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Project

ON

Preparation of Soap

CONTENTS

Acknowledgement Introduction Commonly used Fatty Acids Saturated Acids Unsaturated Acids Types o Soaps Procedure Cold Process Hot Process

Purification and finishing

Bi liography

ACKNOWLEDGEMENT

I take this opportunity to express my profound gratitude and deep regards to our Chemistry Faculty Mr. Dharmendra Mishra for his exemplary guidance, monitoring and constant encouragement throughout the course of this project. His blessings, help and guidance gi en by him time to time shall carry me a long !ay in the journey of life on !hich I am about to embark. I !ould also like to thank our laboratory assistant Mr. ". #. $erma for his help and support. %astly I !ould also like to thank my parents, brother, and friends for their constant encouragement !ithout !hich this assignment !ould not be possible.

Sonakshi Sethi

Introd ction
&oap, from a chemical standpoint, is a salt 'or a mixture of salts( of fatty * *

acids. )s !ith all salts, soap contains a positi e ion, usually #a

or + , and a

negati e ion, usually the anions of long,chained carboxylic acids obtained by the hydrolysis of animal or egetable fats. -hese fatty acids, of !hich there are about ./ naturally occurring members, are carboxylic acids containing 01, 02, or 03 carbon atoms in an unbranched chain. -he e en numbered chains result from the fact that fats are synthesi4ed in cells by the polymeri4ation of a .,carbon acetate unit.

In addition to the normal 'straight chain( saturated acids, there occur se eral !ith hydroxyl groups, and5or one or more double bonds in the carbon chain. the presence of unsaturation 'double bonds( in molecules of fatty acids, fats, or soup tend to lo!er the melting point of these compounds and to cause them to be in the li6uid state at room temperature. -hus, egetable fats are relati ely unsaturated and li6uid under the ordinary conditions, !hile animal fats, being relati ely more saturated, are solid, or semi,solid, at the same temperature. For this reason, egetable fats are commonly refereed to as saturated, or unsaturated because both egetable oils. '7e say relati ely

egetables oils and animal fats contain

saturated and unsaturated chains(. -he reason !hy double bonds lo!er the melting

point of a fatty acid chain, is that the sections of the chain attached to the double bond are attached cis,!ise to each other 'probably because the double bond cis configuration produces a bent chain !hich does not easily adhere to a neighboring chain by a $an der 7aals attraction hence a lo!er temperature 'lo!er mobility( is re6uired for these molecules to adhere in order to form a solid crystal lattice. It is interesting to note, that straight chained carboxylic acids ha ing an odd number of carbon atoms melt lo!er than e en chained acids of comparable molecular !eights.

Co!!on"# sed $att# Acids


-he most commonly encountered fatty acids in natural fats are gi en belo!8

Sat rated Acids

0.( %auric )cid 'Dodecanoic )cid(

CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,C::H
9 . . . . . . . . . .

..( Myristic )cid 'tetraderanoic )cids(

CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,C::H
9 . . . . . . . . . . . .

9.( ;almitic acid 'hexadecanoic acid(

CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,C::H
9 . . . . . . . . . . . . . .

1.( &tearic acid 'octadecanoic acid(

CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,
9 . . . . . . . . . . . . . . .

CH ,C::H
.

%nsat rated acids&

0.( :leic acid 'octadec,<,enoic acid(

CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH=CH,


9 . . . . . . .

CH ,CH ,CH ,CH ,CH ,CH ,


. . . . . .

CH ,C::H
.

..( %inoleic acid 'octadec,<, 0.,dienoic acid(

CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH ,CH=CH,


9 . . . . . . .

CH ,CH ,CH ,CH ,CH ,CH ,


. . . . . .

CH ,C::H
.

)ll fats are esters 'though, not all esters are necessarily, fat>( of the trihydroxy alcohol, glycerin, and fatty acids. &ince each molecule of fat contains three ester groups, fats are often referred to as triglycerides to distinguish them from other materials ha ing a fatty or greasy texture, such as !axes 'mono esters of long chain alcohols are carboxylic acids( mineral oil, and petroleum jelly 'long,chain

hydrocarbons(.

If ",C::H represents a generali4ed fatty acid '" is a hydrocarbon chain of 09, 0?, or 0@ carbons( then, the general formula for a fat is

-he fatty,acid residues in a typical fat molecule are usually different> Fats from different sources ha e different percentages of the common fatty acids, and can be distinguished from one another by a 6uantitati e analysis of these constituents. &oap is prepared by hydroly4ing a fat under alkaline 'basic( conditions. -he reaction is called saponification, and produces one molecule of glycerin and three molecules of soap, for each molecule of fat taken.

-he fats and oils most commonly used in soap preparation are lard and tallo! from animal sources, and coconut, palm and oli e oils from egetable sources. -allo! and lard are the fats separated from solid beef fat 'suet( and hog fat, by the process of rendering. "endering consists of boiling the animal fat in a pot !ith an e6ual olume of !ater until a layer of melted fat collects on top. '!hen the animal tissue is heated, the fat in the cells melts, expands, ruptures the cell membrane, and then flo!s out. &ince the fat is immiscible !ith !ater, and has a lo!er density, it forms a floating layer on the top of the !ater in the pot.( the rendered fat is then dra!n off, and allo!ed to solidify by cooling. -he length of the hydrocarbon chain and the number of double bonds in the carbonylic,acid portion of the fat or oil determine the properties of the resulting soap. For example, a salt of a saturated, long,chain acid makes a harder, more insoluble soap. Chain length also affects solubility. -allo! is the principal fatty material used in soap making, !ith coconut or palm oil blended in, to produce a softer 'more soluble( soap !hich !ill readily lather. &oaps made !ith +:H 'caustic

potash( instead of #a:H 'caustic soda( are li6uid rather than solid, at room temperature. 'potassium salts ha e a lo!er melting point than sodium salts.( -oilet soaps are generally carefully !ashed free of any remaining alkali used in the saponification procedure to a oid irritation and drying of the skin. )s much glycerine as possible is usually left in the soap, and perfumes, coloring, and medicinal agents are sometimes added. )lso added, are antioxidants to pre ent the soap from turning rancid. Many soaps are superfatted, i.e. not all of the fat is hydrolysed, in order that the final soap ha e some fat remaining to lubricate and smooth dry and sensiti e skin. Aesides tallo! and coconut oil, there are many other natural fats and oils !hich can be economically employed to make soaps of arying degrees of 6uality.

-he less pure the ra! material is, the more likely the soap !ill ha e an off,color 'generally yello! or bro!n(, and an undesirable odor. 'impure fats are sometimes treated !ith bleaching agents before saponification, but this adds to their cost.( Bxamples of such other starting materials in soap manufacture are8 coconut oil, palm oil, oli e oil, cottonseed oil, sesame oil, corn oil, &oya bean oil, hydrogenated egetable oils, rosin, naphthelinic acids, and greases made from animal skins, bones, tankage and garbage. -he lo!er grades of soaps are used as yello! laundry soap, soap po!ders, cleansers, and industrial soaps.

T#pes of Soaps

Aelo! are some important terms employed to describe special types of soap8

Casti"e soap ,, a mild soap originally made in &pain !ith pure oli e oil. -oday many CcastileD soaps are made !ith other egetable oils. Castile is a mar elous cleanser, producing a rich lather.

Crea! soaps E soaps containing cold cream materials, moisturi4ers and emollients. Cream soaps are particularly good for dry and delicate skin

Deodorant soaps E soaps to !hich antibacterial agents ha e been added to reduce odor,causing bacteria.

$"oatin' soaps E soaps ha ing air bubbles incorporated to lo!er the density. -his causes the bar to float.

(#po)a""er'enic soaps E Mild formula soaps, lo! in potential irritants. -hey usually produce a poor lather.

Medicated soaps E soaps containing medications such as tar, sulphur, or antibacterial ingredients, used to treat acne and other skin disorders. Medicated soaps re6uire through rinsing and are not recommended for sensiti e skin.

Milled soaps E these are the most commonly used, mass produced soaps. Milling refers to the mixing of color, perfume and soap flakes.

:atmeal soap E ) rough Etextured soap to !hich oatmeal has been added as a mild abrasi e and lather. Food for oily, dry, and normal skin.

Proced re
-!o procedures for soap making are gi en, a CcoldD and a ChotD process. -he cold process, suitable for homemade soaps, produces soap bars !hich retain the glycreine by,product, and if the amount of alkali employed in the saponification is limited, an excess of fat 'superfatted(. -he hot process, more suitable for laboratory or industrial preparation, yields a more chemically pure po!derG by,products and excess starting materials are separated.

I* Co"d process

7hen using a thermometer in this experiment, ne er use it to stir li6uids. Instead, use a fire polished glass rod. to properly measure the temperature of a li6uid, hold the thermometer so that its bulb is suspended in the center of the li6uid !hile reading the mercury le el. If the li6uid is being heated on a hot plate, do not the thermometer bulb to rest on the bottom of the container, as it !ill then be o erheated. "emo e the thermometer from the container after each reading. #ote8 the thermometer supplied does not re6uire shaking do!n before or after reading. ;lug in a hot plate and set to high. 7eigh a 0?/ ml beaker on the trip scale and add 3g of #a:H pellets to it. Handle #a:H !ith care as #a:H can burn the skin and is especially harmful to the eyes. In the hood, add .? ml of cold !ater to the beaker. &tir the mixture of #a:H pellets and !ater, until a clear solution results. Caution8 the beaker !ill become

ery hot as the #a:H dissol es. 7eigh a .?/ml beaker on the trip,scale and add ?3g of fat 'Crisco egetable shortening !orks !ell( to it. -hen place the beaker on the hot plate !ith lo! heat and !ith occasional stirring, melt the fat to melt completely. 7arm the melted fat to bet!een 1/,?/ C. "emo e the fat from the hot plate and add the lye solution to the fat !ith stirring. &tir the fat and #a:H mixture continuously and until an emulsion is formed. Hour mixture should look like a thick, light yello! milk shake and should stay emulsified 'should not separate into a fat and #a:H layer(. If your emulsion separates, the fat is too hot and needs to cool. %et the mixture cool on the bench top !ith occasional stirring until an emulsion, !hich does not separate, is formed. Hou may !ant to add perfume or other additi es at this point. ;our the emulsion into a plastic cup and place in your dra!er for the reaction to run 'it takes about .1 hours for the reaction to be complete(. -ake the soap home !ith you and let age for about t!o !eeks. During this time a po!dery layer of #aC: 'soda ash(
9 o

!ill form on the surface, as residual #a:H reacts !ith C: in the air !hile the soap
.

is drying. -his po!dery layer should be sliced off and the soap is ready to be used.

II* (ot process


;lug in a hot plate and set it on HIFH. Half fill a 1// ml beaker !ith hot !ater from the sink and place on the hot plate. 7hen the !ater begins to boil, adjust the heat, so that the !ater boils gently, but continuously. 7hile !aiting for the !ater to boil, !eigh a .?/ml Brlenmeyer flask on a triple beam balance and add 0/g of fat 'Crisco, spry, or lard( to it. In a 0?/ml beaker prepare 0// ml of a ?/,?/ solution of alcohol,!ater, by mixing ?/ ml of !ater and ?/ ml of <?I ethanol or methanol. 7eigh another 0?/ ml beaker on the triple beam balance, and add 0/g of #a:H pellets to the beaker. Handle #a:H !ith care as #a:H can burn the skin and is especially harmful to the eyes. In the hood, mix the #a:H !ith 92 ml of the of the ?/,?/ alcohol,!ater solution to it. &tir the mixture until a transparent solution is formed. Caution8 the beaker !ill get ery hot as the lye dissol es. ;our the lye solution into the Brlenmeyer flask containing the fat and mix !ell using a stirring rod or by s!irling !ith a beaker tongs. Clamp the Brlenmeyer in the boiling,!ater bath and !ith occasional stirring, allo! it to cook for at least 9/ minutes. 7hile the mixture boils, some foam !ill form 'due to soap formation(. -ry to minimi4e excessi e foaming, by adding small adding small portions of your alcohol,!ater solution. -he reaction is complete !hen oil globules are no longer

isible !hen the reaction mixture is stirred. Half fill a 2// ml beaker !ith 9// ml of clear 'filtered( saturated salt '#aC0( solution and ?/ ml of !ater. ;our the still hot reaction mixture containing soap, glycerine, excess #a:H, and alcohol into the salt solution. &tir the resulting

mixture and allo! to stand for ?,0/ minutes. -he soap !ill collect as a !hite layer on the surface of the salt !ater in the beaker. ;repare a suction trap from the acuum flask, !hich !ill be used later to filter the soap preparation. Aend a long piece of glass tubing into a right angle 'instructor !ill demonstrate(, and push one leg of the bend through a one,hole rubber stopper fitted for the mouth of the flask. 7hen inserted, the glass tube should extend to about J inch from the bottom of the flask. -he exposed leg of the bend should be cut off at about 9 inches from the bend, and, by means of a piece of rubber connector tubing, be attached to a 0.,inch length of glass tubing. -he side,arm of the acuum flask is no! connected to the acuum outlet !ith pressure tubing. 7hen the suction is turned on, this de ice !ill act like a acuum cleaner, sucking up li6uid instead of dust. Ae sure the suction is :FF, before proceeding. Aring the beaker containing the soap preparation next to the suction trap, and place the CspoutD of the trap into the beaker ha ing it touch the bottom. &lo!ly turn on the suction, and !atch the bottom 'a6ueous( layer being dra!n into the acuum flask. Dra! off most, but not all, of the bottom layer. Ae ready to stop the suction instantly, if it appears that some of the

soap crystals are being sucked up. Hou can stop the suction 6uickly by pulling the pressure tubing a!ay from the outlet, then turning off the acuum. Caution8 )t no time should the acuum flask be allo!ed to fill more than half,the trap, and pour out its contents. 7hen most of the a6ueous layer in the beaker has been dra!n off, filter the remaining mixture of soap and li6uid through a Auchner funnel '!ith filter paper attached ( to the suction flask. 7ash the crystals on the filter !ith ? ml portions of ice,cold !ater. ;ress out any remaining moisture from the cake of filtered crystals on the funnel !ith the flat end of a clean cork, or the clean bottom of a small beaker. )llo! the product to suck dry for 0/,0? minutes.

-urn off the suction, detach the Auchner funnel, and !ith the help of a clean spatula, transfer the soap crystals to a large sheet of smooth paper. ;ick up the sheet and slide the cystals into a clean, dry 0?/ ml beaker. %ea e the beaker stand, unco ered in your dra!er for se eral days to air,dry the product.

Purification and finishing

) generic bar of soap, after purification and finishing In the fully boiled process on factory scale, the soap is further purified to remove any excess sodium hydroxide, glycerol, and other impurities, colour compounds, etc. These components are removed by boiling the crude soap curds in water and then precipitating the soap with salt. At this stage, the soap still contains too much water, which has to be removed. This was traditionally done on chill rolls, which produced the soap flakes commonly used in the 19 !s and 19"!s. This process was superseded by spray dryers and then by vacuum dryers. The dry soap #about $%1&' moisture( is then compacted into small pellets or noodles. These pellets or noodles are then ready for soap finishing, the process of converting raw soap pellets into a saleable product, usually bars.

)oap pellets are combined with fragrances and other materials and blended to homogeneity in an amalgamator #mixer(. The mass is then discharged from the mixer into a refiner, which, by means of an auger, forces the soap through a fine wire screen. *rom the refiner, the soap passes over a roller mill #*rench milling or hard milling( in a manner similar to calendering paper or plastic or to making chocolate li+uor. The soap is then passed through one or more additional refiners to further plastici,e the soap mass. Immediately before extrusion, the mass is passed through a vacuum chamber to remove any trapped air. It is then extruded into a long log or blank, cut to convenient lengths, passed through a metal detector, and then stamped into shape in refrigerated tools. The pressed bars are packaged in many ways.

')4ul e branco soap( E ) bar of blue,!hite soap )and or pumice may be added to produce a scouring soap. The scouring agents serve to remove dead cells from the skin surface being cleaned. This process is called

exfoliation. -any newer materials that are effective, yet do not have the sharp edges and poor particle si,e distribution of pumice, are used for exfoliating soaps. .anoscopic metals are commonly added to certain soaps specifically for both colouration and antibacterial properties. Titanium dioxide powder is commonly used in extreme /white/ soaps for these purposes0 nickel, aluminium, and silver compounds are less commonly used. These metals exhibit an electron1robbing behaviour when in contact with bacteria, stripping electrons from the organism2s surface, thereby disrupting their functioning and killing them. )ince some of the metal is left behind on the skin and in the pores, the benefit can also extend beyond the actual time of washing, helping reduce bacterial contamination and reducing potential odours from bacteria on the skin surface.3

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