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Method for extracting and refining long-chain dicarboxylic acid from fermentation liquor

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

Active Publication Date: 2018-12-07
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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  • Method for extracting and refining long-chain dicarboxylic acid from fermentation liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) Take 0.5m of dodecyl dicarboxylic acid fermentation broth 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 di...

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 broth 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 dica...

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Abstract

The invention relates to a method for extracting and refining long-chain dicarboxylic acid from a fermentation liquor. The method comprises the following steps: (1) adding an alkaline pH regulator into the fermentation liquor to control the pH value of the system to be in an alkaline range, and carrying out heating; (2) carrying out filtering to obtain a fermentation clear liquid, carrying out standing and layering, and taking a water-phase clear-liquid layer; and (3) controlling the temperature of the water-phase clear liquid to be 70-85 DEG C, adding an organic solvent according to a ratio,carrying out heating to 80-90 DEG C, then adding an acidic pH regulator to control the pH value of the system to be in an acidic range, carrying out heating to 90-100 DEG C until long-chain dicarboxylic acid in the system is completely dissolved, carrying out standing and layering to separate out a water phase, filtering an organic phase and performing drying to obtain a long-chain dicarboxylic acid refined product. According to the method disclosed by the invention, the fermentation clear liquid is extracted by conventional demulsification, and the solvent extraction and acidification processes are combined and completed in one unit through temperature control, so that the operation is simplified, cyclic use of the organic solvent is realized, and large-scale production and application are easier.

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 Applications(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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