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A method for extracting and refining long-chain dicarboxylic acids from fermentation broth

A long-chain dicarboxylic acid and fermentation broth technology, which is applied in the separation/purification of carboxylic acid compounds, carboxylate preparation, chemical instruments and methods, etc., and can solve the problems of high energy consumption and large loss of dicarboxylic acids , to achieve the effect of good product quality, improved solubility, and small crystal particles

Active Publication Date: 2021-08-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both of the above two schemes adopt the method of solvent extraction and refining on the basis of extracting crude acid. Although the quality of the obtained dicarboxylic acid is obviously improved, the process of dicarboxylic acid is dissolved in water phase, acid precipitation and precipitation, and drying and dehydration. , Organic phase heating up and dissolving, cooling down to precipitate, drying and other multi-step operations, through three heating up processes, the energy consumption is high and the loss of dicarboxylic acid is large

Method used

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  • A method for extracting and refining long-chain dicarboxylic acids from fermentation broth

Examples

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Effect test

Embodiment 1

[0030] (1) Take 0.5m of dodecyl dicarboxylic acid fermentation liquid 3 Add to 1m3 In a closed container with stirring, add potassium hydroxide to the fermentation broth to make the pH of the fermentation broth 9, stir at 100rpm, continue to heat up to 90°C, and keep the temperature constant for 20min;

[0031] (2) After the treatment in step (1), filter through a 20 nm membrane filtration device to obtain the fermentation clear liquid into 0.7m 3 In the fermentation clear liquid tank, let it stand at a constant temperature of 80°C for 20 minutes, and remove the aqueous phase clear liquid layer;

[0032] (3) Inject 380L aqueous phase clear liquid layer into 1m 3 In a closed container with stirring and heating, add 100L butyl ether at a temperature of 80°C and a speed of 100rpm, and raise the temperature to 90°C; then add sulfuric acid to control the pH of the system to 5, raise the temperature to 97°C, and increase the speed to 200rpm until the system Medium and long chain d...

Embodiment 2

[0035] (1) Take 0.5m of thirteen carbon dicarboxylic acid fermentation broth 3 join 1 m 3 In a closed container with stirring, add potassium hydroxide to the fermentation broth to make the pH of the fermentation broth to 10, stir at 100 rpm, continue to heat up to 80 ° C, and keep the temperature for 30 minutes;

[0036] (2) After the treatment in step (1), filter through a 40nm membrane filtration device to obtain the fermentation clear liquid into 0.7 m 3 Fermentation clear liquid tank, let it stand at a constant temperature of 90°C for 20 minutes, and remove the aqueous phase clear liquid layer;

[0037] (3) Inject 380L aqueous phase clear liquid layer into 1m 3 In a closed container with stirring and heating, add 80L ethyl acetate at a temperature of 85°C and a speed of 150rpm, and heat up to 90°C; then add sulfuric acid to control the pH of the system to 4, heat up to 97°C, and increase the speed to 200rpm until The long-chain dicarboxylic acid is completely dissolved ...

Embodiment 3

[0040] (1) Take 0.5m of dodecyl dicarboxylic acid fermentation liquid 3 Add to 1m 3 In a closed container with stirring, add sodium hydroxide to the fermentation broth to make the pH of the fermentation broth 9.5, stir at 100rpm, continue to heat up to 90°C, and keep the temperature constant for 30min;

[0041] (2) After the treatment in step (1), filter through a 25nm membrane filtration device to obtain the fermentation clear liquid into 0.7m 3 Fermentation clear liquid tank, let it stand at a constant temperature of 80°C for 30 minutes, and remove the phase water phase clear liquid layer;

[0042] (3) Inject 350L aqueous phase clear liquid layer into 1m 3 In a closed container with stirring and heating, add 100L propyl ether at a temperature of 80°C and a speed of 100rpm, and raise the temperature to 85°C; then add sulfuric acid to control the pH of the system to 5, raise the temperature to 97°C, and increase the speed to 200rpm until the system Medium and long chain dic...

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Abstract

The invention relates to a method for extracting and refining long-chain dicarboxylic acids from fermentation broth, comprising (1) adding an alkaline pH regulator to the fermentation broth to control the pH of the system in an alkaline range, and heating; (2 ) to obtain the fermentation clear liquid by filtration, after standing and stratifying, take the aqueous phase clear liquid layer; (3) control the temperature of the aqueous phase clear liquid at 70-85°C, add organic solvents in proportion, and raise the temperature to 80-90°C; then add Acidic pH adjuster, control the pH of the system in the acidic range, raise the temperature to 90-100°C, until the long-chain dicarboxylic acid in the system is completely dissolved, let it stand and separate the water phase, filter and dry the organic phase After that, the refined product of long-chain dicarboxylic acid is obtained. The invention combines the solvent extraction and the acid precipitation process in one unit through temperature control while extracting the fermented serum by conventional demulsification, which simplifies the operation, realizes the recycling of the organic solvent, and is easier for large-scale production and application.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry, and in particular relates to a method for extracting and refining long-chain dicarboxylic acids from fermentation broth. Background technique [0002] Long chain dicarboxylic acids (Long chain dicarboxylic acids) refer to aliphatic dicarboxylic acids (DCn or DCA for short) containing more than 10 carbon atoms in the carbon chain, including saturated and unsaturated dicarboxylic acids. It is a fine chemical product with a wide range of industrial uses. It is the synthetic high-grade spices, high-performance nylon engineering plastics, high-grade nylon hot-melt adhesives, high-temperature dielectrics, high-grade paints and coatings, high-grade lubricants, cold-resistant plasticizers, resins, and pharmaceuticals in the chemical industry. and pesticides and other important raw materials. [0003] The preparation of long-chain dicarboxylic acids usually uses alkanes as substrates and is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/42C07C51/487C07C51/43C07C51/48C07C55/21C07C55/02
CPCC07C51/42C07C51/43C07C51/48C07C51/487C07C55/21C07C55/02
Inventor 张霖李晓姝樊亚超孙启梅廖莎师文静
Owner CHINA PETROLEUM & CHEM CORP
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