Neutralization method of citric acid

A technology of citric acid and citrate, applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation and other directions, can solve the problems of residual extractant, large washing water volume, high power consumption, and reduce the consumption of concentrated steam , The effect of reducing the content of citrate and producing less calcium sulfate

Inactive Publication Date: 2010-02-10
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 traditional calcium salt method are: firstly, each ton of citric acid consumes about 0.85 tons of sulfuric acid and 0.85 tons of calcium carbonate, and the consumption of auxiliary materials is high; second, it produces about 2 tons of solid waste calcium sulfate; third, the specific surface area of ​​calcium citrate precipitate Large, adsorbed impurities, resulting in a large amount of washing water, high consumption of hot water, the highest neutralization yield can only reach 94%, and the yield is low; Fourth, the highest acidity after acidolysis of citric acid can only reach about 40%, and the energy consumption of concentration high
[0004] The disadvantages of the chromatography process are: first, the high investment in equipment and auxiliary facilities; second, the pre-treatment of materials is more complicated, consumes a lot of money, and costs a lot
[0005] The disadvantages of electrodialysis are: first, high investment in equipment and auxiliary facilities; second, high power consumption and high production costs
[0006] 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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. The citric acid fermented liquid that is produced with corn as raw material, the concentration that obtains after degerming is 12% (weight / volume percentage, g / 100ml, hereinafter the same). 500 liters of citric acid clear liquid are put into neutralization pot, heat After reaching 50°C, add calcium carbonate and / or calcium hydroxide for a neutralization, and control the pH at the end of the reaction at 3.8 to form citrate-containing precipitates.

[0027] 2. solid-liquid separation obtains 105 kilograms of solid phases containing citrate (containing 47.72 kilograms of citric acid) after washing the solid phase, and the liquid phase is 490 liters of solutions (containing 12.28 kilograms of citric acid) that the concentration of citric acid is 2.51%. In this case, the citrate is calcium citrate and / or calcium hydrogen citrate and / or calcium dihydrogen citrate.

[0028] 3. 490 liters of the liquid phase containing citric acid obtained in step 2 and calcium carbonate and...

Embodiment 2

[0038] 1. 30 kilograms of solid phases (containing citric acid 11.81 kilograms) that embodiment 1 step 4 produces are added to 500 liters of citric acid concentration in the sterilized clear liquid of 12%, heated to 80° C. after mixing.

[0039] 2. Slowly add calcium carbonate, when the pH value is 3.0, maintain the temperature and pH for 30 minutes.

[0040] 3. solid-liquid separation obtains 127 kilograms of solid phases containing citrate (containing 57.45 kilograms of citric acid) after washing the solid phase, and the liquid phase is 510 liters of solutions containing citric acid concentration of 2.82% (containing 14.36 kilograms of citric acid).

[0041] 4. Carry out secondary neutralization with 510 liters of the liquid phase containing citric acid obtained in step 3 with calcium carbonate and calcium hydroxide, and the pH at the end of the reaction is controlled at 7.5 to generate a citrate-containing precipitate.

[0042] 5. above-mentioned reaction solution is carrie...

Embodiment 3

[0053] 1. Heat the sterilized clear solution with a citric acid concentration of 12% to 80°C. Slowly add in 35 kilograms of solid phases (containing 13.87 kilograms of citric acid) that embodiment 2 step 4 produces.

[0054] 2. When the pH value is 2.5, add calcium carbonate and citric acid sterilizing liquid at the same time, maintain the temperature at 80°C and pH 2.5, add a total of 500 liters of citric acid sterilizing liquid, stop feeding and keep warm for 30 minutes.

[0055] 3. solid-liquid separation obtains 123 kilograms of solid phases containing citrate (containing 55.4 kilograms of citric acid) after washing the solid phase, and the liquid phase is 513 liters of 3.6% solution containing citric acid concentration (containing 18.47 kilograms of citric acid).

[0056] 4. 513 liters of the liquid phase containing citric acid obtained in step 3 is neutralized twice with calcium carbonate and calcium hydroxide, and the pH at the end of the reaction is controlled at 8 to ...

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Abstract

The invention provides a neutralization method of citric acid, comprising the following steps: neutralizing once degerming clear solution of the citric acid with calcium carbonate and/or calcium hydroxide to pH 2-5 to generate precipitate containing citrate; carrying out solid-liquid separation and washing solid phase to obtain a solid phase containing the citrate, a liquid phase is solution containing the citric acid; secondarily neutralizing the solution containing the citric acid with the calcium carbonate and/or calcium hydroxide to pH 3-9 to generate the precipitate with the citrate; allowing the solid phase containing the citrate after separation to return for once neutralization, and allowing the liquid phase without the citric acid after separation to be discharged; and adding sulfuric acid into the solid phase containing the citrate obtained by once neutralization for acidolysis reaction to obtain acidolysis solution of the citric acid and calcium sulfate precipitate. The neutralization method of the invention has the advantages of good product quality, a small quantity of consumed water volume, small load on solid-liquid separation equipment 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 fermentation broth by using a calcium salt method, which 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 700,000 tons. The extraction methods of citric acid at home and abroad are mainly calcium salt method, chromatography, membrane separation method and extraction method. [0003] The disadvantages of the traditional calcium salt method are: firstly, each ton of citric acid consumes about 0.85 tons of sulfuric acid and 0.85 tons of calcium carbonate, and the consumption of auxiliary materials is high; second, it produces about 2 tons of solid waste calcium sulfate; third, the specific surfac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/265C07C51/487
CPCC07C51/412C07C51/02
Inventor 李荣杰尚海涛潘声龙
Owner ANHUI BBCA FERMENTATION TECH ENG RES
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