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Chromatographic separation method for citric acid

A chromatographic separation and citric acid technology, which is applied to the extraction and separation of citric acid in fermentation broth by chromatography, and the extraction of citric acid, can solve the problems of high power consumption, low automation level, unstable quality of intermediate products, etc. The effect of reduced consumption of auxiliary materials, high level of automation, and stable product quality

Inactive Publication Date: 2009-12-23
ANHUI BBCA FERMENTATION TECH ENG RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The disadvantages of the calcium salt process are: first, the neutralization process is intermittently operated, the operating conditions are poor, the labor intensity of the workers is high, and the automation level is low; the second is that the quality of the intermediate product is unstable, which is not conducive to process control; the third is that the equipment investment is large and the operating cost High; Fourth, high consumption of auxiliary materials, about 0.85 tons of sulfuric acid and 0.85 tons of calcium carbonate per ton of citric acid; Fifth, about 2 tons of solid waste calcium sulfate per ton of citric acid
[0004] The disadvantages of electrodialysis are: first, high investment in equipment and auxiliary facilities; second, high power consumption and high production costs
[0005] The disadvantages of the extraction method are: first, the product quality is poor; second, the product cannot be used in the food and pharmaceutical industries due to the residue of the extractant
[0006] At present, the treatment of citric acid is also carried out by chromatography, but all of them use substances that can adsorb citric acid as the stationary phase. This method will consume a large amount of auxiliary materials such as sulfuric acid in the process of separating citric acid, which consumes a lot and costs a lot. high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The chromatographic separation method of citric acid comprises the steps:

[0031] 1. First put 2m 3 The fermented mash with a citric acid concentration of 15% was filtered with a plate and frame, and then filtered with an ultrafiltration membrane with a molecular weight cut-off of 2000 Daltons to obtain a 2.4m clear liquid with a citric acid concentration of 12%. 3 .

[0032] 2. Decolorize the citric acid clear liquid with activated carbon, and then use 001×7 cation exchange resin and D315 anion exchange resin to remove anions and cations.

[0033] 3. The citric acid decolorization and desalination clear liquid is pumped into the chromatographic system composed of 6 chromatographic columns filled with FLC-10 cation exchange resin, and water is used as the eluent to obtain 7.1m 3 A citric acid extract with a citric acid concentration of 4%.

[0034] 4. Concentrate the citric acid extract with a reverse osmosis membrane until the concentration of citric acid is 12%, t...

Embodiment 2

[0038] The chromatographic separation method of citric acid comprises the steps:

[0039] 1. First put 2m 3 The fermented mash with a citric acid concentration of 15.5% was filtered with a plate and frame to obtain a 2.39m clear liquid with a citric acid concentration of 12.6%. 3 .

[0040] 2. Decolorize the citric acid clear liquid with activated carbon, and then use 732 cation exchange resin and D318 anion exchange resin to remove anions and cations.

[0041] 3. The citric acid decolorization and desalination clear liquid is pumped into the chromatographic system composed of 4 chromatographic columns filled with PCR642 cation exchange resin, and water is used as the eluent to separate impurities to obtain an extract with a citric acid concentration of 4.8% 6.15m 3 .

[0042] 4. Concentrate and crystallize the citric acid extract by heat.

[0043] 5. Separation of citric acid crystals and mother liquor, obtaining 197 kilograms of citric acid wet crystals containing 2.4% w...

Embodiment 3

[0046] The chromatographic separation method of citric acid comprises the steps:

[0047] 1. First put 2m 3 The fermented mash with a citric acid concentration of 14.5% was filtered by plate and frame to obtain a 2.45m clear liquid with a citric acid concentration of 11.5%. 3 .

[0048] 2. Decolorize the citric acid clear liquid with activated carbon, and then use 732 cation exchange resin and D296 anion exchange resin to remove anions and cations.

[0049] 3. Citric acid decolorization, desalination clear liquid is pumped into a chromatographic system composed of 12 chromatographic columns filled with CR1320 cation exchange resin, and dilute sulfuric acid with a concentration of 1000ppm is used as an eluent to separate impurities and obtain citric acid extraction with a concentration of 5%. Liquid 5.53m 3 .

[0050] 4. After the citric acid extract is desalted, it is concentrated and crystallized by heat.

[0051] 5. separate citric acid crystals and mother liquor, obtai...

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Abstract

The invention provides a chromatographic separation method for citric acid, which comprises the following steps: removing bacteria and impurities from citric acid fermented liquor to obtain clear citric acid liquor; decolorizing and desalting the clear liquor; then feeding the clear liquor to an ion exclusion chromatographic system; treating the clear liquor by water or dilute acid as an eluting agent to obtain citric acid solution; and removing impurities, concentrating and crystallizing the citric acid solution to obtain citric acid crystals. The method has the advantages of stable product quality, high product yield, little accessory consumption, no calcium sulphate discharge, and the like.

Description

technical field [0001] The invention relates to a method for extracting citric acid, in particular to a method for extracting and separating citric acid in fermented liquid by chromatography, and belongs to the field of food chemical industry. Background technique [0002] Citric acid is an organic acid widely used in beverage, food and pharmaceutical industries. my country is a major producer of citric acid, with more than 20 production plants, and the output has exceeded 550,000 tons. The extraction methods of citric acid at home and abroad are mainly calcium salt method, adsorption method, membrane separation method and extraction method. [0003] The disadvantages of the calcium salt process are: first, the neutralization process is intermittently operated, the operating conditions are poor, the labor intensity of the workers is high, and the automation level is low; the second is that the quality of the intermediate product is unstable, which is not conducive to process...

Claims

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Application Information

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IPC IPC(8): C07C59/265C07C51/47
Inventor 李荣杰尚海涛潘声龙
Owner ANHUI BBCA FERMENTATION TECH ENG RES
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