Project 2

REPORT ON PETROLEUM REFINING
TITLE:- MANUFACTURING OF GREASE
CERTIFICATE
ALL INDIA SHRI SHIVAJI MEMORIAL

SOCIETY COE PUNE
DEPARTMENT OF CHEMICAL ENGINEERING
This is to certify Seminar report on
MANUFACTURING OF GREASE
Submitted by
KRISHNA NAIR
PARTH SHAH
In the partial fulfillment of Final year syllabus in Chemical
Engineering of Savitribai Phule Pune University during academic year
2016-2017.
Dr M.S.Deshpande
Dr K.R.Jethani
Guide
HOD
Acknowledgement
We find great pleasure in expressing our deep sense of gratitude towards all, who have made it
possible for us to complete this petroleum refining project with success.
We would like to express our deepest and sincerest gratitude to Dr M.S.Deshpande, our
internal guide for her dynamic and valuable guidance and keen interest in our project work. We
are grateful for her constant encouragement in fulfilment of the project work. She provided
valuable knowledge, gave us plenty of her precious time and shared her vast experience in this
field.
This project cannot be considered complete without mention of our Head of department
Dr K.R.Jethani . He have always been supportive and helpful throughout the course of our
final year engineering.
Last but not least; we would also like to thank all staff members and our colleagues for
their valuable suggestion and support.
Krishna Nair
Parth Shah
Index
Chapter no. Title
Page No.
Acknowledgement
Index
Introduction
Grease
Classification of Grease
Lubrication
NLGI Grade
Raw Materials
Base Oil
Thickener
10
Additives
10
Characteristics of Grease
11
Manufacturing Process
13
Testing Methods
17
Advantages and Disadvantages
20
Applications
21
Chemistry of the Process Studied
22
Future upcomings
23
Conclusion
References
INTRODUCTION
Grease:
The word grease is derived from the Latin word Crassus, meaning fat. Early examples of
systematic lubrication with animal fats date back to 1,400 BC, with efforts to reduce friction
on wheel axels. From these very early roots, efforts to reduce friction were dependent on
relatively abundant animal and vegetable-based oils. Mineral oil, as it turns out, is a pretty
good raw material for lubricating surfaces. Taking the lead from the soap manufacturing
industry, which has been robust for centuries, lubricant manufacturers adopted a soap
manufacturing technique called saponification to produce the basis for building stable, useful
petroleum greases. Saponification is the chemical reaction that produces soap, which
becomes the grease thickener. High school chemistry teaches that a mixture of an acid and a
base produces a salt and water. If the acid happens to be an organic or fatty acid, then the
product called is soap. Saponification occurs following the mixing of a fatty acid with an
alkali component. The early fatty acids were produced by cooking animal and vegetable fats
with water to separate glycerine and the inherent fatty acid. The early alkali component for
soap manufacture was derived from soda ash, which comes from the alkali remains of burned
vegetable matter. Owing to the benefit of many early chemical industry developments,
namely large-volume production of organic acids (Stearic acid C 17H35COOH and Benzoic
acid C6H5COOH are both common organic fatty acids used in grease manufacture) and
metallic hydroxides (lithium, aluminium, calcium, sodium and barium hydroxides), grease
manufacturers learned to create specialized soaps into which mineral oils and additives were
introduced to deliver highly specialized product functions. In the manufacturing process the
raw materials for forming the soap, and some portion of the lubricating oil itself, are
combined in a mixing vessel and blended/agitated to initiate the chemical reaction between
the selected metallic thickener and fatty acid. The types and volumes of the materials used
have a dramatic impact on the characteristics of the finished products.
ASTM defines lubricating grease as A solid to semi-solid product consisting of dispersion of
a thickening agent in a liquid lubricant. Greases are used where a mechanism can only be
lubricated infrequently and where a lubricating oil would not stay in position.
Classification of Grease
Grease
Soap Based
Lithium
Calcium
Non-Soap
Alumini
um
Barium
Sodium
OrganoClay
Polyurea
Lubrication:
Lubrication, by a lubricating oil or grease, focuses on the key principle of building an oil film
between two mating surfaces that move relative to each other to separate the surfaces and
prevent them from touching. Achieving this goal reduces friction and can help prevent wear
caused by direct surface to surface contacts. Selecting the right viscosity oil is critical to
preventing surface-to-surface contact. Cooling and debris removal are the other important
benefits provided by a fluid lubricant.
The fluid film in the lubricated area can have a thickness ranging from a few nanometres
(billionths of a meter) to hundreds of microns (millionths of a meter) thick. The most important
property of a lubricant is the viscosity. Loosely defined, the viscosity is the fluid s ability to resist
motion. A high viscosity means that a fluid is thicker and does not flow as easily. For example,
molasses has a much higher viscosity than water, which has a much higher viscosity than air. The
viscosity of oil is usually between that of water and molasses. A
higher viscosity fluid will typically make a thicker film between the moving surfaces and
support greater loads. Like most fluid properties, it depends on the temperature and pressure,
especially temperature.
The thickness of the fluid film determines the lubrication regime, or the type of lubrication.
The basic regimes of fluid film lubrication are:
Hydrodynamic lubrication two surfaces are separated by a fluid film,
Elastohydrodynamic lubrication two surfaces are separated by a very thin fluid film,
Mixed lubrication two surfaces are partly separated, partly in contact, and,
Boundary lubrication two surfaces mostly are in contact with each other even
though a fluid is present.
The fluid viscosity, the load that is carried by the two surfaces and the speed that the two
surfaces move relative to each other combine to determine the thickness of the fluid film.
This, in turn determines the lubrication regime. How these factors all affect the friction losses
and how they correspond to the different regimes is shown on the Stribeck curve. Engineers
to evaluate lubricants, to design bearings and to understand lubrication regimes, use the
Stribeck Curve.
Stribeck Curve:
The Stribeck Curve is a plot of the friction as it relates to viscosity, speed and load. On the
vertical axis is the friction coefficient. The horizontal axis shows a parameter that combines
the other variables: mN/P. In this formula, m is the fluid viscosity, N is the relative speed of
the surfaces, and P is the load on the interface per unit bearing width. The combination of low
speed, low viscosity and high load will produce boundary lubrication. Boundary lubrication is
characterized by little fluid in the interface and large surface contact. We can see on the
Stribeck curve that this results in very high friction.
As the speed and viscosity increase, or the load decreases, the surfaces will begin to separate,
and a fluid film begins to form. The film is still very thin, but acts to support more and more
of the load. Mixed lubrication is the result, and is easily seen on the Stribeck curve as a sharp
drop in friction coefficient. The drop in friction is a result of decreasing surface contact and
more fluid lubrication. The surfaces will continue to separate as the speed or viscosity
increase until there is a full fluid film and no surface contact. The friction coefficient will
reach its minimum and there is a transition to hydrodynamic lubrication. At this point, the
6
load on the interface is entirely supported by the fluid film. There is low friction and no wear
in hydrodynamic lubrication since there is a full fluid film and no solid-solid contact.
You might notice that the Stribeck curve shows the friction increasing in the hydrodynamic
region. This is due to fluid drag (friction produced by the fluid) - higher speed may result in
thicker fluid film, but it also increases the fluid drag on the moving surfaces. Likewise, a
higher viscosity will increase the fluid film thickness, but it will also increase the drag.
Machinery will see boundary lubrication at start-up and shutdown (low speeds and thin film),
before transition to hydrodynamic lubrication at normal operating conditions (high speeds
and thick film). Inspection of the Stribeck curve will show us that a machine will see the most
friction and wear during start-up and shutdown.
Fig 2 Stribeck Curve
The NLGI Grade:

The NLGI consistency number, sometimes referred to as the NLGI grade, expresses a
measure of the relative hardness of a grease used for lubrication as specified by the standard
classification of lubricating grease established by NLGI (National Lubricating Grease
Institute). Reproduced in standard ASTM D-4950 (Standard Classification and Specification
of Automotive Service Greases) and SAE J-310 (Automotive Lubricating Greases).
NLGIs classification is widely used. The NLGI consistency number is also a component of
the code specified in standard ISO-6743-9 Lubricants, Industrial Oils and Related Products
(Class L)
The NLGI classification define nine grades, each associated to a range of ASTM worked
penetration values, measured using the test defined by the standard ASTM D217 cone
penetration of lubricating grease. This involves two test apparatus.
The first apparatus contains of a closed container and a piston like plunger. The face
plunger is perforated to allow a grease to flow from one side of the plunger to the
other as the plunger is worked up and down. The test grease is inserted into the
container and plunger is stroked sixty times while the test apparatus and grease are
o
maintained at 25 C.
Once worked, the grease is placed in a penetration test apparatus this apparatus
consist of container, specially configured cone and dial indicator. The container is
filled with grease and top surface of the grease is smoothed over. The cone is placed is
so that its tip just touches the grease surface and the dial indicator is set to zero at this
position. When the test starts, the weight of the cone will cause it to penetrate it into
the grease. After specific time interval the depth of the penetration is measured.
Fig 3 NLGI Grades

8
RAW MATERIALS
As this definition indicates, there are three components that form lubricating grease. These
components are oil, thickener and additives. The base oil and additive package are the major
components in grease formulations, and as such, exert considerable influence on the
behaviour of the grease. The thickener is often referred to as a sponge that holds the lubricant
(base oil and additives).
Base Oil:
Most greases produced today use mineral oil as their fluid components. These mineral oilbased greases typically provide satisfactory performance in most industrial applications. In
extreme temperature conditions (low or high), grease that utilizes synthetic base oil provide
better stability.
When formulating grease the selection of base fluid is not only about product properties, it is
also about production costs and a significant proportion of the production cost is the amount
of soap required to achieve a certain NLGI grade. The solvating power of the base fluid
affects the amount of soap needed. The following test was performed to determine the
difference in amounts of soap needed between naphthenic (high solvating power) and
paraffinic (lower solvating power) oils. NLGI grade 2 greases were produced using three
naphthenic oils with increasing degrees of refining and a paraffinic oil, all of approximately
the same viscosity. As can be seen, the naphthenic oils with higher solvating power result in a
saving of as much as 25% on soap consumption. This would obviously have a significant
impact on production costs as 25% less soap would be needed to produce the same NLGI
9
grade. Another production cost to consider is energy consumption. When cooking the
grease, the temperature must be raised until the fatty acids are dissolved. Obviously higher
the temperature needed, more is the energy consumed. Higher temperatures also increase the
risk of soap oxidation. The concentration of hydroxystearic acid in each oil was 30 wt%,
which is representative of the typical concentration during grease cooking. It was seen that
the temperature at which the fatty acid dissolves is significantly lower for all the naphthenic
oils than for the paraffinic oil. The lower temperatures needed in greases with naphthenic oils
is due to their higher solvating power. Oils with higher solvating power by definition have a
higher capability of dissolving additives. The additives are dissolved at lower temperatures
and smaller amounts of them are required to achieve the same grades. Due to the higher
solvating power of naphthenic oils they display a higher affinity towards the soap. In
naphthenic-based greases there is a prevalence of physiochemical interaction between the oil
and the soap, as opposed to paraffinic-based greases where most of the oil is physically rather
than physiochemically trapped in the soap structure. This means the naphthenic oil is more
intimately bonded with the soap structure and displays a lower tendency to separate or bleed
from the grease.
Thickener:
The thickener is a material that, in combination with the selected lubricant, will produce the
solid to semi fluid structure. The primary type of thickener used in current grease is metallic
soap. These soaps include lithium, aluminium, clay, Polyurea, sodium and calcium. Lately,
complex thickener-type greases are gaining popularity. They are being selected because of
their high dropping points and excellent load-carrying abilities. Complex greases are made by
combining the conventional metallic soap with a complexing agent. The most widely used
complex grease is lithium based. These are made with a combination of conventional lithium
soap and a low- molecular-weight organic acid as the complexing agent. Non-soap thickeners
are also gaining popularity in special applications such as high-temperature environments.
Smectonite or Bentonite and silica aerogel are examples of thickeners that do not melt at high
temperatures. There is a misconception, however, that even though the thickener may be able
to withstand the high temperatures, the base oil will oxidize quickly at elevated temperatures,
thus requiring a frequent relube interval.
10
Additives:
Additives can play several roles in lubricating grease. These primarily include enhancing the
existing desirable properties, suppressing the existing undesirable properties, and imparting
new properties. The most common additives are oxidation and rust inhibitors, extreme
pressure, antiwear, and friction-reducing agents. In addition to these additives, boundary
lubricants such as molybdenum disulphide or graphite may be suspended in the grease to
reduce friction and wear without adverse chemical reactions to the metal surfaces during
heavy loading and slow speeds.
Different types of additives with their functions are as follows:
FUNCTIONS
TYPE OF ADDITIVE
Antioxidant
Phenols, amines, phosphorous compounds,

sulphur compounds
Extreme pressure and corrosion inhibitor
Tricrysylphosphate, amine phosphate,

Triphenylthiophosphate
Rust Inhibitor
Barium and calcium sulphonates
Corrosion Inhibitor
Benzotrizoles, Mercapto enzothiozoles,

Di-mercaptothiozoles, alkyl benzene
Sulphonates
VI Improvers
Methacrylates
Anti-wear
ZDDP, antimony di-alkyl di-thiophosphate
Water repelling agent
Fatty oils
Tackiness Agent
Polymers (Methacrylate)
Friction Modifiers
MoS2, Graphite
11
Characteristics of Grease
As with oil, grease displays its own set of characteristics that must be considered when being
chosen for an application. The characteristics commonly found on product data sheets include
the following:
Pumpability:
Pumpability is the ability of a grease to be pumped or pushed through a system. More
practically, pumpability is the ease with which pressurized grease can flow through lines,
nozzles and fittings of grease-dispensing systems.
Water Resistance:
This is the ability of grease to withstand the effects of water with no change in its ability to
lubricate. Soap/water lather may suspend the oil in the grease, forming an emulsion that can
wash away or, to a lesser extent, reduce lubricity by diluting and changing grease consistency
and texture.
Consistency:
Grease consistency depends on the type and amount of thickener used and the viscosity of its
base oil. Greases consistency is its resistance to deformation by an applied force. The
measure of consistency is called penetration. Penetration depends on whether the consistency
has been altered by handling or working
Dropping Point:
Dropping point is an indicator of the heat resistance of grease. The dropping point is the
temperature at which grease becomes fluid enough to drip. The dropping point indicates the
upper temperature limit at which grease retains its structure, not the max temperature at which
grease may be used.
Oxidation Stability:
This is the ability of grease to resist a chemical union with oxygen. The reaction of grease
with oxygen produces insoluble gum, sludge and lacquer-like deposits that cause sluggish
operation, increased wear and reduction of clearances.
12
High Temperature Effects:

High temperatures harm greases more than they harm oils. Grease, by its nature, cannot
dissipate heat by convection like circulating oil. Consequently, without the ability to transfer
away heat, excessive temperatures result in accelerated oxidation or even carbonization
where grease hardens or forms a crust. Effective grease lubrication depends on the grease's
consistency. High temperatures induce softening and bleeding, causing grease to flow away
from needed areas. The mineral oil in grease can flash, burn or evaporate at temperatures
greater than 177C
Low Temperature Effects:

If the temperature of grease is lowered enough, it will become so viscous that it can be
classified as hard grease. Pumpability suffers and machinery operation may become
impossible due to torque limitations and power requirements. As a guideline, the base oil's
pour point is considered the low-temperature limit of grease.
13
Manufacturing Process
The heart of the lubricating grease manufacturing process is the Contactor reactor. All
energy input through the mixing impeller is expended within the materials being
mixed and there is virtually no pressure differential between the reactor's inlet and
outlet. The outstanding feature of the reactor is its high turbulent circulation in a
0closed cycle path.
The Contactor reactor is first charged with the specified base oil which is at its storage
temperature. A hinged opening at the top of the reactor is used for charging the active
chemical ingredients used in the grease formula. Once the specified amount of the raw
chemicals is loaded, the charge opening is closed and the reactor is heated.
The high dispersion mixing in the reactor is achieved by the hydraulic head assembly.
The impeller forces frequent changes in the velocity and direction of flow through the
reactor. The oil and chemical ingredients are pulled down through the inside of the
circulation tube via the impeller. Turbulence is established between the stationary
shear vanes and the blades of the impeller, resulting in a zone of high shear and
intense mixing.
As the material passes through the impeller, its velocity is greatly increased. At the
discharge side of the impeller, the stream is impinged against the diffuser vanes. The
direction of the flow is reversed at the bottom of the hydraulic head where the vanes
force an axial turbulent flow as the dispersion passes through the annular space
14
formed by the circulation tube and reactor wall. The liquid then flows over the top of
the circulation tube and back into the impeller.
Once circulation is established, the reactor is heated, typically using a hot oil
heating system. The reactor is equipped with two jackets, an external jacket and an
internal jacket. Heat transfer oil is circulated in both the internal and external
heating jackets. High heat transfer coefficients are achieved by the high
circulation rates across the heating surface. The saponification reaction is
exothermic and the combination of applied heat and reaction heat results in a rapid
temperature rise. The entire contents of the reactor reach a temperature in excess
of 400F (204.4C) in less than an hour. At this temperature, the saponification
reaction is complete.
As the saponification reaction proceeds to completion, water is generated as a

product of the reaction. Pressures in the range of 70-100 psig (482.7-689.5 KPa
gauge) are typical of those used for efficient and complete saponification. This
pressure prevents foaming of the soap concentrate as well as accelerates the
saponification reaction. The reactor pressure is maintained by manually venting or
by automatic controls as the temperature rises.
The next step involves the addition of cooling or quench oil used to reduce the
temperature below the soap crystallization temperature. At this point, the reactor
contents are pumped into a finishing kettle. These are large mixing vessels, typically
either pressure or open atmospheric types. The kettles are equipped with large slow
speed mixing assemblies, whose function is to provide a gentle blending action and
aid in cooling of the semi-finished product. Cooling is typically accomplished by cold
oil circulation in a shell jacket.
When the final amount of finishing oil has been added and the kettle contents are
cooled to an acceptable temperature, additives are typically introduced and
blended into the cooled finished grease. Since many additives are temperature
sensitive, they are added in the cooled kettles rather than in the reactor.
Some greases require milling. Milling (sometimes referred to as homogenizing)

is performed to ensure that the grease product is truly homogeneous. Once the
finished grease passes the quality control tests, it may be sent to packaging.
15
Base Oil
Charging
Fat/Alkali
Charging
Starting of
Reactor
Heating of
Reactor
Base oil cutback
Reactor Wash
Blow in Kettle
Venting
Kettle Cooling
Additives and
Base oil
addition
Homogenizing
/ Milling
Penetrat
ion Test
Filling
General Process Flow
Advantages of Batch Process:
In batch process equipment can be reuse.

Process variables can be subjected to adjustments.
In batch process multi-product operation can be done.
Grease has a demand that changes over time or has seasonal variability. And this type
of variability is well suited to batch manufacturing.
Cost required is less in case of batch process.
16
Testing Methods
Test:- Cone Penetration
The penetration is determined at 25 C by releasing the cone assembly from penetrometer
and allowing the cone to the drop freely in the grease for 5 seconds.
Penetration: - It is the depth in the tenths of millimetre that a standard cone penetrates the
sample under prescribed condition of weigh, time and temperature.
Working:-It is the subjection of lubricating grease to shearing action of standard grease

worker.
Worked penetration: - It is the penetration of grease sample subjected to 60 double

o
strokes in standard grease worker and penetration is done at 25 C.
Unworked penetration: - It is the penetration at 25oC of grease which is transferred in

grease worker cup and levelled with minimum working.
Block penetration: - It is the penetration at 25oC or grease sample that is sufficiently

hard to hold its shape determined on the freshly prepared face of a cube cut from a block of
the grease.
Test:- Method for working stability of grease in presence of water
Method: - The method is intended for the determination of change when subjected to work
in presence of water.
Working: - Grease is filled in cup and exposed to prolonged mechanical working in

presence of water (10% water) and in absence of water and difference in penetration is
determined.
Test:- Dropping Point Test
Method: - This method covers the determination of dropping point of lubrication grease.
This point being the temperature at which first drop of material falls from cup.
17
Working: - Small quantity of grease is taken in drop point and heated slowly to the
temperature at which first drop of the oil comes out from the whole bottom of the test cup.
The temperature at which grease drop falls is noted as the dropping point of the grease.
Test:- Determination Of Heat Stability

Method: The method describes a procedure for the determination of heat stability of
grease by observing the separated out and structure of the grease after test.
Working: - About 10 gm. Grease is heated at 120 C for 1hr and grease is examine
visually for any evidence of oil separation and structure change after 24hrs.
Test:- Determination of Evaporation Test

Method: - This method covers determination of the evaporation loss in lubricating grease.
Working: - The sample weighted in Petri dish and kept for 2hrs. In oven maintained at
105+/- 10C. The loss in mass is calculated as evaporation loss of sample.
Test:- Oxidation Stability

Method: - The method for oxidation stability of lubricating grease bomb method.
Working: - - The sample of grease is oxidized in bomb heated to 99C and fitted with
oxygen at 7.5 bar. Pressure is observed and recorded at started. Then the degree of oxidation
after a given period of time determined by corresponding decrease in oxygen pressure.
Test:- Determination of free acidity and alkalinity of grease

Method: - This method is used for determining free acidity and alkalinity of grease
Working: - Grease is dispersed in hexane 50ml of neutral rectified spirit is added followed by
10ml 0.5N HCl and reflux for 10-15min. Cooled and titrate against standard alkali.
Test:- Copper Corrosion Test

Method: - The test is intended for the determination of corrosive substances in the
lubricating grease oil, fat and additives. As the grease is employed under diversity of
18
conditions it is not possible to specify either temperature or duration of test. It is

o
recommended that temperature be not higher than 20 C below the drop pint of grease.
Working: - Clean and polished copper strip is immersed in the sample which is then
maintain in the specified temperature and duration. The strips are removed, wash with
petroleum sprit and examined for evidence of etching, pitting and discoloration.
Test:- Determination of storage stability of grease

Method: - This method described a procedure for determine the storage stability of grease.
Working: - The consistency, both worked and unworked penetration of material is

determined by cone penetration test. Sample of original material are stored in dark in a
container for six month at 38+ or -3*c. The consistency, both worked and unworked
penetration of the stored sample is then determined.
19
ADVANTAGES OF GREASE LUBRICATION
Better stop-start performance- when the system shuts down, oil drains away while
grease remains in the component
Squeeze film lubrication- under vertical loading condition, grease acts as an elastic
slide provide enhanced lubrication.
Sealing problems- surplus grease acts as an effective sealant.
Contamination- the risk of the contamination products such as food and

pharmaceutical type products is reduced with the use of grease due to resistant to flow
into the products.
Supply of surplus lubrication- the semi-solid nature of the grease enables it to be fed
easily into the space around the working surfaces.
Lubricated On the Run- a machine filled with greasing valves can be relubricated
on the run without shutting down the machine or interrupting operation.
DISADVANTAGES OF GREASE LUBRICATION
Reduced cooling / heat transfer the flow of the oil removes the heat from the point
of generation where it can be removed or dissipate. Grease tends to hold heat in place.
Bearing speed limitation:- the high effective viscosity of grease imposes speed
limitation on bearings to avoid excess of heat generation. This problem is worsened
by greases poor heat transfer properties.
Poorer storage stability grease are less stable than oils when stored under same
condition. To long of storage can lead to separation of base oil and thickener and
altered properties.
Lack of uniformity due to poor predictability of the batch process of grease making
and the added variability associated with thickener, uniformity of the grease tend to be
inferior to that of the oil.
Compatibility the use must be careful about thickener compatibility of grease. In

many cases, the compatibility is poor.
Lower resistance to oxidation - the effects of oxidation products on the stability of the
thickener makes grease more susceptible to oxidation.
Contamination control oil lubricants suspend and transport particle to filter and
allow the particle to settle under the force of gravity. The grease lubricant suspend
particles, continuously subjecting component surfaces to their abrasive effects.
Difficult volume control the difficulty in gauging the proper quantity of grease to
add, especially during relubrication, leads to frequent over and under greasing.
20
APPLICATIONS
General processing industries.

High temperature, pressure and shock load conditions.
Food processing industries.
Mining applications.
Automotive industries.
Defence purpose, pumps, and tanks.
Railways, steel industry, nuclear power plant.
Aircraft landing wheel bearing.
Water pumps.
Building equipment.
Farm machineries.
Ball and roller bearing.
Railway antifriction bearing.
Lubricant for wire ropes and chains.
Lubricant for open gear aircraft industry.
Elevators.
Paper mills
Textile industries.
Steam locomotives.
Drilling machine.
21
CHEMISTRY OF THE PROCESS STUDIED:The manufacturing of grease mainly consist of saponification reaction.
The reaction is carried out between higher fatty acids (such as 12-Hydroxy stearic acid,
Hydrogenated castor oil) and various metal hydroxides (eg. LiOH.H2O , NaOH,
Ca(OH)2....etc.)
Saponification reaction follows first order kinetics.
MOLECULAR FORMULAE: HCO

CH3-(CH2)5-CH(OH)-(CH2)10-COOCH2
CH3-(CH2)5-CH(OH)-(CH2)9-COOCH
12-HSA
CH3-(CH2)5-CH(OH)-(CH2)10-COOH
REACTION
SAPONIFICATION OF HCO
CH3-(CH2)5-CH(OH)-(CH2)9-COOCH
CH3-(CH2)5-CH(OH)-(CH2)10-COOLiCH2OH
CH3-(CH2)5-CH(OH)-(CH2)10-COOLi + CH2OH
+ 3LiOH
HYDROGENATED CASTOR OIL
CH3-(CH2)5-CH(OH)-(CH2)10-COOLi
LITHIUM
HYDROXIDE
CH2OH
LITHIUM SALT OF HCO (SOAP)
GLYCEROL
SAPONIFICATION OF 12-HSA
CH3-(CH2)5-CH(OH)-(CH2)10-COOH + LiOH.H2O
12 HYDROXY STEARIC ACID
CH3-(CH2)5-CH(OH)-CH2)10-COOLi + H2O
LITHIUM
HYDROXIDE MONOHYDRATE
22
LITHIUM STEARATE
WATER
MASS BALANCE OF SERVO GEM RR3 GRADE GREASE

Batch no: - 0047
Reactor: - R-102
Penetration: - 225/230
Kettle: - K-105
RAW MATERIAL REQUIRED FOR CHARGING IS:COMPONENT
QUANTITY(Kg)
BASE OIL 500N
3000
1200
LITHIUM HYDROXIDE
180
MONOHYDRATE
TOTAL
4380
AVERAGE MOLECULAR WEIGHT:COMPONENT
MOLECULAR WEIGHT
12-HAS
309
LIOH
24
LiOH.H2O
SOAP OF 12-HAS
42
306
23
OVERALL MASS BALANCE OVER REACTION DURING

REACTION:-
Now,
INPUT = OUTPUT
12 HSA + LiOH.H2O +BASE OIL = SOAP + VENT
1200 + 180 + 3000 = SOAP + VENT
4380 = SOAP + VENT . (1)
OVERALL MASS BALANCE OVER REACTOR DURING WASHING:-
24
BRIGHT STOCK FOR WASHING = WASHED OIL + VENT

2005 = WASHED OIL + VENT.. (2)
OVERALL MASS BALANCE OVER KETTLE:-
SOAP + WASHED OIL+ ADDITIVES + CORRECTION/CUTBACK OIL = EXHAUST +

OUTPUT (GREASE)
SOAP + WASHED OIL + 40 + 45 + 36 + 510 + 905 = EXHAUST + 7826 (3)
WATER / VOLATILES BALANCE:WATER OF CRYSTALLISATION OF LiOH.H2O

42 Kg LiOH.H2O = 18 Kg of WATER
180 Kg of LiOH.H2O = X Kg of WATER
Hence X = 180 * 18 = 77.142 Kg
42
25
WATER RELEASED DURING REACTION:

I Mole HSA= 1 Mole Water
309 gm HSA =18 gm Water
1200 kg HSA = Y Kg Water
Y=69.90 kg of Water as Steam
MOISTURE CONTENT OF FATTY ACIDS (0.25%):

TOTAL AMOUNT OF FATTY ACID = 1200 Kg
Hence,
TOTAL AMOUNT OF MOISTURE = 1200*0.25/100
= 3 Kg of MOISTURE
VOLATILE AND MOISTURE CONTENT OF BASE OIL:

FOR 1 mg of BASE OIL = 400 ppm of (WATER & VOLITILE)
Hence,
For 6420 Kg of BASE OIL = 6420*400*10-6
= 2.568 Kg of (WATER & VOLITILE)
TOTAL AMOUNT OF WATER RELEASED= 77.142 + 69.90 + 3.0 + 2.568

TOTAL AMOUNT OF WATER RELEASED = 152.61 Kg of water . (4)
WATER BALANCE OVER REACTOR:DURING REACTION:

WATER ADDED + WATER/VOLATILES IN BASE OIL + WATER IN FATTY ACID + WATER
OF CRYSTALISATION + WATER RELEASED DURING REACTION = STEAM VENTED
0 + 3000*400*10-6 + 1200*0.25% + 77.142 + 69.90 = STEAM VENTED
0 + 1.2 + 3.0 + 77.142 + 69.90= STEAM VENTED
151.242 Kg = STEAM VENTED FROM REACTOR . (5)
FROM OBSERVATIONS,
SOAP LOST IN VENT=35 Kg
TOTAL VENT FROM REACTOR= 151.242 + 35 =186.242 Kg
26
Now from equation (1),

4380 = SOAP +VENT FROM REACTOR .. (From 1)
4380 = soap + 186.242
Soap = 4193.75 Kg
DURING WASHING:2005 = WASHED OIL + VENT

Water content of 150 BS = 400ppm
Hence, water in base oil = vent
= 400*10-6*2005
VENT DURING WASHING =0.802 kg. (6)
WATER BALANCE OVER KETTLE:WATER IN SOAP+WATER/VOLATILES IN BASE OIL + WATER IN ADDITIVES = WATER IN
EXHAUST+ WATER IN OUTPUT (GREASE)
0 + (510 + 905)*400*10-6 + 0 = EXHAUST + 0
EXHAUST = 0.566 Kg .. (7)
FROM EQUATIONS (4), (5), (6) & (7),

TOTAL AMOUNT OF WATER RELEASED = STEAM VENTED FROM REACTOR + VENT
DURING WASHING + EXHAUST
152.61 = 151.242 + 0.802 + 0.566
= 152.61 Kg of water
THUS, WATER IS BALANCED.
27
ALKALI BALANCE:Stoichiometric proportion:

1 mole of LiOH.H2O = 1MOLE OF LITHIUM STEARATE
= 1 MOLE OF 12 HSA
309 Kg OF 12 HSA = 42 Kg LiOH.H2O
1200 Kg OF 12 HSA = X Kg LiOH.H2O
X = 163.106 kg of LiOH.H2O
FREE ALKALI CONTENT = 0.15% WT. OF FEED

TOTAL QUANTITY FED = 4380 kg FREE ALKALI CONTENT
= 6.57 kg of LiOH
Hence,
LiOH CONTENT = 6.27*(42/24)
= 11.49 Kg OF FREE ALKALI
TOTAL QTY OF ALKALI REQUIRED = 163.106 + 11.49
TOTAL QTY OF ALKALI REQUIRED (theoretical) =174.603 Kg
PRACTICAL QTY. FED TO REATOR = 180 Kg
EXCESS ALKALI = 180 174.603
EXCESS ALKALI = 5.39 Kg
NOW,
OVERALL BALANCE
TOTAL INPUT = OUTPUT + LOSSES
TOTAL INPUT = 7921
TOTAL OUTPUT = NO. OF BARRELS *182
=
43 *182
7826 Kg
PROCESS LOSS = 7921 - 7826

= 95 Kg
ACTUAL % LOSS = 95*100/7921
= 1.19 %
28
THEORITICAL LOSS = MASS LOST AS STEAM
= 151.242 Kg
THEORITICAL % LOSS = 151.242*100/7921 =
1.90 %
Hence,
DEVIATION = 1.90 - 1.19
DEVIATION = +0.71% (ADVANTAGEOUS)
29

Batch no: - 0075
Reactor: - R-102
Kettle: - K-105
QUANTITY(Kg)
BASE OIL 500N
2800
1200
LITHIUM HYDROXIDE
180
MONOHYDRATE
TOTAL
4180
MOLECULAR WEIGHT
12 HAS
309
LiOH
24
LiOH.H2O
SOAP OF 12 HAS
42
306
30

REACTION:-
Now,
INPUT = OUTPUT
1200 + 180 + 2800 = SOAP + VENT
4180 = SOAP + VENT . (1)
31


OUTPUT (GREASE)
SOAP + WASHED OIL + 45 + 54 + 36 + 500 + 2300 = EXHAUST + 7826 (3)

Hence, X = 180 * 18 = 77.142 Kg
42
32

I Mole HSA= 1 Mole WATER
309 gm HSA =18 gm WATER
1200 kg HSA = Y Kg WATER
Y= 69.90 kg OF WATER AS STEAM

Hence,
= 3.0 Kg of MOISTURE

Hence,
For 6205 Kg of BASE OIL = 6205*400*10-6
= 2.482 Kg of (WATER & VOLITILE)
TOTAL AMOUNT OF WATER RELEASED=77.142+69.90+3.0+2.482


0 + 2800*400*10-6 + 1200*0.25% + 77.142 + 69.90 = STEAM VENTED
0 + 1.12 + 3.0 + 77.142 + 69.90 = STEAM VENTED
FROM OBSERVATIONS,
33

4180 = soap + 186.162
Soap = 3993.83 Kg
DURING WASHING:605 = WASHED OIL + VENT Water

content of 150 BS = 400ppm Hence,
water in base oil = vent
= 400*10-6*605
0 + (500+2300)*400*10-6 + 0 = EXHAUST + 0
EXHAUST = 1.12 Kg .. (7)
FROM EQUATIONS (4), (5), (6) & (7),

152.524 = 151.162 + 0.242 + 1.12
= 152.524 Kg of water
THUS, WATER IS BALANCED.
34

= 1 MOLE OF 12 HSA

= 6.27 kg of LiOH
Hence,
LiOH CONTENT = 6.27*(42/24)
NOW,
OVERALL BALANCE
TOTAL INPUT = 7720 kg
=
42 *182
7644 Kg

= 76 Kg
ACTUAL % LOSS = 76*100/7720
= 0.98 %
35
= 151.162 Kg
1.95 %
Hence,
DEVIATION = 1.95 0.98
DEVIATION = +0.97% (ADVANTAGEOUS)
36

Batch no: - 0088
Reactor: - R-102
Kettle: - K-105
QUANTITY(Kg)
BASE OIL 500N
2810
1200
LITHIUM HYDROXIDE
184
MONOHYDRATE
TOTAL
4194
MOLECULAR WEIGHT
12 HAS
309
LIOH
24
LiOH.H2O
SOAP OF 12 HAS
42
306
37

REACTION:-
Now,
INPUT = OUTPUT
1200 + 184 + 2810 = SOAP + VENT
4194 = SOAP + VENT . (1)
38


OUTPUT (GREASE)
SOAP + WASHED OIL + 45 + 40+ 36 + 510 + 1474 = EXHAUST + 8190 (3)

Hence, X = 184* 18 = 78.85 Kg
42
39

I Mole HSA= 1 Mole Water
309 gm HSA =18 gm Water
1200 kg HSA = Y Kg Water
Y= 69.90 kg of Water as Steam

Hence,
= 3.0 Kg of MOISTURE

Hence,
For 6804 Kg of BASE OIL = 6804*400*10-6
= 2.72 Kg of (WATER & VOLITILE) TOTAL
AMOUNT OF WATER RELEASED=78.85 +69.90 +3.0 + 2.72

0 + 2810*400*10-6 + 1200*0.25% + 78.85 + 69.90 = STEAM VENTED
0 + 1.124 + 3.0 + 78.85 + 69.90 = STEAM VENTED
FROM OBSERVATIONS,
40

4194= soap + 187.87
Soap = 4006.13 Kg
DURING WASHING:2010 = WASHED OIL + VENT

Water content of 150 BS = 400ppm
Hence, water in base oil = vent
= 400*10-6*2010
0 + (510+1474)*400*10-6 + 0 = EXHAUST + 0
EXHAUST = 0.7936 Kg .. (7)
FROM EQUATIONS (4), (5), (6) & (7),

154.79
= 152.87 + 0.804 + 0.7936

=
154.79 Kg of
water THUS,
WATER IS
BALANCED.
41

= 1 MOLE OF 12 HSA

= 6.291kg of LiOH
Hence,
LiOH CONTENT = 6.291*(42/24)
NOW,
OVERALL BALANCE
TOTAL INPUT = 8309 kg
=
45 *182
8190 Kg

= 119 Kg
ACTUAL % LOSS = 119*100/8309
= 1.43 %
42

= 152.874 Kg
1.839 %
Hence,
DEVIATION = 1.839-1.43
DEVIATION =+0.409% (ADVANTAGEOUS)
BATCH
NO.
TOTAL
INPUT
OUTPUT
ACTUAL
% LOSS
7921
7720
8309
7826
7644
8190
1.90
1.95
1.43
THEOROTICAL
% LOSS
1.19
0.98
1.83
43
%
DEVIATION
PENETRATION
+0.71
+0.97
+0.40
225/230
227/230
235/240
FUTURE UPCOMINGS
Manufacturing Bio-Based Grease Using Microwaves
The University of Northern Iowas National Ag-Based Lubricants Centre (UNI-NABL) along
with Iowa-based Environmental Lubricants Manufacturing (ELM) have been engaged in
research and development of manufacturing processes and bio based greases made from
vegetable oils. Several commercial grease products, including large volumes of rail curve
grease made from soybean oils, owe their origin to these centres.
There is growing interest in bio-lubricants that use vegetable and mineral oils to reduce
petroleum-based oil stock. Some of this development is being driven by environmental and
regulatory pressures. These new compounds blend a variety of eco-friendly oils such as
soybean, canola (rapeseed) and sunflower seed which are nontoxic and renewable. In
addition, some research indicates vegetable-based lubricants, made with individual fatty acids
can perform better in motor vehicle engines and other applications than their petroleum-based
counterparts.
Vegetable oils, due to their polar nature, respond to microwave energy like water does, by
vibrating, and can be effectively heated with surprisingly high efficiency. When polar
molecules of vegetable oils are exposed to high energy microwaves, they absorb the
microwave energy which results in a rapid heat rise. The molecules of mineral oils and nonpolar liquids, when exposed to microwaves, do not vibrate. Instead they pick up speed and
can rotate resulting in less friction at the molecular level and less heat rise. There are means
available for increasing the effective energy absorption of non-polar materials like mineral
oils, thus rendering them a better candidate for processing with microwave energy.
UNI-NABL and ELM have joined forces with Marion Mixers and AMTek Microwave. Both
companies are located in the Cedar Rapids, Iowa area. These two companies are working in
collaboration with NABL researchers and ELM product engineers to introduce processing
systems that incorporate microwaves for heating and drying applications.
This revolutionary technology, featured in a segment of the History Channels Modern
Marvel television show, has been field tested at the ELM manufacturing facility. Numerous
trials with varying levels of microwave energy and variation in the speed of the circulating
pump were tested at ELM. The initial test run (shown below) proved that the Marion
horizontal mixer with gentle agitation and AMTek microwave system was successful in
making Aluminium grease in a fraction of the time it takes to produce the same product in a
conventional jacketed kettle system.
23
Most conventional grease processing systems continue to use hot oil and steam to heat grease
materials in open kettles. This slow and inefficient process has many safety, operability,
environmental and maintenance issues. Microwaves are not forms of heat but rather forms of
energy; electromagnetic energy that is manifested as heat through their interaction with
materials. Microwaves initially excite the outer layers of molecules. The inner part of the
material is warmed as heat travels from the outer layers inward.
If the material is very wet and the pressure inside rises rapidly the liquid will be removed
from the material due to the difference in pressure. Electromagnetic energy eliminates the
need for the equipment to warm up and cool down; heating only the product, not the room or
vessel. This results in shorter batch times and significant savings. The various elements of the
process include:
Microwave Source:
The microwave source is a compact electrical unit that converts electrical energy in
this case from a 480 Volt power source to microwave energy at 75 kW of power.
The output microwave power is adjustable between 0 and 75 kW allowing for the
exact amount of energy needed to be applied to the media being heated.
The magnetron within the transmitter is considered consumable and would need to be
replaced after some hours (several thousand) of operation depending on the severity
of usage. In general these transmitters, like their smaller household versions, can
provide years of operation without major maintenance requirements.
The systems are networkable and troubleshooting can be accomplished remotely by

the manufacturer of the system. Most components are easily replaceable by a
qualified electrician making the transmitter a rather trouble free and clean heat source
with a small footprint.
24
Grease Reactor:
The grease reactor, in this case, was an atmospheric stainless steel tank that was adapted for
manufacturing grease. Despite common misconceptions, provided that there is a sufficient
mass of product to absorb the microwave energy, metal containers can be used for microwave
heating. In order to facilitate circulation and mixing, the reactor was fitted with a pump that
circulated the product from the bottom centre of the tank into the vessel through four pipes
welded to its sides. Figure shows the reactor and some of its attachments.
Energy Transfer Waveguides

The microwave energy can be effectively transmitted through special conducting ducts called
waveguides. These are specially designed, usually aluminium, square ducts that allow
microwaves to travel and go around the corners without any notable losses. This feature would
allow the microwave transmitter to be placed close to, above, or away from the reactor. Figure
shows the waveguides as attached to the top of the reactor.
Viewing the grease production process, or inspection of the product during the process can be
performed through Viewing Ports on top of the reactor where, using a flash light, the operator
25
could peak through to inspect the condition of the product while the microwaves are being
applied. The concept incorporates a design that prevents microwave leakage, based on the size of
the viewing ports. The viewing port on top of the reactor could also be used for the addition of
additives and oils as needed.
Programming the Control System
A programmable logic controller (PLC) which can be interfaced with a number of sensors, can
be used to control the microwaves power level.
A temperature sensor placed at the bottom of the reactor was interfaced with the controller. Once
the desired temperature and microwave power level is set on the touch screen controller the
heating starts until the desired temperature is reached. At that time, the PLC would reduce the
power level to near zero and would ramp up or down the power level as needed to maintain the
set temperature. This assures a near perfect reaction temperature every time.
Economics of Microwave Heating

Conventional heating is limited in several ways. Surface heating can go only as fast as allowed
by the specific heat, thermal conductivity, density and viscosity of the material being heated.
While youre waiting for the material at the centre of the vessel to heat up, surfaces are getting
sticky and hot, and the edges and corners of the product are over-heating, leading to product
rejections, wasted energy and extended process times.
But with microwaves, you can heat the entire volume of a material at the same rate. It s called
volumetric heating and it transfers energy through the material electro-magnetically, not as a
thermal heat flux. This creates a sort of pumping action forcing liquid to the surface, often as
vapour. The result is very rapid drying without the need to overheat the atmosphere which may
cause case hardening or other surface overheating phenomena. The rate of heating is not limited
and the uniformity of heat distribution is greatly improved. Heating times can be reduced to less
than one percent of that required using conventional techniques
26
Energy Savings
There was a time when electrically powered systems were considered too costly to operate for
high-power applications. Today, with the rising costs of oil and gas, this is no longer necessarily
true. There is significant interest today in the potential energy saving from a microwave heating
system. The offsets to the current cost of electricity include the increased speed of drying, the
direct coupling of energy into the material and possible lower drying temperatures. Processors
that use steam, gas or electric heating systems are aware of the high costs of running these
systems. A summary of the energy-saving benefits of microwave heating verses conventional
heating are as follows:
Slash energy consumption by up to 50%

Reduce man-hours and downtime involved in cleaning
Minimize ancillary equipment such as heated jackets, boiling pans and heating vessels
Shrink your heating and drying equipment footprint
Eliminate warm up and cool down time
Microwave energy does not heat the room only the material
The microwave mixer heating system is available in virtually any vessel size for any industry
where consistent energy efficient volumetric heating application is required. Other industries
where microwave mixing has proven successful in either sanitary or non-sanitary applications
include chemicals, plastics, minerals, textiles, food, waste-to-energy and recycling. .
27
CONCLUSION
Innovative Technology
As one of the leading grease manufacturing in the world, AXEL is committed to continue
providing technological breakthroughs, bringing to market greases that truly exceed
customer expectations and industry standards. Below are the few examples of our innovation.
Epoch Technology
Inert thickener system.
Increased additive response.
Resistance to water and aggressive chemicals.
Controlled oil separation
Excellent low to ambient temperature performance.
Long life.
Bismuth Technology
Key advantages by using bismuth as an additive compared to conventional EP/AW additives
Increased EP performance.
Increased wear protection.
Increased corrosion inhibition.
Key advantages by incorporating bismuth in the soap structure (Dubbilit)
Increased mechanical stability.
Increased thermal stability.
Decreased fretting.
Decreased friction.
This contributes to extend the grease life in harsh conditions.
28
REFERNCES
1. A.A. Gordon, European patent office 0072184 B1; 1986, Lubricating Grease Guide, Kansas City,
National lubricating Grease Institute 1989.
2. Adams, Robert C., and Patton, Harrison E., ASTM proceedings, 41, 1095- 1104(1941).
3. Analytical test method manual of IOCL.
4. ASTM standards on petroleum products,p.156, 1950.
5. Batch processes : 1979,Ekaterini Korovessi, Andreas A. Linninger, CRC press, 2005.
6. C.J. Boner, Manufacture & application of lubricating greases. (New York: Reinhold publishing,
1954).
7. Edition 1996 of annual book of ASTM standards, section 5, petroleum products, lubricants &
fossil fuels, volume 05.01, petroleum & lubricants ,designation: D-217-94 page-111 to 122
8. E. Armstrong, U.S. patent 2,704,363;1955.
9. Jarrod Potteiger, Precision Lubrication for Grease lubricated bearing;
magazine.
Machinery lubrication
10. Jarrod Potteiger Step-By-Step Grease Selection. Machinery Lubrication Magazine, September
2005.
30

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REPORT ON PETROLEUM REFINING

TITLE:- MANUFACTURING OF GREASE

ALL INDIA SHRI SHIVAJI MEMORIAL

This is to certify Seminar report on

Advantages and Disadvantages

Chemistry of the Process Studied

Hydrodynamic lubrication two surfaces are separated by a fluid film,

Fig 2 Stribeck Curve

The NLGI Grade:

Fig 3 NLGI Grades

Phenols, amines, phosphorous compounds,

Extreme pressure and corrosion inhibitor

Tricrysylphosphate, amine phosphate,

Barium and calcium sulphonates

Benzotrizoles, Mercapto enzothiozoles,

ZDDP, antimony di-alkyl di-thiophosphate

Water repelling agent

High Temperature Effects:

Low Temperature Effects:

As the saponification reaction proceeds to completion, water is generated as a

Some greases require milling. Milling (sometimes referred to as homogenizing)

Base oil cutback

General Process Flow

Advantages of Batch Process:

In batch process equipment can be reuse.

Working:-It is the subjection of lubricating grease to shearing action of standard grease

Worked penetration: - It is the penetration of grease sample subjected to 60 double

strokes in standard grease worker and penetration is done at 25 C.

Unworked penetration: - It is the penetration at 25oC of grease which is transferred in

Block penetration: - It is the penetration at 25oC or grease sample that is sufficiently

Test:- Method for working stability of grease in presence of water

Working: - Grease is filled in cup and exposed to prolonged mechanical working in

Test:- Dropping Point Test

Test:- Determination Of Heat Stability

Test:- Determination of Evaporation Test

Test:- Oxidation Stability

Test:- Determination of free acidity and alkalinity of grease

Test:- Copper Corrosion Test

conditions it is not possible to specify either temperature or duration of test. It is

Test:- Determination of storage stability of grease

Working: - The consistency, both worked and unworked penetration of material is

ADVANTAGES OF GREASE LUBRICATION

Contamination- the risk of the contamination products such as food and

DISADVANTAGES OF GREASE LUBRICATION

Compatibility the use must be careful about thickener compatibility of grease. In

General processing industries.

MOLECULAR FORMULAE: HCO

LITHIUM SALT OF HCO (SOAP)

MASS BALANCE OF SERVO GEM RR3 GRADE GREASE

RAW MATERIAL REQUIRED FOR CHARGING IS:COMPONENT

BASE OIL 500N

12 HYDROXY STEARIC ACID

AVERAGE MOLECULAR WEIGHT:COMPONENT

OVERALL MASS BALANCE OVER REACTION DURING

OVERALL MASS BALANCE OVER REACTOR DURING WASHING:-

BRIGHT STOCK FOR WASHING = WASHED OIL + VENT

OVERALL MASS BALANCE OVER KETTLE:-

SOAP + WASHED OIL+ ADDITIVES + CORRECTION/CUTBACK OIL = EXHAUST +

WATER / VOLATILES BALANCE:WATER OF CRYSTALLISATION OF LiOH.H2O

WATER RELEASED DURING REACTION:

MOISTURE CONTENT OF FATTY ACIDS (0.25%):

VOLATILE AND MOISTURE CONTENT OF BASE OIL:

TOTAL AMOUNT OF WATER RELEASED= 77.142 + 69.90 + 3.0 + 2.568