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A method for extracting succinic acid diester from succinic acid fermentation broth

A technology for succinic acid diester and succinic acid, which is applied in the field of extracting succinic acid diester, can solve the problems of complex separation process of bio-based succinic acid, and achieve the effects of high purity and low production cost

Active Publication Date: 2018-12-11
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to propose a method for extracting succinic acid from succinic acid fermentation broth for the preparation of succinic acid diester in the prior art using pure succinic acid as raw material and the complicated separation process of bio-based succinic acid. Diacid diester method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take 100L of sodium salt fermentation broth with a succinic acid concentration of 45.0g / L and filter it through a 0.2μm microfiltration membrane and an ultrafiltration membrane with a molecular weight cutoff of 5000 Daltons to remove bacteria and large particle suspensions to obtain an ultrafiltrate 98L, the concentration was 45.3g / L, and the ultrafiltrate was concentrated until the mass concentration of succinic acid was 60%, to obtain 7.4L of concentrated solution. Mix the above concentrate with 12.0kg of methanol, add 2.5kg of sulfuric acid, stir at 58°C for 30 minutes, filter the precipitate containing sodium sulfate to obtain 19.0kg of esterified clear liquid, rectify at 0.05MPa to obtain butanediol with a purity of 99.2% Acid dimethyl ester 5.2kg.

Embodiment 2

[0028] Take 100L of sodium salt fermentation broth with a succinic acid concentration of 45.0g / L and filter it through a 0.2μm microfiltration membrane and an ultrafiltration membrane with a molecular weight cutoff of 5000 Daltons to remove bacteria and large particle suspensions to obtain an ultrafiltrate 98L, the concentration was 45.3g / L, and the ultrafiltrate was concentrated until the mass concentration of succinic acid was 60%, to obtain 7.4L of concentrated solution. Mix the above concentrate with 17.0kg of ethanol, add 2.5kg of sulfuric acid, stir at 58°C for 30min, filter the precipitate containing sodium sulfate to obtain 21.6kg of esterified clear liquid, rectify at 0.05MPa to obtain butanediol with a purity of 99.3% Acid diethyl ester 6.2kg.

Embodiment 3

[0030] Take 100L of sodium salt fermentation broth with a succinic acid concentration of 45.0g / L and filter it through a 0.2μm microfiltration membrane and an ultrafiltration membrane with a molecular weight cutoff of 5000 Daltons to remove bacteria and large particle suspensions to obtain an ultrafiltrate 98L, the concentration was 45.3g / L, and the ultrafiltrate was concentrated until the mass concentration of succinic acid was 60%, to obtain 7.4L of concentrated solution. Mix the above concentrate with 23.0kg of n-propanol, add 2.5kg of sulfuric acid, stir at 60°C for 30 minutes, filter the precipitate containing sodium sulfate to obtain 27.2kg of esterified clear liquid, and rectify at 0.03MPa to obtain 99.5% purity Di-n-propyl succinate 7.0kg.

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Abstract

The invention relates to a method for extracting succinic acid diester from succinic acid fermented liquid. The method comprises the following steps that the filtering working procedure is conducted on the succinic acid fermented liquid for removing thallus and large-particle suspended matter, and filtering liquid is obtained; the filtering liquid is subjected to concentration, and concentrated liquid is obtained; the concentrated liquid and alcohol are sufficiently contacted under the acid effect, the esterification and crystallization precipitation concerted reaction is conducted, and esterification and crystallization mixed liquid is obtained; crystals are removed from the esterification and crystallization mixed liquid, and crystal removing esterification clear liquid is obtained; and then rectification is conducted, and the succinic acid diester is obtained. According to the method for extracting the succinic acid diester from the succinic acid fermented liquid, the refining process of the succinic acid diester is omitted; and meanwhile, salts in the fermented liquid can be effectively removed, producing cost is low, prepared succinic acid diester products are high in purity and can be applied to synthetic light stabilizer, high-grade paint, bactericide, medical intermediates or butanediol generation after hydrogen is added.

Description

technical field [0001] The invention relates to a method for extracting succinic acid diester from succinic acid fermentation broth, belonging to the technical field of fine chemicals. Background technique [0002] At present, the production of succinic acid mainly adopts the chemical method of passing butane through maleic anhydride, which is expensive and seriously hinders the large-scale production of succinic acid. Compared with the chemical method, the anaerobic biological method using cheap renewable resources as raw materials to produce succinic acid has the characteristics of high atom economy, green process and low carbon emission reduction. It has been favored by the United States, Japan, South Korea and China. Widespread attention from national academic and industrial circles. Due to its two active carboxylic acid groups, succinic acid can undergo esterification reaction with alcohol to generate important succinic acid diester, and then synthesize light stabilize...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/40C07C67/08C07C67/54
CPCC07C67/08C07C67/54C07C69/40
Inventor 刘经伟方晓江李泽壮杨爱武王英武刘丽娟
Owner SINOPEC YANGZI PETROCHEM
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