Section 3 ChE A

Group No 6

Date Performed: August 18, 2014

Date Submitted: November 7, 2014

Experiment No. 5
Soap Making: Kettle Process
Introduction
Soaps are cleaning agents that are made by reacting alkali with naturally
occurring fat. They are sodium and potassium salts of fatty acids which are saturated or
unsaturated aliphatic carboxylic acids, most of which occur in nature. In the technical
advancement of the twentieth century, a wide assortment of soap products has
developed during the course of time, it would now be impossible to imagine everyday
life in the absence of soap. Even at the start of the twenty-first century, the future of the
good old soap seems to be quite secured. The classical boiling process with live steam
(that induced boiling) in kettles or pans for many decades is still considered as the most
important method of soap-making and the process is still employed in some soap
factories.[1] Soaps have been remarkably useful as it has been improving the cleaning
process by lifting stains from bodies and also possessions.
In soap-manufacture terminology, Saponification is understood to denote simply
the formation of soap. Neutral Oil Saponification is the process of saponification of a
charge of suitable fats and oils with sodium hydroxide solution. [2] The reaction in this
process is a base, usually NaoH or KOH, hydrolysis of triglyceride that produces three
salts and Glycerol.

Figure1. Saponification Reaction

The crystallization of the molecules differs with the dependence on the base
used. NaOH produces a harder soap bar while KOH produces a softer bar, KOH is also
used more frequently for liquid soaps. Two most commonly methods are used to make
soap at home, Cold process and Kettle process. Both of these methods require a
source of heat to work with and careful calculations to make sure that no base would be
left unreacted in the soap. This experiment aims to perform kettle process using the
procedure for home-made production. Also, this experiment aims to further understand
the process of Saponification.
Methodology
The mass of NaoH needed to saponify 250ml of the oil was computed by the
researchers, basing on the saponification value of the oil. A NaOH solution was made
and added slowly to the oil in hot water bath. The temperature of the solution was
maintained from 60C to 70C and continuous stirring was done for homogenization. A
preparation of a salt solution was done; 25g of sodium chloride (NaCl) was dissolved in
150ml of distilled water. A test was done for the completion of the saponification
process; the researchers tested the fat solution by placing a few drops of the solution in
a test tube of deionized water. The indication of fat droplets floating to the top signified
that the reaction was not yet complete and the solution was allowed to be boiled for
another 10 minutes. After judging the completion of the reaction, the researchers poured
the hot reaction mixture into the salt solution. The mixture was cooled and stirred for 2
minutes. A filtration procedure was done. With a ratio of 5 parts soap: 1 part water, the
mixture was dissolved and heated in a water bath until a trace was found. Additives,
colorant, scent and herbal extract, were added by the researchers to improve the
product before placing it in a moulder.

Results and Discussion

Saponification is the hydrolysis of the fatty acid esters under basic conditions. A
process where Triglycerides are reacted with a strong base such as sodium hydroxide
or potassium hydroxide to form an alcohol and salt of a carboxylic acid.[3]
+ R' OH
RCO O
RCOO R' +O H
Fats and oils can be classified under the group called Triglycerides, they are the
tri-esters of fatty acids. Common vegetable oils that are used in manufacturing soap
are palm oil, olive oil and coconut oil. Each of these oils contains different fatty acid
content which results in different types of soap produced. In this experiment, the
researchers prepared soap from Coconut oil.
Coconut oil
Kettle Process
Amount of oil
250.7g
Saponification Value of oil
191
Theoretical weight of soap
492.66g
Experimental weight of soap
374.96g
Percent Yield
76.11%
Table 1. Data for Kettle Process

mass of NaOH pellets needed : Xg NaoH =

191 ( 250 g fat )

1000

Xg NaoH =47.75 g
mass of H 2 O :47.75 g NaOH (3 )=Xg H 2 O
Xg H 2 O=143.25mL
The researchers first calculated the amount of NaOH needed to react with 250ml
of oil. In order for the reaction to undergo completion an appropriate amount of NaOH
would be needed so it is necessary to determine the amount of NaOH before
proceeding with the experiment. The researchers also determined the amount of water
needed to dissolve the pellets. The mass of sodium hydroxide pellets needed was
47.75g and the water needed to dissolve the pellets was 143.25mL. Determining the

definite amounts needed reduces the possibility of errors, one of which is the impurity
that may be excess hydroxide or unreacted fat in the product.
A calculation of the theoretical value of weight of the product was made by the
researchers, the experimental value of the weight of the product was determined. A
comparison was done in order to determine the efficiency of the production. The
researchers determined that the maximum amount of product that can be produced was
492.66g, the actual yield after the experiment was 374.96g. The percent yield was
determined to be 76.11%. There may be issues involved as to the percent yield that was
obtain by the researchers. The treatment of materials are never perfect, particularly
transfer of reactants or products from one container to another. The filtration procedure
might also had an effect on the loss, the researchers might not have maximized the
amount of product extracted after the filtration.

47.75 g NaoH

1 mol
3 mol soap 222.0317 g

40 g NaoH 3 mol NaoH 1 mol soap

265.0503
=492.66 g soap (theo)
0.538
Percent Yield=

374.96
100=76.11
492.66

Analysis on the Physico-Chemical properties of soap was also performed by the

researchers. Physico-Chemical properties of soap determine the quality and efficiency
as a cleansing material. The soap was tested on different conditions and was compared
to the cold processed soap. Test solutions were made by the researchers for the soaps.
Tests such as Emulsifying property, behavior in hard water, Alkalinity, Cleansing power,
Lathering ability and reaction to mineral acids were done to both soaps.

Physico-Chemical Properties

Cold Process

Kettle Process

Test Solutions- Dissolve

Emulsifying Property

Palm Oil
Hard to dissolve
Present suds; no oil

Coconut Oil
Dissolves easily
Present suds; no oil

Behavior in Hard Water

Alkalinity
Cleansing Power
Lathering Ability
Lathering Ability + 1% Ca2+
Reaction with mineral acids

droplet; no scum
Large precipitate; no suds
1 drop
Washes out oil
Many Lather
Few lather; precipitate
4 drops; with more

droplets; no scum
Large Precipitate; no suds
1drop
Washes out oil more easily
Many Lather
Few lather precipitate
3 drops; with precipitate; 1

precipitate; scattered

Bulk precipitate

precipitate
Table 2. Physico-Chemical Properties of Cold Process and Kettle Process
The table shows that even though different oil and processes were used, the
results show that both soaps made from palm oil and coconut oil exhibit similar
properties. It would be better if same class of oil would be used so that comparison
would be more significant.

Answers to Questions
1. What is a micelle?
A micelle is formed when a variety of molecules including soaps and
detergents are added to water [5]. In these micelles, the carboxylate groups form
a negatively-charged spherical surface, wuth hydrocarbon chains inside the
sphere. Micelles remain dispersed in water and repel each other because they
are negatively charged.

2. What is emulsion? What is an emulsifying agent?

Emulsion is a type of dispersion in which two or more immiscible

substances are stabilized by another substance called emulsifier; an emulsifier is
capable of dispersing one liquid into another immiscible liquid. Soap has an
ability to act as an emulsifying agent, the soap in the mixture of oil or grease and
water would create an emulsion upon agitation.
3. Briefly describe how soap or detergent work to clean your body or to clean
other surfaces, such as dishes. Why are these agents (soap or detergent)
needed in order to have thorough cleaning?
Grease and oil are nonpolar and insoluble in water. When soap and
soiling oils are mixed, the nonpolar hydrocarbon portion of the micelles break up
the nonpolar oil molecules. The grease, oil and dirt attached to them are caught
inside the micelle, a different type of micelle then forms, with nonpolar soiling
molecules in the center which can be washed away by rinsing. The cleansing
action of both soaps and detergent results from their ability of emulsify water
insoluble materials (oil, grease, etc.) and hold them in suspension in water.
4. Differentiate soap from detergent in terms of effect to the environment.
Synthetic detergents were not non-biodegradable due to their
branched hydrocarbon chains. These detergents do not decompose within a few
days. On the other hand, soaps are biodegradable as they are single-chain
hydrocarbons which can be easily broken down within 5 days. Soap anion
molecules forms precipitates (soap scum) when exposed in hard water and this
may also persist on clothing. Synthetic detergents were developed in order to
cover up the failure of soap to work in hard water.
5. If saponification process is not complete, what are the expected impurities
that could be found in the finished product?
If the saponification process is not complete due to insufficient base,
time or heat, the soap product can be very brittle. The soap product may
impurities such as free caustic alkali, sodium chloride and residual glycerol
because of the incomplete conversion.
6. What is the role of the saline solution in the process above?

The role of saline solution in the process is it deprives the soap of

sufficient water to keep it soluble. The salt would react with water and act as a
solvent for the fatty acid salt.

Conclusion
All soaps are made from fats and alkaline solutions. Different kinds of fats, both
animal and vegetable, can produce different types of soaps. Soap is made in basically
the same way but a few modifications can be done in order to make the process more
efficient. Variation of soaps may also possess considerably different physicochemical
properties which can be applied on specific purposes. The objectives of the
experiment were met, though a few recommendations stated by the researchers. Th
researchers would like to recommend to use same class of oil so that the comparison
on the Physico-Chemical Properties of the soaps would be more relevant.

References
[1] Elvers,B. (2003) Ullmanns Encyclopedia of Industrial Chemistry. Wiley-VCH.
[2] Elvers,B. (2003) Ullmanns Encyclopedia of Industrial Chemistry. Wiley-VCH.
[3] http://chemistry.about.com/library/glossary/bldef825.htm
[4] http://www.elmhurst.edu/~chm/vchembook/558micelle.html