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Preparation of Ethyl
acetate
Date: 19-10-10
Muhammad Usman
(2008-chem-02-B)
1. Ethanol:
Harmful:
Pure Ethanol will irritate the skin and eyes. Nausea, vomiting and intoxication
are symptoms of ingestion. Long term use by ingestion can result in serious liver
damage. Death from Ethyl alcohol consumption is possible when blood alcohol
level reaches 0.4%.
A blood level of 0.5% or more is commonly fatal. Levels of even less than 0.1%
can cause intoxication, with unconsciousness often occurring at 0.3–0.4%
Highly flammable:
It has a flash point of 13 oC. It can readily catch fire. So care should be taken
while handling it because its combustion products include Acetaldehyde which
is a strongly carcinogenic substance. However, ethanol itself is not cancer
causing.
Properties of Ethanol:
2. Sulphuric acid:
Corrosive:
It is a strongly corrosive compound as it readily oxidizes anything.
Dangerous to Environment:
Although sulfuric acid is non-flammable, contact with metals in the event of a
spillage can lead to the liberation of hydrogen gas. The dispersal of acid aerosols
and gaseous sulfur dioxide is an additional hazard of fires involving sulfuric acid.
Very toxic:
Sulfuric acid is not considered toxic besides its obvious corrosive hazard, and the
main occupational risks are skin contact leading to burns and the inhalation of
aerosols. Exposure to aerosols at high concentrations leads to immediate and severe irritation of the eyes,
respiratory tract and mucous membranes.
Structure
Appearance
Irritant:
Skin Contact:
Excessive contact may cause irritation with blistering and redness. Solutions may
cause severe irritation or burns.
Eye Contact:
Contact may be corrosive to eyes and cause corneal destruction. Risk of serious
injury increases if eyes are kept tightly closed. Other symptoms may appear from
absorption of sodium carbonate into the bloodstream via the eyes.
Toxic:
Sodium carbonate is only slightly toxic, but large doses may be corrosive to the
gastro-intestinal tract where symptoms may include severe abdominal pain,
vomiting, diarrhea, collapse and death.
Inhalation:
Inhalation of dust may cause irritation to the respiratory tract. Symptoms from
excessive inhalation of dust may include coughing and difficult breathing.
Properties of Na2CO3:
Soda ash
Other names Washing soda
Soda crystals
Structure
Harmful:
Dilute acetic acid, in the form of vinegar, is harmless.
Flammable:
Concentrated acetic acid can be ignited with difficulty in the laboratory. It
becomes a flammable risk if the ambient temperature exceeds 39 °C (102 °F),
and can form explosive mixtures with air above this temperature (explosive
limits: 5.4–16%).
Corrosive:
Concentrated acetic acid is corrosive and must be handled with appropriate care,
since it can cause skin burns, permanent eye damage, and irritation to the
mucous membranes. These burns or blisters may not appear until hours after
exposure. Latex gloves offer no protection, so especially resistant gloves, such
as those made of nitrile rubber, are worn when handling the compound.
Properties of Glacial Acetic acid:
Glacial acetic acid is a trivial name for water-free acetic acid.
Structure
Chemicals Required:
1. C2H5OH 2. CH3COOH
3. H2SO4 (Concentrated) 4. Na2CO3 (30%)
Apparatus:
1. Round Bottom Flask 2. Condenser
3. Knee tube 4. Adopter
5. Separating funnel 6. Beaker
7. Conical flask 8. Wire gauze
Chemical Reaction:
C2H5OH + CH3COOH CH3COOC2H5 + H2O
Procedure:
1. Mix 25 ml of Ethanol & 25 ml of Glacial acetic acid thoroughly in a round bottom flask.
2. Add slowly with cooling & shaking 15 ml of concentrated H2SO4. Ensure that the liquid is
homogenous.
3. Fit the flask with a heat flux water condenser & boil the mixture gently over wire gauze for 10
minutes.
4. Now alter the position of the condenser & distill of about 2/3 of mixture. Then transfer the
distillate to a separating funnel.
5. Add about 12.5 ml of 30% Na2CO3 solution in separating funnel.
6. Cork the funnel & shake carefully in order to neutralize the free acetic acid & H2SO4.
7. Due to the addition of Na2CO3, CO2 will be formed which should be removed by removing the
cork at frequent intervals.
8. Two layers will be formed. Allow the two layers to separate & carefully run off & eject the lower
aqueous layer.
Uses of ethyl acetate:
1. Commercial uses:
In the field of Entomology, ethyl acetate is an effective chemical for use in insect collecting and study. In
a killing jar charged with ethyl acetate, the vapors will kill the collected (usually adult) insect quickly
without destroying it. Because it is not hygroscopic, ethyl acetate also keeps the insect soft enough to
allow proper mounting suitable for a collection.
2. Laboratory uses:
In the laboratory, mixtures containing ethyl acetate are commonly used in column chromatography and
extractions.
Feed tank:
The raw materials are first blended in correct proportion in a vessel called feed tank.
Pre-heater:
Raw materials in the form of a steady stream are fed to the esterifying column through a pre-heater unit.
Here the temperature of feed is increased.
Esterification column:
Feed is introduced into the column from side. Here via chemical reaction feed is converted into products
i.e. ethyl acetate along with some higher esters due to the presence of other acids as impurities along with
acetic acid.
From the top of the column the mixture is taken off whose composition is following.
Ester……………………….20%
Water……………………...10%
Alcohol……………………70%
Separating column:
The ternary mixture taken off passes to the separating column at point “B” here it is rectified by the
closed steam.
Separating tank:
These layers are separated out in separator tank. Watery portion overflows back to the lower portion of
the separating column where it is blended with alcohol and water accumulating in the base of the column.
The watery portion through a pipe “D” is fed to the Esterification column. On the lower plates of column,
the alcohol is exhausted and distills upward as vapor while the slop water goes to waste at “E”.
The washed ester, containing a little dissolved water and alcohol, overflows from the separator and enters
a drying column in which a sufficient amount is distilled off to carry with it water and alcohol.
2. Cooler:
3. Storage tank
References:
1. Unit processes in organic synthesis by P.H. Groggins
5th edition, page 729-730
2. Wikipedia
http://en.wikipedia.org/wiki/ethyl_acetate/