735

T(oC
)
320

Tr(oC)

T(oC)

Q=CpT(Kwatt)

25

295

162.10799

53

Make Up H2Make Make Up H2

11. HIGH PRESSURE SEPARATOR:

=
Energy Balance
Across Separator
300Kg/hr
Input stream
(Kg/hr)

CP(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4930

4.735

320

25

295

162.108

Output stream Gas

(Kg/hr)

CP(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

340

14.35

320

25

295

399.8069

Output stream Lube Oil

CP(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4590

4.735

320

25

295

1780.952

= 4880 Kg/hr

HIGH PRESSURE SEPARATOR

(Kg/hr)

Naphtha
(From Hydro finishing)
Naphtha

= 4580 Kg/hr

(To Fractionation
Table 18 : Energy Balance of High
PressureColoum)
Separator

54

Naphtha Fraction
(From HP Separator)
Diesel OilLube Oil
12. FRACTIONATION COLUMN:

Energy Balance Across Fractionating Column

Light OilLight Light =
Oil 40 Kg/hr
Input Stream
4590

4.735

T(oC)

o
Tr(Fuel
C) Gas
T(oC)

Q=CpT(Kwatt)

320

25

1780.952

Heavy Oil

Output Stream Fuel Gas

(Kg/hr)
CP(KJ.Kg-1.C-1)

T(oC)

40

200

2.8

Output Stream Diesel

(Kg/hr)
CP(KJ.Kg-1.C-1)

T( C)

520

200

2.42

Output Stream Heavy Oil

FRACTIONATION COLUMN

= 4580 C (KJ.Kg-1.C-1)
P
Kg/hr

(Kg/hr)

295

=T
520
Tr(oC)
(oC)

Q=CpT(Kwatt)

25

5.444444

175

= 4020 Kg/hr
Tr( C)

T(oC)

Q=CpT(Kwatt)

25

175

61.17222

(Kg/hr)

CP(KJ.Kg-1.C-1)

T(oC)

Tr(oC)

T(oC)

Q=CpT(Kwatt)

4020

2.1

200

25

175

410.375

Table 19: Energy Balance of Fractionation Column

55

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