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A kind of purification method of long-chain dicarboxylic acid

The technology of a long-chain dicarboxylic acid and a purification method is applied in the purification field of long-chain dicarboxylic acid, which can solve the problems of low yield of dicarboxylic acid product, low alkane recovery rate, complicated operation steps, etc., and achieves equipment saving and purity. The effect of high and shortened process flow

Active Publication Date: 2018-04-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has cumbersome operation steps and high operation cost, and the yield of dicarboxylic acid product is too low, the purity is not high, and the recovery rate of alkane is low

Method used

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  • A kind of purification method of long-chain dicarboxylic acid

Examples

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Effect test

Embodiment 1

[0026] Using n-dodecane as substrate, use Candida tropicalis to ferment and produce dodecanedicarboxylic acid. At the end of the fermentation, the dicarboxylic acid concentration was 164.3 g / L and the pH was 7.4. Take 1000ml of fermentation broth, heat it to 80°C, let it stand for 2 hours, recover unreacted alkanes in the upper layer, and use a membrane with a pore size of 10 -2 Filter through a μm membrane to remove bacterial cells and debris. Add 5% polyethylene glycol with a mass fraction of 4000 molecular weight and 8% dextran with a molecular weight of 300 000 to the fermentation broth, and stir to dissolve each substance in the fermentation broth to form an aqueous two-phase system. Send the system into the high-gravity equipment for high-gravity treatment. The high-gravity level is 150g, and the average residence time of the high-gravity treatment is 5s. The system after the high-gravity treatment is left still for 20 minutes. The upper and lower phases are separated, ...

Embodiment 2

[0028] Using n-dodecane as substrate, use Candida tropicalis to ferment and produce dodecanedicarboxylic acid. At the end of the fermentation, the dicarboxylic acid concentration was 158 g / L and the pH was 7.3. Take 1000ml of fermentation broth, heat it to 95°C, let it stand for 2h, recover the unreacted alkanes in the upper layer, and use a membrane with a pore size of 10 -1 μm microfiltration membrane to remove bacterial cells and debris. 3% polyethylene glycol with a molecular weight of 20,000 and 5% dextran with a molecular weight of 500,000 were added to the fermentation broth, and stirred to dissolve each substance in the fermentation broth to form an aqueous two-phase system. Send the system into the high-gravity equipment for high-gravity treatment. The high-gravity level is 200g, and the average residence time of the high-gravity treatment is 8s. The system after the high-gravity treatment is left still for 30 minutes, the upper and lower phases are separated, and th...

Embodiment 3

[0030] Using n-tridecane as substrate, use Candida tropicalis to ferment and produce tridecanedicarboxylic acid. At the end of the fermentation, the dicarboxylic acid concentration was 154.3 g / L and the pH was 7.5. Take 1000ml of fermentation broth, heat it to 80°C, let it stand for 2 hours, recover unreacted alkanes in the upper layer, and use a membrane with a pore size of 10 -2 μm ultrafiltration membrane to remove bacterial cells and debris. 4% polyethylene glycol with a molecular weight of 10 000 and 6% dextran with a molecular weight of 400 000 were added to the fermentation broth, and stirred to dissolve the substances in the fermentation broth to form an aqueous two-phase system. Send the system into the high-gravity equipment for high-gravity treatment. The high-gravity level is 300g, and the average residence time of the high-gravity treatment is 3s. The system after the high-gravity treatment is left still for 30 minutes. The upper and lower phases are separated, a...

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Abstract

The invention discloses a method for purifying long-chain dicarboxylic acids, comprising: I. heating and inactivating the terminated fermentation liquid; II. removing solid impurities such as bacterial residues and recovering alkanes; III. adding an appropriate amount of polyethylene glycol to the fermentation liquid Alcohol and dextran, so that various substances are dissolved in the fermentation broth to form a two-phase system; IV, the above-mentioned two-phase system is subjected to high-gravity treatment, and the upper and lower phases of the mixed system are quickly separated after high-gravity treatment, and impurities such as proteins Soluble in the upper phase, the product dicarboxylate is dissolved in the lower phase; V, take the lower phase in step IV, acidify to separate out the dicarboxylic acid crystallization, cool, filter, and dry to obtain a refined dicarboxylic acid product. The method of the present invention adopts the combination of two-phase extraction and supergravity to treat the refined dicarboxylic acid, which not only shortens the process flow, saves equipment, time and energy consumption, but also can obtain a refined product with high purity and low total nitrogen content, which is more efficient. Suitable for industrial production.

Description

technical field [0001] The invention relates to a method for purifying long-chain dicarboxylic acids, in particular to a method for obtaining high-purity long-chain dicarboxylic acids from fermentation broth. Background technique [0002] The molecular formula of long chain dicarboxylic acid is C n h 2n-2 o 4 , where n is 10-18, which is a metabolite obtained by fermentation of microorganisms using liquid wax, etc. Its fermentation broth is a complex multiphase system, which contains unreacted carbon sources, microbial cells and debris, unused medium and metabolites, and microbial secretions, etc., especially containing a large amount of impurities such as proteins, pigments, and ash , have a strong impact on the purity and application of the product, and bring difficulties to the extraction and refining of this type of dicarboxylic acid. [0003] At present, the methods for extracting long-chain dicarboxylic acids are generally divided into solvent method and aqueous me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/21C07C55/02C07C51/42
Inventor 李晓姝高大成师文静姚新武樊亚超
Owner CHINA PETROLEUM & CHEM CORP
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