SYNTHESES OF SOAP AND DETERGENT

Francis Dimaandal, Inri Dumlao, Mark Kevin Eusebio

Dennis Giron and Pia Hipolito
Group 4 2A Biochemistry Organic Chemistry Laboratory

ABSTRACT
Synthesis of soap and detergent is the actual creation of soap and detergents itself. Soap is
any sodium or any potassium salt of fatty acids that is either derived from animal or vegetable
fat. Various methods such as saponification, where as fats are broken to form impure salts of
fatty acids and glycerol. This is simply known as crude soap, ready for further purification to
produce a commercially available soap in our homes and offices. In this experiment, to form
soap, has consumed the following solutions and solvents such as 30 mL 6M NaOH, 15 mL
coconut oil, 50 mL cold saturated NaCl solution. It is performed to synthesize soap and
detergents starting from oil and sodium hydroxide to form fatty acids and glycerol as well as
to compare the behavior of the soap and the detergent in hard water.

INTRODUCTION as soap is to water. The micelle’s “tail”

Soap is any salt of a fatty acid may extend or become highly
from the addition of alkali solution. As branched for as long as it still
tested, soap has a capability to bind to dissolves in non polar substances like
grease or any oils as stains in oil.[2]
garments. It serves as a surfactant in EXPERIMENTAL
conjunction to water. This function of A. Compounds, solvents, and
soap is attributed to micelles which solutions utilized and consumed.
have coats of polar carboxylate groups 20% of NaOH, 6M NaOH, concentrated
on the outside, encasing a hydrophobic H2SO4, 1% CaCl2, 1% MgCl2, solid
pocket that can surround any grease NaCl, saturated NaCl, phenolphthalein,
particles.[1] As of today, the most dodecanol (C12H25OH), vegetable oil
common way of creating soap is (coconut oil).
through the cold process method.
“Lye” soap is the common product of B. Procedure
this modern homemade soap DIAGRAM2. Reaction sequence for
production. The rational behind the oil soap
or grease is removed when the
garment stained with oil is dictated by
the “like dissolves like” principle.
Micelles’ explains this function in a
diagram.

DIAGRAM1. Micelles structure

As we all know water is polar and
by adding oil, a non polar substance, it
will not mix. By adding soap, which in
fact has bi-polar reactivity between
water and oil, oil and water will mix
through the suspension of oil in soap
1. Preparation of Soap
Prepare a mixture of 30 mL of 6M
NaOH and 50 mL of distilled water.
Transfer these into a 500 mL beaker,
heat using a small flame, and stir
frequently. Add a total amount of 15
mL coconut oil in the mix gradually
and heat for about 15 to 20 min. with
stirring, just to ensure that water is
replaced via evaporation. To test if the
saponification is complete, add a drop
of the mix into a milliliter of water. If
the mix still exhibits a presence of
coconut oil, heat again for 15 to 20
min. along with stirring. Test again;
expect that the mix is complete of
saponification. Stir until mix is
homogenous. Pour it into a 50 mL of
cold, saturated solution of NaCl while
still hot. As the soap forms, filter the
precipitated soap through a cheese
cloth. The filtrate, a liquid, is now
ready for glycerol test. Wash the
collected soap in 5 mL ice cold water
twice. Squeeze again to remove
excess water. Dissolve in an
evaporating dish, add 10 to 20 mL of
water to dissolve soap, and evaporate
into a jelly like consistency. Cool and
pour into a mold, and use this formed
soap in hard water behavioral test.
2. Extraction for Glycerol
Neutralize the filtrate, the liquid
collected from a repeated squeezing of
the soap, with diluted HCl. If it’s not
clear, filter it. Evaporate it into small
volume or a syrupy consistency and
allow cooling down. Extract the syrup
and add 95% ethanol then filter again.
Evaporate the alcoholic extract in a
water bath and now the residue that
remained has glycerol.
3. Glycerol test
To the residue, add a pinch of
potassium bisulfate (KHSO4). Heat the
mixture strongly, meaning, at high
temperatures. Take note of the odor
formed.
4. Preparation of Detergent
In preparing the detergent, place
5 mL of dodecanol (C12H25OH) into a
100 mL beaker. Add gradually a total
amount of concentrated H2SO4 while
stirring for about a min. after the acid
is completely added and let stand for
an additional 10 min. Mix well 5 mL 6M
NaOH with 10 mL of water and add 4
drops of phenolphthalein which may
begin to fade in the presence of a
strongly basic solution. After 10
minutes has passed, add it now to the
dodecanol- sulfuric acid mix and stir
until the tinge of phenolphthalein
disappears. There should be a large
amount of detergent formed.
Fill a 250 mL of one third of ice
and 10 g of NaCl and thoroughly mix.
Add water until it reaches a total
amount of 75 mL. Pour the detergent
mix to make it lump on the cold NaCl
ice mix. Then filter it in a three layered
cheese cloth. Wash the collected
detergent in two portions of water with
10 mL each portion. Then finally
squeeze to take of any excess water
and prepare for hard water behavioral
tests.
5. Hard Water Behavior
DIAGRAM3.
2C17H35COONa + Ca2+ →
(C17H35COO)2Ca + 2Na+
Above is an example of a reaction
mechanism of sodium stearate soap to
hard water.
Place 5 mL of both soap solution
and the detergent solution into two
test tubes each sample. Add 2 mL 1%
sdCaCl2 to detergent solution and soap
solution. Do the same to the rest of
the test tubes with 2 mL 1% MgCl2.
mix but not shake the mixtures and
note any precipitates formed if it does
so. Add now 4 drops of cooking oil to
each tube put a stopper and vigorously
shake the four tubes. Observe and
record any emulsifying ability of the
soap and detergent in each tube.
Indicate whether if formed suds as
heavy, light, few, or none at all.
RESULTS AND DISCUSSION Fatty acid or any of its derivatives
when burned, exhibits a burnt fat odor
TABLE1. Hard Water test w/ some but in this case, glycerol has a sweet
physical states taste and buttery odor when subjected
soap detergent to heating.
color and white white
appearance solidified solids
gelatin
solubility insoluble soluble
in 1% CaCl2 REFERENCES
solubility insoluble soluble
in 1% MgCl2 [1] en.wikipedia.org
emulsifying light suds more suds August 29, 2010
ability present
[2]chemlab.trueman.edu/
As seen from above, these are CHEMLAB100/SAPONIFICATION.pdf
the behaviors exhibited as the hard August 29, 2010
water test is performed. According to
these observations, soap slightly [3] Bayquen, A.V., Cruz, C.T., de Guia,
produces suds in hard water while R. M., Lampa, F.F., Pena, G.T., Sarile,
detergent can yield more. As a
A.S., Torres, P.C. (2009). Laboratory
personal experience, in Saudi Arabia, a
Manual in Organic Chemistry. C&E
tanker of water delivers cheap hard
water. As a result, soap scum builds publishing, Inc.
up on our containers and tiles. Taking
a bath is also difficult. Shampooing is
easy since it can be classified as a
detergent as well. But, as for soap, it
does not have any effect even on our
hands. A bypass to this occurrence is
adding baking soda into the water,
dissolving the soap scum that could
possibly develop. To the emulsifying
ability test in the laboratory, light suds
on soap indicate that calcium or
magnesium ions are still present in the
water. This is due to the high
reactivity of soap to ions. Unlike in
detergents, ions do not bother the
reaction, which is the main reason why
detergents works best in hard or soft
water unlike soaps, which only react
with soft waters.

Observations from the Glycerol

test:

As the potassium bisulfate is

added to the glycerol and heated, it
exhibited a sweet butter-like odor.
This indicates that a fatty acid
derivative is present in the mixture.