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A kind of refining method of 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 impurity content

Active Publication Date: 2016-08-17
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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  • A kind of refining method of organic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 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.

[0034] C 12 h 22 o 4 Organic acid crystallization solution and 4-heptanone (4-heptanone and C 12 h 22 o 4 The weight ratio is 6:1) and mixed, heated to 115°C. After the organic acid is dissolved, the mixed system is sent to the supergravity equipment heated to 115°C for supergravity treatment. The supergravity level is 50g, and the supergravity treatment The average residence time is 0.2s, and the mixed system treated by supergravity is stilled for 60min, and the lower aqueous phase is separated; then 30ml of deionized water is added to the solvent phase to wash the organic phase, and the aqueous phase is separat...

Embodiment 2

[0036] Take 200ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Organic acid fermentation broth with a concentration of 162g / l, adjust the pH to 10.0, heat to 80°C, let it stand for 2 hours, remove the liquid wax remaining in the solution, use microfiltration equipment to filter the lower layer solution to remove impurities such as bacteria to obtain a clear liquid, Add acid to the obtained clear liquid to adjust the pH value to 3.5, and heat to 80°C to obtain organic acid crystal liquid.

[0037] Put the obtained C 12 h 22 o 4 Organic acid crystallization solution and isobutyl acetate (isobutyl acetate and C 12 h 22 o 4 The weight ratio is 4:1) and mixed, heated to 95°C. After the organic acid is dissolved, the mixed system is sent to the supergravity equipment heated to 95°C for supergravity treatment. The supergravity level is 150g. The average residence time is 0.8s, and the mixed system treated by supergravity is static for 30min, and the lower aqueous ph...

Embodiment 3

[0039] 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.

[0040] Put the obtained C 13 h 24 o 4 Organic acid filter cake with dodecane (dodecane with C 13 h 24 o 4 The weight ratio is 8:1) and mix, heat the system to 98°C, after the organic acid is dissolved, send the mixed system into the supergravity equipment that has been heated to 98°C for supergravity treatment, the supergravity level is 300g, the supergravity The average residence time of the treatment is 5s, and the mixed system treated by supergravity is static for 40min, and the lower aqu...

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Abstract

The invention discloses an 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 an organic acid filter cake obtained after filtration with an organic solvent, carrying out hypergravity treatment, 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 organic solvent and the hypergravity treatment 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 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): C07C51/42C07C55/02C07C55/21
CPCC07C51/42C07C51/48C07C55/02C07C55/21
Inventor 李晓姝高大成师文静张霖王领民
Owner CHINA PETROLEUM & CHEM CORP