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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, organic chemistry, etc., can solve the problems of increased operation steps, limited purification effect, and insufficient yield, so as to simplify the operation process, improve the effect, and ensure Effect of Purity and Yield

Active Publication Date: 2015-07-01
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN 102746136 discloses a kind of purification method of acetic acid, and its method comprises adopting potassium permanganate to carry out oxidation, acetic anhydride to absorb water, tetraacetic acid borax to carry out drying etc., in this method, owing to potassium permanganate, acetic anhydride and tetraacetic acid borax Addition, it is unavoidable to introduce a small amount of new impurities, and it will increase the operation steps of separating these additions in the later stage, resulting in material loss, the yield is not high enough, and the final purification effect is limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Contact 1000g of crude glacial acetic acid (technical grade glacial acetic acid) with ozone made from air (the amount of ozone is 30ppm based on the crude glacial acetic acid) in a fixed-bed reactor with 1g of manganese dioxide at 20 to 50°C for 15 minutes. Then, use 40g ZSM-5 molecular sieve to adsorb for 30min. Finally, after the product obtained by the adsorption is added with trimethylamine, it is placed in a rectification device for rectification at 20 / min. This example collected 931g of glacial acetic acid, the yield was 93.1%, and the tested purity was 99.90%.

Embodiment 2

[0023] Contact 1000g of crude glacial acetic acid (technical grade glacial acetic acid) with ozone made from air (the amount of ozone is 500ppm based on the crude glacial acetic acid) in a fixed bed reactor with 50g of manganese dioxide at 20 to 50°C for 5 minutes. Then, use 60g ZSM-5 molecular sieve to adsorb for 30min. Finally, after the product obtained by the adsorption is added with trimethylamine, it is placed in a rectification device for rectification at 20 / min. This example collects 938g of glacial acetic acid, and the yield is 93.8%, and the tested purity is 99.92%.

Embodiment 3

[0025] 1000g of crude glacial acetic acid (technical grade glacial acetic acid) was contacted with 24g of manganese dioxide at 20 to 50°C for 10 minutes in a fixed-bed reactor equipped with ozone made from air (the amount of ozone was 500ppm based on the crude glacial acetic acid). Then, use 40g ZSM-5 molecular sieve to adsorb for 30min. Finally, after the product obtained by the adsorption is added with trimethylamine, it is placed in a rectification device for rectification at 20 / min. This example collects 942g of glacial acetic acid, and the yield is 94.2%, and the tested purity is 99.94%.

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PUM

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Abstract

The invention discloses a purification method for glacial acetic acid, which comprises the following steps: (1) treating crude glacial acetic acid by ozone contact to obtain a purified product; (2) adsorbing the purified product with a ZSM-5 molecular sieve; and (3) adding aliphatic tertiary amine or lactam into a product obtained after adsorption, placing the product and the aliphatic tertiary amine or lactam into rectification equipment, and rectifying the product and the aliphatic tertiary amine or lactam. According to the purification method, carbonyl impurities and other unsaturate and iodide impurities in the crude glacial acetic acid are removed by ozone contact first, then complexes or oxides formed by the carbonyl impurities, other unsaturate and iodide impurities and ozone are separated from acetic acid by the ZSM-5 molecular sieve, and finally the aliphatic tertiary amine or lactam is adopted as an extraction agent for rectification to improve the rectification effect. According to the method, operation procedures are simplified, the operation process is environment-friendly and the purity and yield of the product are guaranteed.

Description

technical field [0001] The invention relates to the technical field of glacial acetic acid purification, in particular to a purification method of glacial acetic acid. 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 and becomes a colorless crystal 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 acetate for motion picture film and polyvinyl acetate in wood adhesives, as well as...

Claims

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Application Information

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IPC IPC(8): C07C53/08C07C51/42
CPCC07C51/42C07C53/08
Inventor 王永旗王伟吕明陈晓锋
Owner TAICANG HUSHI REAGENT
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