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Long chain organic acid refining method

A refining method and organic acid 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 impact, and achieve the effect of less material consumption, low energy consumption, and simple process

Active 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 monobasic 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 refining method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 200ml of C fermented by Candida tropicalis 12 h 22 o 4 Fermentation broth with a concentration of 160 g / l. Heat to 80°C, let it stand for 2 hours, remove the liquid wax remaining in the solution, filter and remove the bacteria, and obtain C 12 h 22 o 4 Fermentation serum, with H 2 SO 4 Adjust the pH value to 3.0 and heat to obtain organic acid crystallization liquid.

[0032] Put the obtained C 12 h 22 o 4 Organic acid crystallization liquid and n-propyl ether (n-propyl ether and C 12 h 22 o 4 The weight ratio is 7:1) Heat and mix until the organic acid crystals are completely dissolved in the solvent phase (dissolution temperature 80°C), add 0.65 g trinitrophenol to the mixed solution, continue heating and stirring at the dissolution temperature for 20 minutes, and stand still for 60 minutes. Separate 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 ac...

Embodiment 2

[0034] Take 200ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Organic acid fermentation broth with a concentration of 164g / l. Heat to 85°C with H 2 SO 4 Adjust the pH value to 3.5, 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.

[0035] 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) mixed and heated to 90°C, add 1.5g trinitrophenol to the mixture, continue heating and stirring at 90°C for 30min, then stand still for 30min, separate the lower layer of water phase (the sedimented bacteria and The salt complex precipitation generated by the reaction will be removed with water separation); 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 for decolorizati...

Embodiment 3

[0037] 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 80°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.

[0038] 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 3:1) and mix, add 0.95g trinitrophenol to the mixture, continue to heat and mix at 98°C for 40min, then stand still for 60min, then separate the lower aqueous phase; then add 60ml deionized water to the solvent phase Wash the organic phase and separate the water phase again; add 0.15 g of activated carbon to the organic phase for decolorization for 30 minutes,...

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Abstract

The invention discloses a fermentation organic acid refining 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 trinitrophenol, 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 refined organic acid product. The method uses the ether organic solvent and trinitrophenol to refine 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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IPC IPC(8): C07C55/02C07C51/42
CPCC07C51/48C07C55/02
Inventor 李晓姝高大成师文静张霖黎元生王领民
Owner CHINA PETROLEUM & CHEM CORP
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