Method for purifying long chain dicarboxylic acid in fermentation broth

The technology of a long-chain dicarboxylic acid and a purification method is applied in the purification field of long-chain dicarboxylic acid, and can solve the problems of low yield of dicarboxylic acid product, complicated operation steps, low alkane recovery rate, etc., and avoid production safety. and environmental pollution, shorten the process flow, high purity effect

Active Publication Date: 2017-04-05
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 dicarbo

Method used

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  • Method for purifying long chain dicarboxylic acid in fermentation broth

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Example Embodiment

[0027] Example 1

[0028] Using n-dodecane as a substrate, candida tropicalis is used to ferment to produce dodecanedicarboxylic acid. At the end of the fermentation, the dicarboxylic acid concentration was 164.3g / L and the pH was 7.4. Take 1000ml of fermentation broth, add 5% by mass potassium dihydrogen phosphate to the fermentation broth, stir to dissolve the inorganic salt, continue to stir and add 10% by mass NaOH solution until the system pH=10, and the mixing time is 100min. Let stand for 60 minutes to recover the unreacted alkanes in the upper layer, with a membrane pore size of 10 -2 Filter with a μm filter membrane to remove bacterial cells and debris. Add polyethylene glycol with a mass fraction of 5% and a molecular weight of 4000 to the system, and stir to dissolve the polymer to form an aqueous two-phase system. The system is sent to the supergravity equipment for supergravity treatment, the supergravity level is 150g, the average residence time of supergravity tr...

Example Embodiment

[0029] Example 2

[0030] Using n-dodecane as a substrate, candida tropicalis is used to ferment to produce dodecanedicarboxylic acid. At the end of the fermentation, the concentration of dicarboxylic acid was 158g / L and the pH was 7.3. Take 1000ml of fermentation broth, add 10% dipotassium hydrogen phosphate to the fermentation broth, stir to dissolve the inorganic salt, continue to stir and add 20% NaOH solution, until the system pH=12, stirring and mixing time 120min . Let stand for 80 minutes to recover the unreacted alkanes in the upper layer, with a membrane pore size of 10 -2 Filter with a μm filter membrane to remove bacterial cells and debris. Add polyethylene glycol with a mass fraction of 10% and a molecular weight of 10,000 to the system, and stir to dissolve the polymer to form an aqueous two-phase system. The system is sent to the supergravity equipment for supergravity treatment, the supergravity level is 200g, the average residence time of the supergravity trea...

Example Embodiment

[0031] Example 3

[0032] Using n-tridecane as a substrate, Candida tropicalis is used to ferment to 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 fermentation broth, add 15% ammonium sulfate to the fermentation broth, stir to dissolve the inorganic salt, continue to stir and add 30% NaOH solution until the system pH=12, and stir and mix for 20min. Let stand for 100 minutes to recover the unreacted alkanes in the upper layer, with a membrane pore size of 10 -2 Filter with a μm filter membrane to remove bacterial cells and debris. Add polyethylene glycol with a mass fraction of 12% and a molecular weight of 20,000 to the system, stir to dissolve the polymer, and form an aqueous two-phase system. The system is sent to the supergravity equipment for processing, the supergravity level is 300g, the average residence time of the supergravity treatment is 3s, the system after the su...

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Abstract

The invention discloses a method for purifying long chain dicarboxylic acid in fermentation broth. The method comprises the following steps: (I) adding inorganic salts and an alkali solution into fermentation broth, and stirring to dissolve the inorganic salts, wherein under the synergistic effect of alkali and salts, the cell wall of bacteria are dissolved, broken, and demulsified; (II) allowing the system to stand still to carry out layering, removing solid impurities such as bacterium dregs, and recovering alkane; (III) adding a proper amount of polyglycol into the fermentation broth, and dissolving the polymer to prepare a dual water phase system; (IV) subjecting the obtained dual water phase system to a super gravity treatment, wherein after the super gravity treatment, the upper phase and the lower phase are rapidly separated, proteins and pigments are dissolved in the upper phase, and the product (dicarboxylate salts) is dissolved in the lower phase; and (V) acidifying the lower phase obtained in the step (IV) to precipitate dicarboxylic acid crystals, and performing cooling, filtering, water washing, and drying to obtain a refined dicarboxylic acid product. A dual water phase extraction technology and a super gravity technology are combined to refine long chain dicarboxylic acid, the technical flow is shortened, the investment of equipment, time, and energy is saved, and the refined product has the advantages of high purity and low content of total nitrogen.

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 microbial 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 ...

Claims

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Application Information

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IPC IPC(8): C07C55/21C07C55/02C07C51/42C07C51/487C07C51/50C07C51/48
CPCC07C51/42C07C51/48C07C51/487C07C51/50C07C55/21
Inventor 李晓姝高大成师文静张霖樊亚超
Owner CHINA PETROLEUM & CHEM CORP
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