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A kind of production method of calcium hydrogen citrate

A technology of calcium hydrogen citrate and production method, applied in the separation/purification of carboxylic acid compounds, preparation of carboxylate, organic chemistry, etc., can solve the problems of poor quality of calcium sulfate, large consumption of sulfuric acid, and high cost, and achieve crystalline particles Large and uniform crystal particles, the effect of prolonging the crystallization time

Active Publication Date: 2015-10-14
RIZHAO JINHE BOYUAN BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is simple, but there are some problems: the crystal structure of calcium citrate is irregular, and a large number of calcium carbonate particles are embedded, which leads to a large consumption of sulfuric acid in the process of acidolysis of citric acid, poor indicators of easy carbon compounds in the product, poor quality of calcium sulfate, and poor quality of citric acid. Disadvantages such as high content of colloidal substances in the purified liquid
This process reduces the consumption of calcium carbonate and sulfuric acid, and the product purity is improved compared with the traditional calcium salt method, but there are still disadvantages such as the oxalic acid is not removed, and the silicate in the limestone powder enters the calcium sulfate after acid hydrolysis.
[0004] In the existing method for producing calcium hydrogen citrate, the purity requirements of calcium carbonate or calcium hydroxide are very high, generally requiring its purity to be greater than 99%, resulting in high cost
When limestone powder is used as raw material, since the calcium carbonate content of limestone powder is 90-99%, the ratio of silicate to calcium hydrogen citrate crystals in the solution reaches 0.5-2.5%, accounting for 0.5-4‰ of the solution, so it is not removed Impurities in limestone powder will have a great impact on product quality, and at the same time, impurities will have a great impact on calcium sulfate, a by-product of citric acid, making calcium sulfate unable to be further processed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025]A kind of production method of calcium hydrogen citrate, its concrete steps are:

[0026] (1) Add calcium citrate slurry to the citric acid fermentation filtrate, stir and react at 60°C for 1.5 hours, wherein the molar ratio of citric acid in the citric acid fermentation filtrate to citrate in the calcium citrate slurry is 1:0.25;

[0027] (2) Add the slurry obtained in step (1) and the limestone powder slurry into the reactor at the same time to ensure that the molar ratio of citric acid molecules to calcium ions in the entire system is 1:0.65, and complete rapid stirring and filtration within 15 minutes; among them, limestone powder The mass content of calcium carbonate in the medium is 91%, and the particle size is less than 100 mesh; the solid mass content in the limestone powder slurry is 50%;

[0028] (3) Add the refluxing calcium hydrogen citrate slurry to the filtered supernatant for primary crystallization; the volume ratio of the filtered supernatant to the ref...

Embodiment 2

[0033] A kind of production method of calcium hydrogen citrate, its concrete steps are:

[0034] (1) Add calcium citrate slurry to the citric acid fermentation filtrate, stir and react at 70°C for 2 hours, wherein the molar ratio of citric acid in the citric acid fermentation filtrate to citrate in the calcium citrate slurry is 1:0.1;

[0035] (2) Add the slurry obtained in step (1) and the limestone powder slurry into the reactor at the same time to ensure that the molar ratio of citric acid molecules to calcium ions in the entire system is 1:0.70, and complete rapid stirring and filtration within 30 minutes; among them, limestone powder The mass content of calcium carbonate in the medium is 92%, and the particle size is less than 100 mesh; the solid mass content in the limestone powder slurry is 52%;

[0036] (3) Add the refluxing calcium hydrogen citrate slurry to the filtered supernatant for primary crystallization; the volume ratio of the filtered supernatant to the reflu...

Embodiment 3

[0041] A kind of production method of calcium hydrogen citrate, its concrete steps are:

[0042] (1) Add calcium citrate slurry to the citric acid fermentation filtrate, stir and react at 80°C for 3 hours, wherein the molar ratio of citric acid in the citric acid fermentation filtrate to citrate in the calcium citrate slurry is 1:0.17;

[0043] (2) Add the slurry obtained in step (1) and the limestone powder slurry into the reactor at the same time to ensure that the molar ratio of citric acid molecules to calcium ions in the entire system is 1:0.75, and complete rapid stirring and filtration within 45 minutes; among them, limestone powder The mass content of calcium carbonate in the medium is 95%, and the particle size is less than 100 mesh; the solid mass content in the limestone powder slurry is 55%;

[0044] (3) Add the refluxing calcium hydrogen citrate slurry to the filtered supernatant for primary crystallization; the volume ratio of the filtered supernatant to the refl...

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Abstract

The invention relates to a method for producing calcium hydrogen citrate. The method mainly comprises the steps of: shortening reaction time from citric acid to the calcium hydrogen citrate; then providing a supersaturated solution of the calcium hydrogen citrate through a multistage neutralization reaction to realize continuous crystallization of the calcium hydrogen citrate; and prolonging the crystallization time of the calcium hydrogen citrate to realize full crystallization of the calcium hydrogen citrate. The method for producing the calcium hydrogen citrate reduces influence from silicate impurities and the like caused by purity defect of limestone powder to the quality of the calcium hydrogen citrate and the quality of a calcium sulfate by-product, removes most oxalic acid and realizes a method for preparing high-quality calcium hydrogen citrate from low-quality limestone powder. By adopting the method disclosed by the invention to prepare the calcium hydrogen citrate, the returning rate of the mother solution is dropped by about 50%, the obtained calcium hydrogen citrate crystal particles are big and uniform, and the purity of the calcium hydrogen citrate is far higher than that of the traditional calcium hydrogen citrate.

Description

technical field [0001] The invention relates to a production method of calcium hydrogen citrate. Background technique [0002] Citric acid is a high-quality biological fermentation product and one of the largest biochemical products in the world. Its application range covers pharmaceutical intermediates, high-end food and beverage, health care products, high-end daily chemical products, detergent industry and cleaning industry, etc. . The preparation method of citric acid generally includes: starchy raw materials are fermented to obtain citric acid fermentation mash, after filtration, the fermentation clear liquid is obtained, and finally purified by chemical (calcium salt method and hydrogen calcium method) or physical purification (chromatographic method and extraction method) ) to obtain the purified citric acid solution, and obtain the citric acid product through refining. At present, traditional calcium salt method or hydrogen calcium method is generally used at home ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/265C07C51/41C07C51/43
Inventor 寇光智裴振洪周昊高晓彤于海彬鲁建
Owner RIZHAO JINHE BOYUAN BIOCHEM
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