Preparation method of sodium citrate crystal through solvent-out crystallization

A technology of sodium citrate and dissolving crystallization, which is applied in the fields of carboxylate preparation, organic chemistry, chemical instruments and methods, etc., can solve the problem of affecting the quality of sodium citrate products, darkening the color of sodium citrate mother liquor, and increasing the viscosity and other problems, to achieve the effect of being suitable for industrial application, easy to recycle and reuse, and reducing energy loss

Active Publication Date: 2015-01-07
NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing industrial preparation of sodium citrate generally adopts the crystallization method of evaporating and concentrating mother liquor, that is, heating and concentrating the mother liquor of sodium citrate to precipitate crystals. This method needs to evaporate a large amount of water, and has the problems of high energy consumption and low efficiency. The mother liquor contains high iron and other metal ions, a small amount of easily carbonized substances such as protein colloids and organic impurities, and these impurities are likely to remain in the product with heat and water loss, making the color of the sodium citrate mother liquor darker, Viscosity becomes bigger, and then affects the quality of gained sodium citrate product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 9mol (0.36kg) of sodium hydroxide into the reactor, then add 1.5L of water, stir to dissolve the sodium hydroxide; slowly add 3mol (0.576kg) of anhydrous citric acid at 20°C, and stir until the reaction is stable at pH 8.7 constant. Add 4.5L of ethanol dropwise at 20°C, filter after the dropwise addition, and let it dry naturally. Get 1.14kg of sodium citrate pentahydrate. Yield 98.96%, content 99.74%.

Embodiment 2

[0022] Add 11.5mol (0.46kg) of sodium hydroxide and 20mol (2.12kg) of sodium carbonate into the reactor, then add 5L of water, stir to dissolve. Slowly add 10mol (1.92kg) of anhydrous citric acid at 25°C, and stir the reaction until the pH is 8.5 and remains stable. Add 20L of methanol dropwise at 55°C, filter after the dropwise addition, and dry naturally. Obtain 3.23kg of sodium citrate dihydrate. Yield 97.93%, content 99.66%.

Embodiment 3

[0024] Add 35mol (3.71kg) of sodium carbonate into the reactor, then add 10L of water, stir to dissolve. Slowly add 10mol (1.92kg) of anhydrous citric acid at 25°C, and stir the reaction until the pH is 9.0 and remains stable. 35L of isopropanol was added dropwise at 55°C, filtered after the dropwise addition, and dried at 150°C. Obtain 2.87kg of anhydrous sodium citrate. Yield 97.48%, content 99.65%.

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PUM

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Abstract

The invention relates to a preparation method of sodium citrate crystal through solvent-out crystallization. The preparation method comprises the following steps: (A) carrying out salt-forming reactions: preparing critic acid and a salt forming agent according to a certain mole ratio, dissolving the salt forming agent into water at first, then slowly adding critic acid into the water, controlling the reaction temperature at a range of 20 to 30 DEG C, wherein the pH value of the solution is in a range of 7.5 to 9.0 when the reactions finish, and filtering the solution after the reactions so as to obtain a mixed solution, wherein the mixed solution concentration calculated by waterless sodium citrate is 285 g/L to 570 g/L; (B) carrying out solvent-out crystallization: adding a solvent-out agent into the mixed solution obtained in the step (A) according to a certain volume ratio to crystallize the sodium citrate crystals, and controlling the crystallization temperature at 20 to 75 DEG C; (C) filtering and drying so as to obtain the sodium citrate product; wherein the sodium citrate product comprises waterless sodium citrate, dihydrate sodium citrate, and pentahydrate sodium citrate. The provided preparation method is simple and convenient, the yield is high, the crystal is large, the purity is high, and the sodium citrate quality is largely improved.

Description

technical field [0001] The invention relates to an industrial preparation method of sodium citrate, in particular to a method for preparing sodium citrate by a dissolution and crystallization method. Background technique [0002] Sodium citrate is a white or colorless organic compound crystal, which is widely used in food, beverage, chemical and pharmaceutical fields. It can be used as flavoring agent, buffer, emulsifier and stabilizer in food, and can also As a blood anticoagulant in medicine, an acidity buffer for body fluids and urine, etc., the current production of sodium citrate is to use calcium citrate salt neutralization method and ion exchange to prepare sodium citrate, and then the obtained sodium citrate After purification, the finished product of sodium citrate is obtained. [0003] The existing industrial preparation of sodium citrate generally adopts the crystallization method of evaporating and concentrating mother liquor, that is, heating and concentrating ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/265C07C51/43
CPCC07B2200/13C07C51/412C07C51/43C07C59/265
Inventor 左丽华严正人黄娟刘慧勤张春青
Owner NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
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