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A kind of refining method of fermented organic acid

A refining method and organic acid technology, which is applied in the field of obtaining high-purity organic acids, can solve the problems of complex operation process, large solvent consumption, and inability to obtain it, and achieve the effects of simple process, low material consumption, and low energy consumption

Active Publication Date: 2015-09-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the dibasic acid crude product obtained by this method is mixed and dissolved with a solvent, no operation steps such as filtration are taken to remove insoluble impurities. In this way, insoluble impurities must be adsorbed on the crystal surface during the cooling crystallization process, which affects the product purity and brings great harm to the application of the product. bad influence
Moreover, the solvent refining dibasic acid process in this method includes two solvent recrystallization operations, and the solvent consumption is relatively large, which increases the burden of solvent recovery and refining, resulting in a relatively complicated operation process, and the dibasic acid obtained by solvent purification. The highest purity of basic acid is only 98.75wt%. When the production fluctuates slightly, qualified products may not be obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take 200ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Organic acid fermented broth, fermented broth with a concentration of 160g / l. heated to 80°C with H 2 SO 4 Adjust the pH value to 3.0, let it stand for 2 hours, and remove the liquid wax remaining in the solution to obtain the C containing bacteria. 12 h 22 o 4 Organic acid crystallization solution.

[0033] C 12 h 22 o 4 Organic acid crystallization liquid and n-propyl ether (n-propyl ether and C 12 h 22 o 4The weight ratio is 7:1) After mixing, add 32g of 1wt% NaOH aqueous solution, heat to 85°C, stand still for 60min, and separate the lower aqueous phase; then add 30ml deionized water to the solvent phase to wash the organic phase, and then separate the water phase; then add 0.3g of activated carbon to the organic phase and keep it warm for 30min for decolorization, then filter to remove the activated carbon, and cool the decolorized organic phase to 30°C for crystallization to obtain C 1...

Embodiment 2

[0035] Take 200ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Organic acid fermented broth, fermented broth with a concentration of 160g / l. heated to 80°C with H 2 SO 4 Adjust the pH value to 3.0, let it stand for 2 hours, and remove the liquid wax remaining in the solution to obtain the C containing bacteria. 12 h 22 o 4 Organic acid crystallization solution.

[0036] C 12 h 22 o 4 Organic acid crystallization liquid and n-butyl ether (n-butyl ether and C 12 h 22 o 4 The weight ratio is 6:1) and mix, add 20g of 10wt% KOH aqueous solution to the mixed solution, mix and heat to 135°C, stand still for 60min, separate the lower aqueous phase; then add 50ml deionized water to the solvent phase to wash the organic phase, and again Separate the water phase; add 0.2 g of activated carbon to the organic phase and keep it warm for 30 minutes for decolorization, then filter to remove the activated carbon, and cool the decolorized organic phase to 30°C to crystall...

Embodiment 3

[0038] Take 200ml and get C by fermenting Candida tropicalis 13 h 24 o 4 Organic acid fermented broth, fermented broth with a concentration of 154g / l. Heat to 70°C, filter through a ceramic microfiltration membrane, remove bacteria and residual liquid wax to obtain a filtrate. Add H to the filtrate 2 SO 4 Adjust the pH to 2.4 and heat to 95 °C to give C 13 h 24 o 4 The organic acid crystallization solution was cooled to room temperature and filtered to obtain an organic acid filter cake.

[0039] Put the obtained C 13 h 24 o 4 Organic acid filter cake and n-butyl ether (n-butyl ether and C 13 h 22 o 4 The weight ratio is 2:1) mix, add 15wt% Na to it 2 CO 3 50g of aqueous solution, mixed and heated to 100°C, stood still for 60min, and separated the lower aqueous phase; then added 60ml of deionized water to the solvent phase to wash the organic phase, and separated the aqueous phase again; added 0.15g of activated carbon to the organic phase for decolorization for...

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PUM

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Abstract

The invention discloses a fermentation organic acid refining method. The method is as follows: I, heating for inactivation of a terminate fermentation liquid; II, performing acidification for separate out organic acids by crystallization to obtain an organic acid crystallization liquid; III, mixing the organic acid crystallization liquid or a water-containing organic acid filter cake obtained by filtering with an ether organic solvent to dissolve the organic acids, adding a proper amount of an alkaline solution, then separating an organic phase and a water phase; IV, after washing of the separated organic phase, adding an adsorbent, filtering and removing solids; V, cooling the organic phase obtained by the step IV until the organic acids are separated out by crystallization, filtering, and drying to obtain a refined organic acid product. According to the method, the ether organic solvent and the alkaline solution are used for organic acid refining, the technical process is shortened, equipment, time and energy consumption and other investments can be saved, a polymerization-level product with high purity and low total nitrogen content can be obtained, and the method is more suitable for industrial production.

Description

technical field [0001] The invention relates to a method for refining organic acids, in particular to a method for obtaining high-purity organic acids from fermentation broth. Background technique [0002] The general formula of the organic acid molecule referred to in the present invention 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 organic acid. [0003] At present, the market has very high requirements for the purity of this type of organic acid, especially for the polymerization gr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/48C07C51/47C07C51/43C07C55/21C07C55/02
CPCC07C51/43C07C51/47C07C51/48C07C55/02C07C55/21
Inventor 高大成李晓姝吴丹
Owner CHINA PETROLEUM & CHEM CORP