Purification method for long-chain dicarboxylic acid

A long-chain dicarboxylic acid and purification method technology, which is applied in the field of long-chain dicarboxylic acid purification, can solve the problems of low dicarboxylic acid product yield, low alkane recovery rate, cumbersome operation steps, etc., and achieve equipment saving and high purity Higher and shorter process flow effects

Active Publication Date: 2016-06-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Purification method for 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 polyethylene glycol with a mass fraction of 5% and a molecular weight of 4,000 and dextran with a mass fraction of 8% and 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 supergravity equipment for supergravity treatment, the supergravity level is 150g, the average residence time of the supergravity treatment is 5s, the system after the supergravity treatment is left still for 20min, the upper and lowe...

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. After the high-gravity treatment, the system is still for 30 minutes, the upper and lower phases are separated, and t...

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Abstract

The invention discloses a purification method for long-chain dicarboxylic acid. The purification method includes the steps: I, heating and inactivating a terminated fermentation liquid; II, removing bacterial residues and other solid impurities, and recycling alkanes; III, adding an appropriate amount of polyethylene glycol and glucan to the fermentation liquid, and making the substances dissolved in the fermentation liquid, to prepare an aqueous two-phase system; IV, carrying out hypergravity treatment of the aqueous two-phase system, allowing an upper phase and a lower phase of the mixed system after the hypergravity treatment to be rapidly separated, dissolving proteins and other impurities in the upper phase, and dissolving the product dicarboxylic acid salt in the lower phase; and V, taking the lower phase in the step IV, acidifying to make dicarboxylic acid crystallized and precipitated, cooling, filtering and drying to obtain a refined dicarboxylic acid product. The method adopts the aqueous two-phase extraction and hypergravity to be combined for treating and refining dicarboxylic acid, shortens the technological process, saves the investment of equipment, time and energy consumption and the like, also can obtain the refined product with high purity and low total nitrogen content, and is more suitable for industrialized 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 Applications(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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