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Purification method for glacial acetic acid

A purification method, the technology of glacial acetic acid, applied in the separation/purification of carboxylic acid compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of long time and low purity, and achieve stable quality, high purity, and high yield Effect

Inactive Publication Date: 2012-10-24
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by this invention is to provide a kind of purification method of glacial acetic acid, to overcome the low purity of glacial acetic acid purification product in the prior art, the deficiency that the time is long

Method used

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  • Purification method for glacial acetic acid

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Effect test

Embodiment 1

[0019] Preparation of tetraacetylborax: heat boric acid and acetic anhydride with a mass ratio of 1:5 to 60°C, then cool and filter to prepare tetraacetylborax.

[0020] Add 1000g of industrial glacial acetic acid into a 2000ml three-neck flask equipped with a rectification device, a thermometer and a heating device, add 40g of acetic anhydride and 20g of potassium permanganate in sequence, heat and reflux for 2 hours to remove organic impurities in the glacial acetic acid, and then add 30g of tetraacetylborax was heated under reflux for 0.5h, dried, and then 40g of 4A molecular sieve was added for adsorption and purification for 20min. Finally, 909g of purified glacial acetic acid was obtained by rectification at a flow rate of 20mL / min, with a yield of 90.9% and a purity of 99.82%.

Embodiment 2

[0022] Preparation of tetraacetylborax: heat boric acid and acetic anhydride with a mass ratio of 1:4 to 50°C, then cool and filter to prepare tetraacetylborax.

[0023] Add 1000g of industrial product glacial acetic acid into a 2000ml three-neck flask equipped with a rectifying device, a thermometer and a heating device, add 50g of acetic anhydride and 35g of potassium permanganate in turn, heat and reflux for 2.5h to remove organic impurities in the glacial acetic acid, and then Add 40g of tetraacetylborax, heat and reflux for 0.75h, dry, then add 50g of 4A molecular sieve for adsorption and purification for 25min, and finally carry out rectification and collection at a flow rate of 15mL / min to obtain 916g of purified glacial acetic acid, with a yield of 91.6% and a purity of 99.87%. .

Embodiment 3

[0025] Preparation of tetraacetylborax: Heat boric acid and acetic anhydride with a mass ratio of 1:6 to 70°C, then cool and filter to prepare tetraacetylborax.

[0026] Add 1000g of industrial glacial acetic acid into a 2000ml three-necked flask equipped with a rectifying device, a thermometer and a heating device, add 60g of acetic anhydride and 50g of potassium permanganate in sequence, heat and reflux for 3 hours to remove organic impurities in the glacial acetic acid, and then add 50g of tetraacetylborax was heated and refluxed for 1 hour, dried, then added with 60g of 4A molecular sieves for adsorption and purification for 30 minutes, and finally collected by rectification at a flow rate of 10mL / min to obtain 929g of purified glacial acetic acid with a yield of 92.9% and a purity of 99.95%.

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Abstract

The invention discloses a purification method for glacial acetic acid. The method uses industrial grade glacial acetic acid as raw material, acetic anhydride and potassium permanganate are added in turn and heated and refluxed, and then tetraacetyl borax for drying and 4A molecular sieve for adsorption purification are added in turn; at last, purified glacial acetic acid is obtained by distillation method. The purity of the glacial acetic acid obtained by the purification method of the invention is greater than 99.8%. Compared with the prior art, the purification process of the method is safe, simple, energy-saving and emission-reducing. The added raw material of purification agent can be recycled after treatment, and the requirements of green chemical industry and environmental protection are met. The glacial acetic acid product obtained by the purification method has the advantages of stable quality and high purity, and has prospect for industrial production.

Description

technical field [0001] The invention relates to a method for purifying glacial acetic acid, in particular to a method for purifying glacial acetic acid with acetic anhydride, potassium permanganate, tetraacetylborax and 4A molecular sieves. Background technique [0002] Glacial acetic acid widely exists in nature. It is an organic compound, a typical fatty acid, and the source of sour and pungent odor in vinegar. In households, a dilute solution of glacial acetic acid is often used as a descaling agent. In the food industry, glacial acetic acid is an acidity regulator specified in the food additive list E260. Pure glacial acetic acid is a colorless hygroscopic liquid with a freezing point of 16.6°C (62°F) and turns into colorless crystals after solidification. Although a weak acid based on its ability to dissociate in aqueous solutions, glacial acetic acid is corrosive and its vapors are irritating to the eyes and nose. Glacial acetic acid is also used to make cellulose a...

Claims

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Application Information

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IPC IPC(8): C07C53/08C07C51/42C07C51/487
Inventor 王伟顾小焱吕明王永旗
Owner TAICANG HUSHI REAGENT
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