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Purification method of citric acid fermentation broth

A technology of citric acid fermentation liquid and purification method, applied in carboxylate preparation, organic chemistry, etc., can solve the problems of high labor intensity, large waste, low yield of citric acid, etc., and achieve low production cost and pollution reduction Effect

Active Publication Date: 2010-02-17
COFCO BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The disadvantages of the calcium salt method are: great labor intensity, large amount of waste (mainly calcium salt) and waste liquid, 0.9 tons of sulfuric acid and calcium carbonate consumed per ton of citric acid, and lemons remain in the waste liquid and waste Calcium acid, resulting in low yield of citric acid, generally below 92%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The purification method of citric acid fermentation broth, comprises the steps:

[0038] (1) 5m first 3 , the clear liquid after the citric acid fermentation liquid of 11% concentration by weight removes the thalline is added in the calcium hydrogen citrate reaction tank, and the clear liquid is heated to 95 ℃, slowly adding solid content is 30% (weight percent concentration) The calcium carbonate is neutralized. When the pH value is 2.0, stop adding calcium carbonate and let it stand for 20 minutes to generate a reaction solution containing calcium dihydrogen citrate precipitation. Liquid separation to obtain a supernatant, the solid phase (i.e. calcium dihydrogen citrate) is then washed with 85°C hot water, and the liquid produced after washing the solid phase is discharged into the supernatant in the calcium hydrogen citrate reaction tank to obtain a mixed solution ;

[0039] (2) the solid phase (that is, calcium dihydrogen citrate) obtained in the step (1) is put ...

Embodiment 2

[0043]The purification method of citric acid fermentation broth, comprises the steps:

[0044] (1) 8m first 3 , the clear liquid after the citric acid fermentation liquid of 11% concentration by weight is removed the thalline joins in the calcium hydrogen citrate reaction tank, and the clear liquid is maintained at 60 ℃, and slowly adding solid content is 30% (weight percent concentration) The calcium hydroxide is neutralized, when the pH value is 3.5, stop adding calcium hydroxide, and let stand for 20 minutes to generate a reaction solution containing calcium dihydrogen citrate and calcium monohydrogen citrate precipitation, and the reaction solution is layered Then, the solid-liquid separation was carried out by underflow filtration to obtain a supernatant, and the solid phase (ie, calcium dihydrogen citrate and calcium monohydrogen citrate) was washed with hot water at 80°C, and the liquid produced after washing the solid phase was discharged into lemons The mixed solutio...

Embodiment 3

[0049] The purification method of citric acid fermentation broth, comprises the steps:

[0050] (1) 6m first 3 , the clear liquid after the citric acid fermentation liquid of 11% concentration by weight removes the thalline is joined in the calcium hydrogen citrate reaction tank, and the clear liquid is heated to 90 ℃, and slowly adding solid content is 30% (weight percent concentration) The calcium carbonate is neutralized. When the pH value is 4.0, stop adding calcium carbonate and let it stand for 20 minutes to generate a reaction solution containing calcium monohydrogen citrate precipitation. Liquid separation to obtain a supernatant, the solid phase (i.e. calcium hydrogen citrate) is then washed with 70 ° C hot water, and the liquid generated after washing the solid phase is discharged into the supernatant in the calcium hydrogen citrate reaction tank to obtain a mixed solution ;

[0051] (2) the solid phase (that is, calcium monohydrogen citrate) obtained in the step (...

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PUM

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Abstract

The invention relates to a purification method of citric acid fermentation broth, comprising the following steps: adding calcium carbonate or calcium hydroxide into clear liquid to carry out neutralization reaction to generate reaction liquid containing at least one of two precipitates, including calcium dihydrogen citrate and calcium monohydrogen citrate, wherein the bacteria in the clear liquidare removed out of the citric acid fermentation broth, and the pH value at the end point of the reaction reaches 2.0 to 4.0; carrying out solid-liquid separation and washing solid phases; carrying out acidolysis reaction on the solid phases obtained in the previous step, wherein the pH value at the end point of the reaction reaches 1.5 to 2.5; after the reaction, carrying out solid-liquid separation and washing solid phases to obtain calcium salts and citric acid acidolysis liquid with the concentration of 20 percent to 45 percent by weight t; in addition, adding calcium carbonate or calcium hydroxide into liquid phases obtained in the first step to carry out reaction to generate reaction liquid containing at least one of two precipitates, including calcium monohydrogen citrate and calcium citrate, wherein the pH value at the end point of the reaction reaches 5.0 to 7.0; carrying out solid-liquid separation and washing solid phases; and returning the washed solid phases to the step (1) and joining in the reaction again. The method has the advantages of low production cost, high yield and less wastes.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and relates to a method for purifying fermentation broth, in particular to a method for purifying citric acid fermentation broth. Background technique [0002] Citric acid is widely used in food, medicine, cosmetics, detergents, packaging, metal purification, construction, environmental protection and other industries, requiring hundreds of thousands of tons every year. The output and export volume of citric acid in my country has ranked first in the world for many consecutive years. In 2007, the output was 760,000 tons, and the export was 708,300 tons. Most of the products were exported. At present, the EU is the largest export market of my country's citric acid, accounting for about 1 / 3; the United States is the second largest export market, accounting for about 1 / 10. [0003] The separation and purification processes of citric acid at home and abroad mainly include calcium salt m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/265C07C51/02
Inventor 周永生熊结青周勇王浩郭巧芝
Owner COFCO BIOTECHNOLOGY CO LTD
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