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Method for extracting hydroxyacetic acid from water solution mixture containing hydroxyacetic acid

A technology for extracting glycolic acid and glycolic acid, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of difficult recovery of ammonium sulfate from power consumption, limited application and development, and pollution of electrodialysis membranes. The extraction agent is convenient, the labor conditions are improved, and the separation efficiency is high.

Inactive Publication Date: 2008-09-17
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the separation of glycolic acid and ammonium sulfate is the key to whether this method can realize industrial production.
Some methods have been developed to separate such mixtures, such as the esterification hydrolysis method disclosed in Chinese patent CN17204504A, this method is to carry out esterification reaction with methanol or ethanol to generate glycolic acid methyl ester or ethyl glycolate ester, and then carry out rectification and purification to achieve the purpose of separating from the by-product ammonium bisulfate. The disadvantage of this method is that the loss of alcohol is large, a large amount of ammonium sulfate is produced by-product, and the production cost is high; membrane electrodialysis, this method can get High-purity glycolic acid products, but the problems of electrodialysis membrane pollution, power consumption and by-product ammonium sulfate recovery are difficult to solve, which largely limits its application and development

Method used

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  • Method for extracting hydroxyacetic acid from water solution mixture containing hydroxyacetic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The hydrolyzate containing glycolic acid with a concentration of 260g / L at a pH of 2.2 and the extractant containing 60% trioctylamine, 5% trioctyl phosphate, 15% n-octanol and 20% sulfonated kerosene by volume at Φ500mm , In a kühni tower with a height of 1000mm, at 30°C, the hydrolyzate is used as the continuous phase, and the extractant is used as the dispersed phase for countercurrent extraction, and the liquid-liquid interface is controlled below the outlet position of the upper part of the tower (ie, the upper interface of the tower). The speed of the turbine turntable is 650rpm, and the feed volume ratio of the hydrolyzate to the extractant is 1:1.75.

[0037] The concentration of glycolic acid in the extract phase output is about 135g / L, and the concentration of glycolic acid in the raffinate phase output is lower than about 18g / L. Based on the transfer of glycolic acid from the hydrolyzate to the extraction phase, the extraction rate is more than 93%.

[0038] ...

Embodiment 2

[0041] The hydrolyzate containing glycolic acid concentration of 285.7g / L at a pH of 1.9 and the extractant composed of 50% tri-n-octylamine, 10% trioctyl phosphate, 30% n-octanol and 10% sulfonated kerosene by volume In the kühni tower with Φ500mm and height of 1000mm, at 25°C, the extraction agent is used as the continuous phase, and the hydrolyzate is used as the dispersed phase for countercurrent extraction, and the liquid-liquid interface is controlled to be above the outlet of the lower part of the tower (that is, the upper interface of the tower). The speed of the turbine turntable is 600rpm, and the feed volume ratio of the hydrolyzate to the extractant is 1:1.5.

[0042] After the operation of the extraction tower is stable, the concentration of glycolic acid in the output of the extraction phase is about 128g / L, and the concentration of glycolic acid in the output of the raffinate phase is lower than 15g / L. Based on the transfer of glycolic acid from the hydrolyzate t...

Embodiment 3

[0046] The hydrolyzate containing glycolic acid concentration is 305.4g / L and the pH is 1.8 and the extractant that contains volume ratio 50% trin-octylamine, 10% trioctyl phosphate, 20% n-octanol and 20% sulfonated kerosene is formed in In the kühni tower with Φ1500mm and height 9000mm, at 20°C, the oil phase is used as the continuous phase, and the water phase is used as the dispersed phase for countercurrent extraction, and the liquid-liquid interface is controlled to be above the outlet of the lower part of the tower (ie, the upper interface of the tower). The speed of the turbine turntable is 200 rpm, and the feed volume ratio of the hydrolyzate to the extractant is 1:1.5.

[0047] After the operation of the extraction tower is stable, the concentration of glycolic acid in the output of the extraction phase is about 132g / L, and the concentration of glycolic acid in the output of the raffinate phase is lower than about 7g / L. The rate is above 97.7%.

[0048] The extractio...

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Abstract

The invention discloses a method of extracting glycolic acid from water solution mixture containing the glycolic acid. The method has the following steps: synergistic extraction agent is delivered into an extraction column from the bottom, the water solution mixture containing the glycolic acid is delivered into the extraction column from the top, extraction phase after extraction flows out of the upper part of the extraction column, and raffinate phase after extraction flows out of the lower part of the extraction column; the extraction phase flowing out of the upper part of the extraction column is delivered into a back-extraction column from the bottom; back-extraction water is delivered into the back-extraction column from the top of the back-extraction column; back-extraction water phase which flows out of the lower part of the back-extraction column is concentrated to obtain the glycolic acid; back-extraction organic phase flows out of the upper part of the back-extraction column. The method has the advantages that the technological process is simpler, the capacity of the organic phase is large, the production capacity of equipment is high, the extractant regeneration is convenient, the energy consumption during the process is small, and the manufacturing cost is low; the volatility of the extractant is small without toxicity, the emulsification is hard, the misphasing speed is high, and the separative efficiency is high; the operation is convenient and stable, and the product quality is high.

Description

technical field [0001] The present invention relates to a method for extracting glycolic acid from an aqueous solution mixture containing glycolic acid. Background technique [0002] Glycolic acid is a kind of fruit acid, also known as glycolic acid, glycylic acid or glycolic acid. It is an α-hydroxy acid with the simplest chemical structure. It is also an important fine chemical raw material. It is used in medical materials, special washing And cosmetics and other industries have a wide range of applications. [0003] Pure glycolic acid is a colorless, odorless, slightly hygroscopic translucent crystal. Most industrial products are 70% glycolic acid aqueous solution by weight, which is a light yellow liquid with a caramel-like smell. Glycolic acid in nature mainly exists in sugarcane, sugar beet and immature grape juice, its content is low, and it coexists complexly with other substances, so it is difficult to separate and purify. Currently, glycolic acid on the market i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/48C07C59/06
Inventor 施云海陈德兴孙后勇徐鹏坤曹海甬陈健敏
Owner EAST CHINA UNIV OF SCI & TECH
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