Method for producing anhydrous citric acid crystals

A technology of anhydrous citric acid and production methods, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of poor quality of dry crystals, low content of easy carbides and moisture content, high content of easy carbides and moisture content, etc. , to achieve the effects of reduced moisture content, reduced easy carbides, and regular crystal appearance

Active Publication Date: 2014-01-01
COFCO BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the prior art to obtain anhydrous citric acid wet crystal entrainment mother liquor is more, dry crystal quality is poorer, easy carbide and the defect that moisture content is higher, provide a kind of obtained anhydrous citric acid wet crystal entrainment Production method of anhydrous citric acid crystals with less mother liquor, good dry crystal quality, easy carbide and low moisture content

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  • Method for producing anhydrous citric acid crystals
  • Method for producing anhydrous citric acid crystals

Examples

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Embodiment 1

[0045] This embodiment is used to illustrate the production method of the anhydrous citric acid crystal provided by the present invention.

[0046] (1) Evaporation crystallization of citric acid solution

[0047] will be 10m 3 A citric acid solution with a citric acid content of 60% by weight is injected into an effective volume of 15m 3 Evaporation crystallization is carried out in the crystallization container, and the feed rate is controlled to feed 4m per hour 3 , Evaporate while feeding, control the crystallization temperature to 70°C, and the stirring speed of the circulating pump to 750rpm. The crystallization time is controlled so that the content of anhydrous citric acid crystals in the crystal slurry reaches 55% by weight.

[0048] (2) Repair of crystals in crystal slurry

[0049] Pour the crystal slurry obtained in step (1) into the buffer tank, and raise the temperature of the crystal slurry to 75°C at a rate of 3°C / hour under constant stirring at 22rpm, and ma...

Embodiment 2

[0051] This embodiment is used to illustrate the production method of the anhydrous citric acid crystal provided by the present invention.

[0052] (1) Evaporation crystallization of citric acid solution

[0053] will be 9.2m 3 A citric acid solution with a citric acid content of 65% by weight is injected into an effective volume of 15m 3 The evaporative crystallization is carried out in the crystallization container, and the feed rate is controlled to feed 4.3m per hour 3 , Evaporate while feeding, control the crystallization temperature to 50°C, and the stirring speed of the circulating pump to 800rpm. The crystallization time is controlled so that the content of anhydrous citric acid crystals in the crystal slurry reaches 45% by weight.

[0054] (2) Repair of crystals in crystal slurry

[0055] Pour the crystal slurry obtained in step (1) into the buffer tank, and raise the temperature of the crystal slurry to 65°C at a rate of 8°C / hour under constant stirring at 26rpm,...

Embodiment 3

[0057] This embodiment is used to illustrate the production method of the anhydrous citric acid crystal provided by the present invention.

[0058] (1) Evaporation crystallization of citric acid solution

[0059] will be 11m 3 The injection volume of citric acid solution with citric acid content of 55% by weight is 15m 3 Evaporative crystallization is carried out in the crystallization container, and the feed rate is controlled to feed 4.1m per hour 3 , Evaporate while feeding, control the crystallization temperature to 58°C, and the stirring speed of the circulating pump to 650rpm. The crystallization time is controlled so that the content of anhydrous citric acid crystals in the crystal slurry reaches 50% by weight.

[0060] (2) Repair of crystals in crystal slurry

[0061] Pour the crystal slurry obtained in step (1) into the buffer tank, and raise the temperature of the crystal slurry to 68°C at a rate of 6°C / hour under constant stirring at 24rpm, and maintain it for 1...

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Abstract

The invention discloses a method for producing anhydrous citric acid crystals. The method comprises the following steps: crystallizing a citric acid solution under the circulating stirring condition to obtain a crystal slurry solution; changing the initial temperature of the crystal slurry solution to repair crystals in the crystal slurry solution, and obtaining a solution containing the anhydrous citric acid crystals, wherein the process of changing the initial temperature of the crystal slurry solution comprises the following steps: (1) heating the crystal slurry solution to 2-20 DEG C after crystallization; (2) cooling the crystal slurry solution to 1-10 DEG C after crystallization; or (3) heating the crystal slurry solution to 2-20 DEG C at first after crystallization and then cooling the heated crystal slurry solution to 2-25 DEG C. Through the technical scheme, recesses in crystal surfaces can be effectively removed, and residues in mother liquid in the crystals are reduced, so that the content of water in the crystals is reduced; moreover, anhydrous citric acid molecules on the crystal surfaces are rearranged in a repair process, so that the quality is effectively improved and readily carbonizable substances are reduced.

Description

technical field [0001] The invention relates to a production method of anhydrous citric acid crystals. Background technique [0002] At present, the continuous production method of anhydrous citric acid in the industry includes: firstly, the citric acid fermentation liquid is separated from the solid and liquid to obtain the citric acid clear liquid, and then the citric acid clear liquid is extracted by hydrogen-calcium method or calcium salt method, acidolyzed and decolorized to obtain Purified citric acid solution, then heat and concentrate the purified citric acid solution, continuously inject the above-mentioned concentrated citric acid solution into the crystallizer, make the citric acid concentrated solution reach a supersaturated state through evaporation, and the solution will crystallize naturally, and then add The citric acid solution crystallizes while evaporating. When the solid content (anhydrous citric acid crystals) reaches a certain level of the total weight ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/265C07C51/43
CPCC07C51/43C07C59/265
Inventor 李北罗虎周勇满云许贵珍
Owner COFCO BIOTECHNOLOGY CO LTD
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