ANNEXURE-I

1. Safety Precaution used in Laboratory Level:-

i. No running and jumping in laboratory areas shall be permitted.
ii. Lab coats and safety glasses are required in laboratories employing
chemicals or bio hazards.
iii. Foot wear and clothing are to be wear which will not create sparks.
iv. Using nylon clothes is avoided as it can produce static electricity.
v. Wash your hands frequently throughout the day and before leaving the
lab.
vi. Do not smoke and carry the matches.
vii. Keep all aisles and walk ways into the lab clear to provide a safe
walking surface.
viii. Never pipette out by mouth. Always use a pipette bulb.
ix. Wear apron while doing the experiment and also shoes.
x. Be alert and don’t be in dream while handling chemicals and electrical
equipment’s.
xi. Do not stopper on to glass tubing’s.
xii. Report all incidents/accidents to your teacher immediately.
xiii. Never throw sodium metal in sink.
xiv. Notify your instructor about fire accidents immediately to take steps
for firefighting.
xv. Chemical Burn:
General chemicals: Immediately warm off plenty of water.
xvi. Acids: Wash with water and then with dilute Na2Co3 solutions.
xvii. Bases: Wash with water.
2. Safety Precautions used in Soap industry:-
PLANT SAFETY
Every organisation (company or industry) has the moral and legal obligation to
protect the health and welfare of its employees as well as that of the general
public. Therefore, good safety measures have to be put in place to ensure the
safety of lives and prevent damage to equipment. The primary aim of these
safety measures therefore is to prevent or minimize workers exposure to the
potential hazard, injury to workers, loss of lives, and destruction of properties.
They are also needed to ensure safe as well as efficient operation.

These safety measures are employed in industry mainly to prevent or control

hazards.

A hazard is a property which in particular circumstances could lead to harm.

Common safety hazards in the manufacturing industry include; dangerous
machinery, explosion to fires, faulty electrical connections and falling materials
due to poor housekeeping among others.

The potential hazards that could be present in the toilet soap plant include
hazards due to materials handling and hazards due to the various processes.

Hazards due to materials handling

Potentially hazardous situations include handling and packaging operations,

equipment cleaning and repair, decontamination following spills and equipment
failure. Hazards that workers are likely to be exposed to can be prevented by a
number of ways, example of which is the provision of PPEs (Personal
Protective Equipment). These equipments include chemical splash goggles,
overcoat/chemical suit, rubber boots, ear plugs, face shield, etc. These
equipment are worn to protect the worker from the dangers of handling some of
the chemicals especially sodium hydroxide.

Hazards due to various processes

Hazards that might be caused during processes in this plant include fire hazards,
electrical and mechanical hazards.

 Fire Hazards: During the process of heating the raw materials, for
example, heating takes place at high temperatures of about 600-650⁰C
with the production of hot flue gases through a chimney. Care must be
 taken near or during operation of the saponification vessel for example
the control of temperature. Labourers are so careless and tend to attempt
checking temperature manually. This and many other careless practices
may lead to a fire hazard. Overheating of vessel should also be avoided to
prevent explosions or fire outbreak.
 Electrical Hazards: The main source of energy for this plant is
electricity since most of the process units would be powered by it .Care
must be taken in dealing with electric powered units, power should be
shut down immediately when faulty electrical connections are detected
and alternative power source be sought for use. Workers must also be
careful especially during power fluctuations as this might cause
electrocution or explosions that might lead to fires.
 Mechanical Hazards: These hazards may be due to improperly fixed or
dangerous machinery. Some machines are designed in such a way that it
picks everything in its path. For example packaging. Such equipment is
likely to cause a mechanical hazard. Parts of machinery should not be left
just anywhere on the plant site. Rather, good housekeeping of machine
parts should be employed.

With the above mentioned safety measures, the plant can be safe to work on.
 ANNEXURE-II

Introduction

It has been said that the use of soap is a gauge of the civilisation of a nation, but
though this may perhaps be in a great measure correct at the present day, the use
of soap has not always been co-existent with civilisation, for according to Pliny
soap was first introduced into Rome from Germany, having been discovered by
the Gauls, who used the product obtained by mixing goats' tallow and beech ash
for giving a bright hue to the hair. In West Central Africa, moreover, the
natives, especially the Fanti race, have been accustomed to wash themselves
with soap prepared by mixing crude palm oil and water with the ashes of banana
and plantain skins. The manufacture of soap seems to have flourished during the
eighth century in Italy and Spain, and was introduced into France some five
hundred years later, when factories were established at Marseilles for the
manufacture of olive-oil soap. Soap does not appear to have been made in
England until the fourteenth century, and the first record of soap manufacture in
London is in 1524. From this time till the beginning of the nineteenth century
the manufacture of soap developed very slowly, being essentially carried on by
rule-of-thumb methods, but the classic researches of Chevreul on the
constitution of fats at once placed the industry upon a scientific basis, and
stimulated by Leblanc's discovery of a process for the commercial manufacture
of caustic soda from common salt, the production of soap has advanced by leaps
and bounds until it is now one of the most important of British industries.

Definition of Soap: The word soap (Latin sapo, which is cognate with Latin
sebum, tallow) appears to have been originally applied to the product obtained
by treating tallow with ashes. In its strictly chemical sense it refers to
combinations of fatty acids with metallic bases, a definition which includes not
only sodium stearate, oleate and palmitate, which form the bulk of the soaps of
commerce, but also the linoleates of lead, manganese, etc., used as driers, and
various pharmaceutical preparations, e.g., mercury oleate (Hydrargyri oleatum),
zinc oleate and lead plaster, together with a number of other metallic salts of
fatty acids. Technically speaking, however, the meaning of the term soap is
considerably restricted, being generally limited to the combinations of fatty
acids and alkalies, obtained by treating various animal or vegetable fatty
matters, or the fatty acids derived therefrom, with soda or potash, the former
giving hard soaps, the latter soft soaps.

The use of ammonia as an alkali for soap-making purposes has often been
attempted, but owing to the ease with which the resultant soap is decomposed, it
can scarcely be looked upon as a product of much commercial value.

H. Jackson has, however, recently patented the use of ammonium oleate for
laundry work. This detergent is prepared in the wash-tub at the time of use, and
it is claimed that goods are cleansed by merely immersing them in this solution
for a short time and rinsing in fresh water.

Neither of the definitions given above includes the sodium and potassium salts
of rosin, commonly called rosin soap, for the acid constituents of rosin have
been shown to be aromatic, but in view of the analogous properties of these
resinates to true soap, they are generally regarded as legitimate constituents of
soap, having been used in Great Britain since 1827, and receiving legislative
sanction in Holland in 1875.

Other definitions of soap have been given, based not upon its composition, but
upon its properties, among which may be mentioned that of Kingzett, who says
that "Soap, considered commercially, is a body which on treatment with water
liberates alkali," and that of Nuttall, who defines soap as "an alkaline or
unctuous substance used in washing and cleansing".
Kinds of soap:

Soaps are salts of fatty acids, soaps have the general formula
(RCO2−)nMn+ (R = alkyl).
The major classification of soaps is determined by the identity of Mn+. When
M = Na or K, the soaps are called toilet soaps, used for hand washing. Many
metal dications (Mg2+, Ca2+, and others) give metallic soap When M = Li, the
result is lithium soap (e.g., lithium stearate), which is used in high-
performance greases

1. Toilet soap
2. Non toilet soap(metallic soap)
 ANNEXURE-III

Toilet soaps:
In a domestic setting, "soap" usually refers to what is technically
called a toilet soap, used for household and personal cleaning. When used for
cleaning, soap solubilises particles and grime, which can then be separated from
the article being cleaned. The insoluble oil/fat molecules become associated
inside micelles tiny spheres formed from soap molecules with
polar hydrophilic (water-attracting) groups on the outside and encasing
a lipophilic (fat-attracting) pocket, which shields the oil/fat molecules from the
water making it soluble. Anything that is soluble will be washed away with the
water.

Structure of a micelle a cell-like structure formed by the aggregation of soap subunits (such as sodium
stearate): The exterior of the micelle is hydrophilic (attracted to water) and the interior is lipophilic
(attracted to oils).

TOLET SOAP:
RAW MATERIALS USED IN SOAP-MAKING.
Fats and Oils:

All animal and vegetable oils and fats intended for soap-making
should be as free as possible from unsaponifiable matter, of a good colour and
appearance, and in a sweet, fresh condition. The unsaponifiable matter naturally
present as cholesterol, or phytosterol, ranges in the various oils and fats from
0.2 to 2.0 per cent. All oils and fats contain more or less free acidity; but excess
of acidity, though it may be due to the decomposition of the glyceride, and does
not always denote rancidity, is undesirable in soap-making material. Rancidity
of fats and oils is entirely due to oxidation, in addition to free acid, aldehydes
and ketones being formed, and it has been proposed to estimate rancidity by
determining the amount of these latter produced. It is scarcely necessary to
observe how very important it is that the sampling of fats and oils should be
efficiently performed, so that the sample submitted to the chemist may be a
fairly representative average of the parcel.

In the following short description of the materials used, we give, under each
heading, figures for typical samples of the qualities most suitable for soap-
making.

Tallows:

Most of the imported tallow comes from America, Australia and

New Zealand. South American mutton tallow is usually of good quality; South
American beef tallow is possessed of a deep yellow colour and rather strong
odour, but makes a bright soap of a good body and texture. North American
tallows are, as a general rule, much paler in colour than those of South America,
but do not compare with them in consistence. Most of the Australasian tallows
are of very uniform quality and much in demand.
Lard: Lard is largely imported into this country from the United States of
America. The following is a typical sample of American hog's fat offered for
soap-making

Cocoa-nut Oil: The best known qualities are Cochin and Ceylon oils, which are
prepared in Cochin (Malabar) or the Philippine Islands and Ceylon respectively.

The dried kernels of the cocoa-nut are exported to various ports in Europe, and
the oil obtained comes on the market as Continental Coprah Oil, with the prefix
of the particular country or port where it has been crushed, e.g., Belgian, French
and Marseilles Coprah Oil. Coprah is also imported into England, and the oil
expressed from it is termed English Pressed Coprah.

Olive-kernel oil: more correctly termed Sulphur olive oil.

The amount of free fatty acids is always high and ranges from 40-70 per cent.,
and, of course, its glycerol content is proportionately variable. The free acidity
increases very rapidly, and is, doubtless, due to the decomposition of the neutral
oil by the action of hydrolytic ferment.

Palm oil: is produced from the fruit of palm trees, which abound along the west
coast of Africa. Lagos is the best quality, whilst Camaroons, Bonny, Old
Calabar and New Calabar oils are in good request for bleaching purposes.

In the lower qualities we have examples of the result of hydrolytic

decomposition by enzymes, the free acidity often amounting to 70 per cent.

Cotton-seed Oil: This oil is expressed from the seeds separated from the
"wool" of the various kinds of cotton tree largely cultivated in America and
Egypt.In its crude state cotton-seed oil is a dark fluid containing mucilaginous
and colouring matter, and is not applicable for soap-making. The following
figures are representative of well-refined cotton-seed oils:—
Cotton-seed Stearine: The product obtained by pressing the deposit which
separates on chilling refined cotton-seed oil.

Arachis Oil:The earth-nut or ground-nut, from which arachis oil is obtained, is

extensively cultivated in North America, India and Western Africa. Large
quantities are exported to Marseilles where the oil is expressed. Arachis oil
enters largely into the composition of Marseilles White Soaps.

Maize Oil: America (U.S.) produces very large quantities of maize oil.Sesame
Oil.—Sesame oil is very largely pressed in Southern France from the seeds of
the sesame plant which is cultivated in the Levant, India, Japan and Western
Africa.

Linseed Oil: Russia, India, and Argentine Republic are the principal countries
which extensively grow the flax plant, from the seeds of which linseed oil is
pressed. It is used to a limited extent in soft-soap making.

Hemp-seed oil: is produced from the seeds of the hemp plant which grows in
Russia. This oil is used in soft soap-making, more particularly on the Continent.

Castor Oil: The castor oil plant is really a native of India, but it is also
cultivated in the United States (Illinois) and Egypt.

Fish and Marine Animal Oils: Various oils of this class have, until recently,
entered largely into the composition of soft soaps, but a demand has now arisen
for soft soaps made from vegetable oils.

Pale seal oil,Straw seal oil,Brown seal oil,Whale oil,Dark whale oil , Japan fish
oil, Japan fish oil, Brown cod oiL, Pure herring oil, Kipper are listof few oils
used in soap manufacturing
Waste Fats: Under this classification may be included marrow fat, skin greases,
bone fats, animal grease, melted stuff from hotel and restaurant refuse, and
similar fatty products.

Fatty Acids: We have already described the various methods of liberating fatty
acids by hydrolysis or saponification.

Under this heading should also be included stearines produced by submitting

distilled fat to hydraulic pressure, the distillates from e from unsaponifiable
matter, cocoa-nut oleine, a bye-product from the manufacture of edible cocoa-
nut butter and consisting largely of free acids, and palm-nut oleine obtained in a
similar manner from palm-nut oil.

These are all available for soap-making.

Less-known Oils and Fats of Limited Use:

Shea Butter: Shea butter is extracted from the kernels of the Bassia Parkii and
exported from Africa and Eastern India. This fat is somewhat tough and sticky,
and the amount of unsaponifiable matter present is sometimes considerable

Mowrah-seed Oil: The mowrah-seed oil now offered for soap-making is

derived from the seeds of Bassia longifolia and Bassia latifolia. It is largely
exported from India to Belgium, France and England.

Chinese vegetable tallow is the name given to the fat which is found coating the
seeds of the "tallow tree" (Stillingia sebifera) which is indigenous to China and
has been introduced to India where it flourishes.

Borneo Tallow: The kernels of several species of Hopea (or Dipterocarpus),

which flourish in the Malayan Archipelago, yield a fat known locally as
Tangawang fat. This fat is moulded (by means of bamboo canes) into the form
of rolls about 3 inches thick, and exported to Europe as Borneo Tallow.
Kapok oil is produced from a tree which is extensively grown in the East and
West Indies. The Dutch have placed it on the market and the figures given by
Henriques (Chem. Zeit., 17, 1283) and Philippe (Monit. Scient., 1902, 730),
although varying somewhat, show the oil to be similar to cotton-seed oil.

Various New Fats and Oils Suggested for Soap-making.

Carapa or Andiroba oil, derived from the seeds of a tree (Carapa Guianensis)
grown in West Indies and tropical America, has been suggested as suitable for
soap-making. Deering (Imperial Institute Journ., 1898, 313)

Candle-nut oil: obtained from the seeds of a tree flourishing in India and also
the South Sea Islands. Curcas oil is produced in Portugal from the seeds of the
"purging nut tree," which is similar to the castor oil plant, and is cultivated in
Cape Verde Islands and other Portuguese Colonies.

Goa butter or Kokum butter: is a solid fat obtained from the seeds of
Garcinia indica, which flourishes in India and the East Indies.

Safflower oil: is extracted from the seeds of the Carthamus tinctorius, which,
although indigenous to India and the East Indies, is extensively cultivated in
Southern Russia (Saratowa) and German East Africa.

Maripa fat: is obtained from the kernels of a palm tree flourishing in the West
Indies, but, doubtless, the commercial fat is obtained from other trees of the
same family. It resembles cocoa-nut oil and gives the following figures:—

Niam fat: obtained from the seeds of Lophira alata, which are found
extensively in the Soudan. The fat, as prepared by natives, has been examined
by Lewkowitsch, and more recently Edie has published the results of an
analysis.

Cohune-nut oil: it is produced from the nuts of the cohune palm, which
flourishes in British Honduras. This oil closely resembles cocoa-nut and palm-
nut oils and is stated to saponify readily and yield a soap free from odour.

Rosin:

Rosin is the residuum remaining after distillation of spirits of

turpentine from the crude oleo-resin exuded by several species of the[Pg 38]
pine, which abound in America, particularly in North Carolina, and also flourish
in France and Spain. The gigantic forests of the United States consist principally
of the long-leaved pine, Pinus palustris (Australis), whilst the French and
Spanish oleo-resin is chiefly obtained from Pinus pinaster, which is largely
cultivated.

Rosin is a brittle, tasteless, transparent substance having a smooth shining

fracture and melting at about 135° C. (275° F.). The American variety possesses
a characteristic aromatic odour, which is lacking in those from France and
Spain. It is graded by samples taken out of the top of every barrel, and cut into
7/8 of an inch cubes, which must be uniform in size—the shade of colour of the
cube determines its grade and value

Alkali (Caustic and Carbonated).

The manufacture of alkali was at one time carried on in

conjunction with soap-making, but of late years it has become more general for
the soap manufacturer to buy his caustic soda or carbonated alkali from the
alkali-maker Although there are some alkali-makers who invoice caustic soda
and soda ash in terms of actual percentage of sodium oxide (Na2O), it is the
trade custom to buy and sell on what is known as the English degree, which is
about 1 per cent. higher than this. The English degree is a survival of the time
when the atomic weight of sodium was believed to be twenty-four instead of
twenty-three, and, since the error on 76 per cent. Na2O due to this amounts to
about 1 per cent., may be obtained by adding this figure to the sodium oxide
really present.

Caustic soda (sodium hydrate) comes into commerce in a liquid form as 90°
Tw. (and even as high as 106° Tw.), and other degrees of dilution, and also in a
solid form in various grades as 60°, 70°, 76-77°, 77-78°. These degrees
represent the percentage of sodium oxide (Na2O) present plus the 1 per cent.
The highest grade, containing as it does more available caustic soda and less
impurities, is much more advantageous in use.

Carbonate of soda or soda ash, 58°, also termed "light ash," and "refined alkali".
This is a commercially pure sodium carbonate containing about 0.5 per cent.
salt (NaCl). The 58° represents the English degrees and corresponds to 99 per
cent. sodium carbonate (Na2CO3).

Soda ash, 48°, sometimes called "caustic soda ash," often contains besides
carbonate of soda, 4 per cent. caustic soda (sodium hydrate), and 10 per cent.
salt (sodium chloride), together with water and impurities.

The 48 degrees refers to the amount of alkali present in terms of sodium oxide
(Na2O), but expressed as English degrees.
Caustic potash (potassium hydrate) is offered as a liquid of 50-52° B. (98-103°
Tw.) strength, and also in solid form as 75-80° and 88-92°. The degrees in the
latter case refer to the percentage of potassium hydrate (KHO) actually present.

Carbonate of Potash.—The standard for refined carbonate of potash is 90-92 per

cent. of actual potassium carbonate (K2CO3) present, although it can be
obtained testing 95-98 per cent.

Other Materials.

Water:

water intended for use in soap-making should be as soft as

possible. If the water supply is hard, it should be treated chemically; the
softening agents may be lime and soda ash together, soda ash alone, or caustic
soda. There are many excellent plants in vogue for water softening, which are
based on similar principles and merely vary in mechanical arrangement. The
advantages accruing from the softening of hard water intended for steam-raising
are sufficiently established and need not be detailed here.

Salt (sodium chloride or common salt, NaCl):

It is a very important material to the soap-maker, and is obtainable in a

very pure state.Brine, or a saturated solution of salt, is very convenient in soap-
making, and, if the salt used is pure, will contain 26.4 per cent. sodium chloride
and have a density of 41.6° Tw.The presence of sulphates alters the density, and
of course the sodium chloride content.Salt produced during the recovery of
glycerine from the spent lyes often contains sulphates, and the density of the
brine made from this salt ranges higher than 42° Tw. (25° B.)
Soapstock:

This substance is largely imported from America, where it is

produced from the dark-coloured residue, termed mucilage, obtained from the
refining of crude cotton-seed oil. Mucilage consists of cotton-seed oil soap,
together with the colouring and resinous principles separated during the
treatment of the crude oil. The colouring matter is removed by boiling the
mucilage with water and graining well with salt; this treatment is repeated
several times until the product is free from excess of colour, when it is
converted into soap and a nigre settled out from it

Methods of preparation of Toilet soap:

In cold-process and hot-process soap making, heat may be required for
saponification. Cold-process soap making takes place at a sufficient temperature
to ensure the liquefaction of the fat being used. The lye and fat may be kept
warm after mixing to ensure that the soap is completely saponified. Unlike cold-
processed soap, hot-processed soap can be used right away because lye and fat
saponify more quickly at the higher temperatures used in hot-process soap
making. Hot-process soap making was used when the purity of lye was
unreliable, and this process can use natural lye solutions, such as potash. The
main benefit of hot processing is that the exact concentration of the lye solution
does not need to be known to perform the process with adequate success. Cold-
process soap making requires exact measurements of lye and fat amounts and
computing their ratio, using saponification charts to ensure that the finished
product is mild and skin-friendly. Saponification charts can also be used in hot-
process soap making, but are not as necessary as in cold-process soap making.

Hot process

In the hot-process method, lye and fat are boiled together at 80–100 °C until
saponification occurs, which before modern thermometers, the soapmaker
determined by taste (the bright, distinctive taste of lye disappears once all the
lye is saponified) or by eye; the experienced eye can tell when gel stage and full
saponification have occurred. Beginners can find this information through
research, and classes. It is highly recommended to not "taste" soap for readiness.
Lye, when not saponified is a highly caustic material. After saponification has
occurred, the soap is sometimes precipitated from the solution by adding salt,
and the excess liquid drained off. The hot, soft soap is then spooned into a mold.
The soap lye is processed for recovery of Glycerine.

Cold process

A cold-process soapmaker first looks up the saponification value of the fats

being used on a saponification chart, which is then used to calculate the
appropriate amount of lye. Excess unreacted lye in the soap will result in a very
high pH and can burn or irritate skin. Not enough lye, and the soap is greasy.
Most soap makers formulate their recipes with a 4-10% deficit of lye so that all
of the lye is reacted and that excess fat is left for skin conditioning benefits.The
lye is dissolved in water. Then oils are heated, or melted if they are solid at
room temperature. Once both substances have cooled to approximately 100-110
°F (37-43 °C), and are no more than 10°F (~5.5°C) apart, they may be
combined. This lye-fat mixture is stirred until "trace" (modern-day amateur soap
makers often use a stick blender to speed this process). There are varying levels
of trace. Depending on how additives will affect trace, they may be added at
light trace, medium trace or heavy trace. After much stirring, the mixture turns
to the consistency of a thin pudding. "Trace" corresponds roughly to viscosity.
Essential oils, fragrance oils, botanicals, herbs, oatmeal or other additives are
added at light trace, just as the mixture starts to thicken. The batch is then
poured into molds, kept warm with towels, or blankets, and left to continue
saponification for 18 to 48 hours. Milk soaps are the exception. They do not
require insulation. Insulation may cause the milk to burn. During this time, it is
normal for the soap to go through a "gel phase" where the opaque soap will turn
somewhat transparent for several hours, before once again turning opaque. The
soap will continue to give off heat for many hours after trace. After the
insulation period the soap is firm enough to be removed from the mold and cut
into bars. At this time, it is safe to use the soap since saponification is complete.
However, cold-process soaps are typically cured and hardened on a drying rack
for 2–6 weeks (depending on initial water content) before use. If using caustic
soda it is recommended that the soap is left to cure for at least four weeks.

LABORATORY METHOD OF SOAP PREPERATION:

Dissolve KOH, (4.5g) in a distilled water (10 ) in order

to get 0.1N KOH solution in a beaker (100 ml) by continuous stirring. Place oil
(20ml) in a flask (125 ml) and oil is heated on a water bath upto 45-50oC above
room temperature. Then the heated oil is weighed initially then add 0.1N KOH
solution and continuously stirred for about 30 minutes using an agitator. During
this time the contents in the beaker becomes more viscous. Finelly soap formed
after this a 20ml of saturated NaCl solution mixed, added and cooled to
precipitate the soap in the mixture. Then the beaker is weighed along with soap
is eliminated
Fig. 3.1 Flow diagram for Toilet Soap Production

ANNEXURE-IV

Metallic soaps:

Grease is a lubricant of higher initial viscosity than oil, consisting originally of a

calcium, sodium, or lithium soap jelly emulsified with mineral oil. Lubrication
has a remarkable importance in many industrial applications. However, most
traditional lubricants have a large negative impact on the environment.

Fig: Greases for automotive applications contain metallic soap

A proper lubrication not only reduces cost but also affects the natural
environment in appositive way. There is a great challenge for lubricating grease
developers to find new products that increase demands on long life, higher
speed, higher running temperatures and compatibility with the mechanical seals
and the global environment.

Lubricating gases are made from petroleum oils thickened with metal soaps.
Particularly lithium 12-hydroxystearate soap is the most widely used thickening
agent. The manufacture of lubricating gases is an example of mixing operation
in which rheological properties of the medium change during processing. In this
casa, firstly, the progress of saponification reaction occurs and then a
subsequent structural modification takes place.

However, the current industrial process of manufacturing of lubricating grease

is somewhat complicated, with generation of soap thickener during the mixing
process that consists of the saponification reaction of fatty acids followed by
dehydration, heating up to near the phase transformation temp of soap
crystallites and cooling down to crystallize the soap finely, an intense
homogenization or milling treatment has been usually applied to reduce crustal
size in some cases greases were processed with a pre made soap and then the
saponification and dehydration steps are replaced by a simple mixing of the
components. Our method is categorized into three main process such as
preparation of metallic soap and then finely obtained lubricating grease using
waste lubricating oil
(i.e.:; engine oil)

Metallic soaps are basically the sparingly soluble or in soluble salts of saturated
and unsaturated, straight chain and branched aliphatic carboxylic acids with 8-
22 carbon atoms. They are reaction products of saturated or unsaturated fatty
acids (carboxylic acids) with alkaline, alkaline earth or transiting metals ex;
oxides, hydroxides, carbonates, sulphates and chlorides that are used in metal
soap production.

Metal soaps also known as fatty acids salts. Sodium and potassium are not in
the above classification since the synthesized soaps by these metals are
traditional soaps, which exhibit different properties then metallic soaps by these
metal ion source and fatty acid depends on process type some commercially
important metal soaps include those of aluminium, barium, cadmium, calcium,
cobalt, copper, iron, lead, lithium, magnesium, manganese, potassium, nickel,
zinc and zirconium.

Significant application areas for metal soaps include lubricates and heat
stabilizers in plastics as well as dryers in paint and varnishes, and painting inks.
Other uses are as processing aids in rubber, fuel and lubricant additives, in the
rubber, fuel and lubricant additives, catalysts, gel thickeners, emulsifiers, water
repellents and fungicides.

The metallic soap can be prepared by either fusion process or double

decomposition process. The fusion process involves a reacting metal oxide or
hydroxide with fused fatty acids such as triglyceride in the presence of water.

The process yields desired metallic soap and glycerine. However, the double
decomposition process involves reacting an alkali soap that is comprised of an
alkaline metal salt or an aluminium salt of fatty acid with an inorganic metal salt
in our case we prepared metallic soap paste solution (i.e. addition of above dried
soluble soap + water) and metal salt soap (i.e. CaCl2/BaCl2) it has been
observed that the precipitation of metallic soaps occurred at different pH ranges
depending on their precipitation equilibrium and atomic weight of the metal
involved , show by the following equations

RCOOH + NaOH RCOONa + H2O

RCOONa + MSO4 M (RCOO)2 + Na2SO4

Calcium chloride or CaCl2 , is a salt of calcium and chlorine and behaves as a

typical ionic halide, hygroscopic in nature serve as a source of calcium ions in a
solution as calcium chloride is soluble Barium Chloride is the inorganic
compound with the formula BaCl2 react with sulphate into produce a thick
white precipitate of barium sulphate.

For preparation of metallic soap, neem and karanja oil has been selected. Their
selection is due to abundantly availability requirements. Also, the karanja plant
is said to be highly tolerant to salinity and can be grow in various soil textures
viz., stony and clayey. And can be grown in humd as well as subtropical
environments with annual rainfall ranging between 500 and 2500mm. The
present production of karanja oil approximately is 200 million tons per annum.
The time needed by the tree to mature, ranges from 4 to 7 years and almost 8 to
24kg per tree, oil seeds are abundantly and hence they are abundantly available
in nature.

This is one of the reasons for wide availability of this plant species and so far
there are no reports on advise effects of karanja on fauna, flora, human or even
on environment similar case is obtained for neem oil which is obtained from
fully matured seeds of Azadirachta indica, and collected in late summer,
secondly, the melting points of the metallic soaps for neem oil are between 100-
110oC and for karanaja oil are between 85-100oC which makes them suitable for
various applications as high M.P pose solubility and handling problem. Higher
ions and carboxyl ate ions.

The objective of the present study is to establish new experimental data for the
preparation of different metallic soaps which metal salt using laboratory scale
operation with metal salt using laboratory scale operation with karanja oil and
neem oil. The present study investigates the present study investigates the
physico-chemical properties of metallic soap and grease two metal salts have
been selected in the work viz,. Barium Chloride and Calcium chloride.

The work is also first of its kind to report the use of waste lubricating oil since
disposal of used lubricating oil results environmental hazards Metal soaps are
also included in modern artists' oil paints formulations as a rheology modifier.
Most heavy metal soaps are prepared by neutralization of purified fatty acids
PROCESS DESCRIPTION
INDUSTRIAL METHOD:

This is a continuous process which uses a plant. The process is best understood
in terms of two streams: soap flowing in the order given below against a
counter-current of lye.
Step 1 - Saponification
The raw materials are continually fed into a reactor in fixed proportions.
Tallow: 735.29 kg hr-1
NaOH solution: 272.33 kg hr-1
Lye: 35.22 kg hr-1
These ingredients alone would give a low water, high glycerine soap. Soap
needs to be about 30% water to be easily pumpable, and even then needs to be
held at around 70oC, so excess lye is added to hydrate the soap and dissolve out
some of the glycerine. The lye added is known as "half spent lye" and is the lye
discharged from the washing column. This lye already contains some glycerine,
but it is further enriched by that formed in the saponification reaction.
Step 2 - Lye separation
The wet soap is pumped to a "static separator" - a settling vessel which does not
use any mechanical action. The soap / lye mix is pumped into the tank where it
separates out on the basis of weight. The spent lye settles to the bottom from
where it is piped off to the glycerine recovery unit, while the soap rises to the
top and is piped away for further processing.
Step 3 - Soap washing
The soap still contains most of its glycerine at this stage, and this is removed
with fresh lye in a washing column. The column has rings fixed on its inside
surface. The soap solution is added near the bottom of the column and the lye
near the top. As the lye flows down the column through the centre, a series of
rotating disks keeps the soap / lye mixture agitated between the rings. This
creates enough turbulence to ensure good mixing between the two solutions.
The rate of glycerine production is calculated and the rate at which fresh lye is
added to the washing column then set such that the spent lye is 25 - 35 %
glycerine. Glycerine is almost infinitely soluble in brine, but at greater than 35%
glycerine the lye no longer efficiently removes glycerine from the soap.
The soap is allowed to overflow from the top of the column and the lye ("half
spent lye") is pumped away from the bottom at a controlled rate and added to
the reactor.
Step 4 - Lye separation
The lye is added at the top of the washing column, and the soap removed from
the column as overflow. As the lye is added near the overflow pipe the washed
soap is about 20% fresh lye, giving the soap unacceptably high water and
caustic levels. Separating off the lye lowers the electrolyte levels to acceptable
limits.
The soap and lye are separated in a centrifuge, leaving a soap which is 0.5%
NaCl and 0.3% NaOH, and about 31% water. The lye removed is used as fresh
lye.
Step 5 - Neutralisation
Although the caustic levels are quite low, they are still unacceptably high for
toilet and laundry soap. The NaOH is removed by reaction with a weak acid
such as coconut oil (which contains significant levels of free fatty acids),
coconut oil fatty acids, citric acid or phosphoric acid, with the choice of acid
being made largely on economic grounds. Some preservative is also added at
this stage.
Step 6 - Drying
Finally, the water levels must be reduced down to about 12%. This is done by
heating the soap to about 125oC under pressure (to prevent the water from
boiling off while the soap is still in the pipes) and then spraying it into an
evacuated chamber at 40 mm Hg (5.3 kPa). The latent heat of evaporation lost
as the water boils off reduces the soap temperature down to 45oC, at which
temperature it solidifes onto the chamber walls.The soap chips are scraped off
the walls and "plodded" (i.e. squeezed together) by screws known as "plodder
worms" to form soap noodles. The soap is now known as base or neat soap chip,
and can be converted into a variety of different soaps in the finishing stages.
The moisture evaporated off the wet soap is transported to a barometric
condensor, which recondenses the vapour without the system losing vacuum.
The moisture can contain soap dust (.Fines.) which is removed by cyclones and
returned by augers to the spray chamber, while the water is recycled.
Process Flow Diagram of Toilet Soap Production