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Long chain organic acid purifying method

An organic acid and organic phase technology, applied in the field of obtaining high-purity long-chain organic acids, can solve the problems of large solvent consumption, complicated operation process, and lack of availability, and achieve less material consumption, low energy consumption, and simple process. Effect

Inactive Publication Date: 2015-05-06
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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  • Long chain organic acid purifying method

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Take 200ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Organic acid fermentation broth, the concentration is 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), and heated to 80°C. After the organic acid is dissolved, add 16 ml of cetyltrimethylammonium chloride with a mass fraction of 0.05% to the mixture, mix well, and stand still for 60 minutes. , and remove the lower water 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 activated carbon to the organic phase and decolorize for 30min, then filter to remove the activated carbon, and the decolorized or...

Embodiment 2

[0035] Take 200ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Organic acid fermentation broth, the concentration is 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 heated to 93°C. After the organic acid is dissolved, add 6.4 ml of dodecyltrimethylammonium chloride with a mass fraction of 0.1% to the mixture, mix well, and stand still for 60 minutes. , and remove the lower water phase; then add 50ml deionized water to the solvent phase to wash the organic phase, and then separate the water phase; add 0.2g activated carbon to the organic phase and decolorize for 30min, then filter to remove the activated carbon, and the organic phase afte...

Embodiment 3

[0038] Take 200ml and get C by fermenting Candida tropicalis 13 h 24 o 4 Organic acid fermentation 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 24 o 4 The weight ratio is 2:1), and heated to 97°C. After the organic acid is dissolved, add 12.5 ml of tetradecyltrimethylammonium halide with a mass fraction of 0.3% to the mixture, mix well, and stand still for 60 minutes. Separate the lower water phase; then add 60ml of deionized water to the solvent phase to wash the organic phase, and then separate the water phase; add 0.15g of a...

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Abstract

The invention discloses a fermentation organic acid purifying method. The method comprises the following steps: 1, carrying out heating inactivation on a fermentation ending liquid; 2, acidifying to crystallize an organic acid in order to obtain an organic acid crystal liquid; 3, mixing the organic acid crystal liquid or a water-containing organic acid filter cake obtained after filtration with an ether organic solvent to dissolve the above organic acid, adding a proper amount of a cationic surfactant, and carrying out organic phase and water phase separation; 4, washing the separated organic phase, adding an adsorbent, and filtering to remove solids; and 5, cooling the organic phase obtained in step 4 to crystallize the organic acid, filtering, and drying to obtain a purified organic acid product. The method uses the ether organic solvent and the cationic surfactant to purify the organic acid, so the process flow is shortened, device, time and energy investment is saved, the polymer grade product with high purity and low total nitrogen content is obtained, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for refining long-chain organic acids, in particular to a method for obtaining high-purity long-chain organic acids from fermentation broth. Background technique [0002] The general formula of long-chain organic acids 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 grade. Generally, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/48C07C55/21C07C55/02
CPCC07C51/43C07C51/47C07C51/48C07C55/02C07C55/21
Inventor 李晓姝高大成张霖师文静王领民
Owner CHINA PETROLEUM & CHEM CORP
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