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Method for obtaining high pure dicarboxylic acid

A technology of pure dicarboxylic acid and dicarboxylic acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of strict selection of refining equipment, inability to obtain qualified products, high operation and maintenance costs, and save The effect of drying equipment, low production cost and low material consumption

Inactive Publication Date: 2013-02-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the solvent method, only when acetic acid, ethylene glycol and ethyl acetate are used as solvents, the purity of dicarboxylic acid monoacid can be ≥98.5%, and the highest purity is only 98.75%. product
When acetic acid is used as the solvent at the same time, the material selection requirements for the refining equipment are strict, the operation and maintenance costs are high, and the reuse of acetic acid requires dehydration and other complicated refining processes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Get 200ml and obtain dodecanedicarboxylic acid by Candida tropicalis fermentation, concentration is the fermented liquid of 160g / l, with H 2 SO 4 Adjust the pH value to 3.0, heat to 80°C, let it stand for 2 hours, remove the liquid wax remaining in the solution, then lower it to room temperature, filter and wash to obtain a rough filter cake of dodecanedicarboxylic acid containing bacteria.

[0029] Mix the coarse filter cake of dodecanedicarboxylic acid containing bacteria and n-propyl ether (weight ratio: 1:10) and heat it to 90°C. After the filter cake is completely dissolved, let it stand still for 60 minutes. After separating the lower water phase, Add 1.6 g of activated carbon to the organic phase and keep it warm for 30 minutes for decolorization, then filter to remove the activated carbon, and the decolorized organic phase is cooled to 30° C. to crystallize to obtain dodecanedicarboxylic acid, and then undergo a drying step to obtain the product. The product qu...

Embodiment 2

[0032] Get 200ml and obtain dodecanedicarboxylic acid by Candida tropicalis fermentation, concentration is the fermented liquid of 160g / l, with H 2 SO 4 Adjust the pH value to 3.0, heat to 80°C, let it stand for 2 hours, remove the liquid wax remaining in the solution, then lower it to room temperature, filter and wash to obtain a rough filter cake of dodecanedicarboxylic acid containing bacteria.

[0033] Mix the coarse filter cake of dodecanedicarboxylic acid containing bacteria and n-butyl ether (weight ratio: 1:6) and heat it to 135°C. After the filter cake is completely dissolved, let it stand still for 60 minutes. After separating the lower aqueous phase, Add 1.6 g of activated carbon to the organic phase and keep it warm for 30 minutes for decolorization, then filter to remove the activated carbon, and the decolorized organic phase is cooled to 40° C. to crystallize to obtain dodecanedicarboxylic acid, and then undergo a drying step to obtain the product. The product q...

Embodiment 3

[0035] Get 200ml fermented by Candida tropicalis to obtain tridecanedicarboxylic acid with a concentration of 154g / l fermented liquid. Heat the terminated fermentation liquid at 70°C, filter through a ceramic microfiltration membrane, remove bacteria and residual liquid wax to obtain a clear liquid. Add sulfuric acid to the clear liquid to adjust the pH value to 2.4, and heat it to 95°C, then keep it warm for about 1 hour, then lower it to room temperature, filter and wash to obtain a crude acid filter cake.

[0036] Mix the obtained tridecanedicarboxylic acid coarse filter cake with n-butyl ether (weight ratio: 1:9) and heat to 100°C. After the filter cake is completely dissolved, let it stand still for 60 minutes. Add 1.54g of activated carbon to decolorize for 30min, then remove the activated carbon by filtration, and the decolorized organic phase is cooled to 18°C ​​to crystallize to obtain tridecanedicarboxylic acid, and then undergo a drying step to obtain the produc...

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Abstract

The invention relates to a method for obtaining high pure dicarboxylic acid. The method comprises the steps of I. heating a termination fermentation broth for inactivation; II. acidizing to make dicarboxylic acid crystallized and precipitated, and filtering to obtain a filter cake of dicarboxylic acid; III. mixing the filter cake of dicarboxylic acid and an ether solvent to make the dicarboxylic acid dissolved, separating an organic phase and a water phase, wherein the ether solvent is ether, n-propyl ether, iso-propyl ether, butyl ether, amyl ether or hexyl ether; IV. adding organic an adsorbent to the organic phase obtained from the step III, and filtering to remove solid materials; and V. cooling the organic phase obtained from the step IV until dicarboxylic acid is crystallized and precipitated, filtering to obtain a filter cake of crystallized dicarboxylic acid, and drying the filter cake of crystallized dicarboxylic acid to obtain a dicarboxylic acid product with a purity, by weight, higher than 98.5%. The method overcomes the shortages of complex operation, high production cost, low product purity, high colourity, high equipment investment and the like in a conventional refining method.

Description

technical field [0001] The invention relates to a method for purifying dicarboxylic acid, in particular to a method for obtaining high-purity dicarboxylic acid from fermentation broth. Background technique [0002] The general formula of the dicarboxylic acid molecule referred to in this patent is C n h 2n-2 o 4 (10≤n≤18), is a metabolite obtained by microorganisms using liquid wax fermentation. Its fermentation liquid is a complex multiphase system, which contains unreacted liquid wax, microbial cells and debris, unused medium and metabolites, and microbial secretions, etc., especially containing a large amount of impurities such as proteins and pigments. It affects the purity and appearance quality of the product, and brings difficulties to the extraction and refining of dicarboxylic acids. [0003] The purity requirements of dicarboxylic acids are very high in domestic and foreign markets, especially the purity requirements of polymeric dicarboxylic acids are higher. ...

Claims

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Application Information

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IPC IPC(8): C07C55/02C07C51/42
Inventor 高大成李晓姝
Owner CHINA PETROLEUM & CHEM CORP
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