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Production method of sodium citrate

A technology of sodium citrate and production method, which is applied in the separation/purification of carboxylic acid compounds, preparation of carboxylate, calcium carbonate/strontium/barium, etc. Sodium products are unqualified, calcium sulfate cannot be further processed, etc., to avoid excessive calcium ions, avoid influence, and large crystal particles

Active Publication Date: 2013-04-17
RIZHAO JINHE BOYUAN BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has the following disadvantages: 1. Raw material defects: lead to the unqualified main indicators of sodium citrate products, iron ions, chloride ions and easy carbon compounds
However, in this process, calcium hydrogen citrate is used as an acid salt, which easily leads to a large amount of calcium ions (calcium bicarbonate or calcium hydroxide) in the final sodium citrate solution, resulting in excessive calcium ions in the product.
[0005] In addition, in the existing method for producing calcium hydrogen citrate, the purity requirements of calcium carbonate or calcium hydroxide are very high, 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

[0036] A kind of production method of sodium citrate, its concrete steps are:

[0037] (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;

[0038] (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, complete rapid stirring and filtration within 15 minutes, and use a mass fraction of 25% ionic membrane caustic soda absorbs the carbon dioxide released by the reaction to prepare sodium carbonate solution; wherein, the mass content of calcium carbonate in the limestone powder is 91%, and the particle size is less than 100 mesh; the solid mass content in the limestone powder slurry is 50%;

[0039] (3) Add the refluxing calcium hydrogen c...

Embodiment 2

[0045] A kind of production method of sodium citrate, its concrete steps are:

[0046] (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;

[0047] (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%;

[0048] (3) Add the refluxing calcium hydrogen citrate slurry to the filtered supernatant for primary crystallization; the volume ratio of the filtered supernatant to the refluxing calci...

Embodiment 3

[0054] A kind of production method of sodium citrate, its concrete steps are:

[0055] (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;

[0056] (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, complete rapid stirring and filtration within 45 minutes, and use a mass fraction of The 18% ionic membrane caustic soda solution absorbs the carbon dioxide emitted by the reaction to prepare a sodium carbonate solution; wherein, the mass content of calcium carbonate in the limestone powder is 95%, and the particle size is less than 100 mesh; the solid mass content in the limestone powder slurry is 55%;

[0057] (3) Add the refluxing calciu...

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Abstract

The invention relates to a production method of sodium citrate. The method comprises the main steps that limestone powder and citric acid fermentation liquor are reacted, filtered and crystallized, and then are conducted to at least one time of neutralization and crystallization, so that calcium hydrogen citrate crystal is continuously and directly obtained; and the calcium hydrogen citrate crystal is reacted with the mixed solution of sodium hydroxide and sodium carbonate, so that sodium citrate and calcium carbonate are obtained. The method increases the content of carbonate in a whole system, reduces the hydrolysis rate of the carbonate, avoids the affect to finished products by calcium bicarbonate, and prevents the calcium ion in the finished products from exceeding standard. Part of sodium in the sodium citrate is provided by ionic membrane caustic soda, and compared with the traditional one-step method for producing sodium citrate, the production method has the advantages that the purity of solution is high, contents of calcium ion, iron ion and chloride ion are low, and return rate of sodium citrate mother liquor is greatly reduced.

Description

technical field [0001] The present invention relates to a kind of production method of sodium citrate. Background technique [0002] Sodium citrate is the largest derivative product of citric acid, which is mainly used in the fields of raw materials, high-end food and beverage, health care products, high-end daily chemical products, detergent industry and cleaning industry. Its preparation method generally includes: fermentation and filtration of starchy raw materials to obtain fermentation clear liquid, and then chemical (calcium salt method and hydrogen calcium method) purification or physical purification (chromatographic method and extraction method) to obtain citric acid purification liquid, citric acid purification The solution is neutralized with ion membrane caustic soda to obtain a sodium citrate solution, and then concentrated and crystallized to obtain a sodium citrate product. [0003] At present, domestically, there are techniques for purifying sodium citrate t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/265C07C51/41C07C51/43C01F11/18
Inventor 李昌涛安丰民孔玉刘剑雄任守会周昊
Owner RIZHAO JINHE BOYUAN BIOCHEM
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