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Method for recovering glutaric acid from 7-ACA waste liquid

A 7-ACA, recovery method technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, ammonium halide and other directions, can solve problems such as interference with glutaric acid separation, achieve considerable economic benefits, create economic benefits, and the process is simple Effect

Active Publication Date: 2012-02-01
焦作健康元生物制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional method for recovering glutaric acid is not an ideal separation method for recovering glutaric acid from 7-ACA waste liquid with a large amount of ammonium chloride salt, and there are residual 7-ACA, MLL in the 7-ACA waste liquid -7-ACA impurity, both interfere with the separation of glutaric acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) Adjust the pH of 2000ml 7-ACA waste liquid to 2.5 with hydrochloric acid with a concentration of 5mol / L. At this time, glutaric acid forms acid, which increases the amount of by-product ammonium chloride and reduces the amount of other salts in the final waste liquid , then concentrated to 400ml, decolorized with 6g of activated carbon, then concentrated to 300ml, cooled to crystallize, filtered to obtain 55g of ammonium chloride by-product;

[0014] (2) The filtrate in step (1) was adjusted to pH 1.5 with 6mol / L sulfurous acid, then concentrated to 160ml, cooled to 0°C to crystallize, filtered to obtain 30g of crude glutaric acid;

[0015] (3) The crystals in the step (2) were recrystallized with diethyl ether, the crystal purity was 99%, and 25 g of glutaric acid was obtained.

Embodiment 2

[0017] (1) Adjust the pH of 2000ml 7-ACA waste liquid to 2.0 with hydrochloric acid with a concentration of 5mol / L. At this time, glutaric acid forms acid, which increases the amount of by-product ammonium chloride and reduces the amount of other salts in the final waste liquid , then concentrated to 800ml, decolorized with 4g of activated carbon, then concentrated to 260ml, cooled to crystallize, filtered to obtain 60g of ammonium chloride by-product;

[0018] (2) The filtrate in step (1) was adjusted to pH 1.0 with 6mol / L phosphoric acid, then concentrated to 160ml, cooled to 10°C to crystallize, filtered to obtain 35g of crude glutaric acid;

[0019] (3) Recrystallize the crystal in the step (2) with acetone, the crystal purity is 99%, and 22 g of glutaric acid is obtained.

Embodiment 3

[0021] (1) Adjust the pH of 2000ml 7-ACA waste liquid to 2.5 with hydrochloric acid with a concentration of 5mol / L. At this time, glutaric acid forms acid, which increases the amount of by-product ammonium chloride and reduces the amount of other salts in the final waste liquid , then concentrated to 600ml, decolorized with 8g of activated carbon, then concentrated to 240ml, cooled to crystallize, filtered to obtain 55g of ammonium chloride by-product;

[0022] (2) The filtrate in step (1) was adjusted to pH 1.5 with 6mol / L permanganate, then concentrated to 160ml, cooled to 0°C to crystallize, filtered to obtain 38g of crude glutaric acid;

[0023] (3) The crystals in the step (2) were recrystallized with ethyl acetate, the crystal purity was 99%, and 22 g of glutaric acid was obtained.

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Abstract

The invention discloses a method for recovering glutaric acid from 7-ACA waste liquid, comprising the following steps: (1) regulating the pH value of the 7-ACA waste liquid to 2.0-2.5 with hydrochloric acid, concentrating to 20-40 % of the original volume of the 7-ACA waste liquid, decoloring with active carbon, then concentrating to 12-15 % of the original volume of the 7-ACA waste liquid, cooling, carrying out crystallization, and filtering; (2) regulating the pH value of the filtrate obtained by the step (1) to 1.0-1.5 with inorganic acid, then concentrating to 8-11 % of the original volume of the 7-ACA waste liquid, cooling to 0-10 DEG C, carrying out crystallization, and filtering; and (3) carrying out recrystallization on the crystals with organic solvent. According to the invention, the white glutaric acid with the purity of more than 99 % can be obtained, and simultaneously, a large amount of ammonium chloride byproducts are recovered. The invention has the advantages of simple process, no need of special devices, no generation of new byproducts, and no secondary pollution to the environment.

Description

technical field [0001] The invention relates to a recovery method of waste liquid, in particular to a recovery method of glutaric acid in 7-ACA waste liquid. Background technique [0002] Glutaric acid is an extremely important chemical raw material, widely used in chemical industry, construction, medicine, agriculture and so on. Currently, glutaric acid is mainly recovered from the by-product of the production of adipic acid. The separation methods that have been developed include recrystallization, extraction, urea complexation, rectification, etc. Recrystallization is carried out under vacuum flash evaporation, which requires multiple crystallizations, long process routes, low yields, and high energy consumption The extraction method is complex and the water solubility of glutaric acid is large, so the extraction rate is low; the complex formed by the urea complexation method is relatively stable, and it is difficult to dissociate it by general methods; the rectification...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/16C07C51/42C07C55/12
Inventor 乔晓光王增霞江国华
Owner 焦作健康元生物制品有限公司