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Method for preparing L-asparaginic acid disodium

A technology of disodium aspartate and aspartic acid, applied in the field of preparation of disodium L-aspartate, which can solve problems such as easy blockage of equipment, difficulty in drying, easy softening, etc., and easy control of water content , reduce the safety factor, and stabilize the water content

Active Publication Date: 2016-11-16
宜兴市前成生物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the difficulty in crystallization of disodium L-aspartate and the particularity of easy water absorption, the inventor has tried spray drying and direct drying at room temperature. Because the product in spray drying is easy to become soft and sticky under high temperature conditions, it has extremely fluidity. Poor, easy to block equipment
Direct drying Because the moisture is difficult to dry, the appearance of the product will turn yellow seriously under the condition of high temperature and long time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A method for preparing disodium L-aspartate, comprising the following steps:

[0021] (1) Add water to the reaction kettle, equipped with a motor to stir, heat to a temperature of 75°C, keep stirring, after adding L-aspartic acid, gradually add sodium carbonate, sodium carbonate needs to be added slowly to prevent excessive foaming of the material liquid Splashing; wherein the mass of L-aspartic acid is 20% of the water mass, and the mass ratio of L-aspartic acid to sodium carbonate is 1:1.

[0022] Take a small amount of reaction solution to filter and remove impurities, test the pH, and correct the pH of the reaction solution to 10.5; decolorize and filter the reaction solution, concentrate in vacuum to the solution Baume degree: 43.2°Bé, stir the solution and cool it to room temperature, at this time the material is very viscous Thick, but no crystals separated out.

[0023] (2), transfer the solution to a vacuum freeze dryer, pre-freeze at -25°C for 3 hours, then s...

Embodiment 2

[0026] A method for preparing disodium L-aspartate, comprising the following steps:

[0027] (1) Add water to the reaction kettle, equipped with a motor to stir, heat to a temperature of 75°C, keep stirring, after adding L-aspartic acid, gradually add sodium carbonate, sodium carbonate needs to be added slowly to prevent excessive foaming of the material liquid Splashing; wherein the mass of L-aspartic acid is 20% of the water mass, and the mass ratio of L-aspartic acid to sodium carbonate is 1:1.

[0028] Take a small amount of the reaction solution to filter and remove impurities, test the pH, and correct the pH of the reaction solution to 11.2; decolorize and filter the reaction solution, concentrate in vacuum to the solution Baume degree: 43.6°Bé, stir the solution and cool it to room temperature, at this time the material is very viscous Thick, but no crystals separated out.

[0029] (2), transfer the solution to a vacuum freeze dryer, pre-freeze at -25°C for 3 hours, th...

Embodiment 3

[0032] A method for preparing disodium L-aspartate, comprising the following steps:

[0033] (1) Add water to the reaction kettle, equipped with a motor to stir, heat to a temperature of 75°C, keep stirring, after adding L-aspartic acid, gradually add sodium carbonate, sodium carbonate needs to be added slowly to prevent excessive foaming of the material liquid Splashing; wherein the mass of L-aspartic acid is 20% of the water mass, and the mass ratio of L-aspartic acid to sodium carbonate is 1:1.

[0034] Take a small amount of reaction solution to filter and remove impurities, test the pH, and correct the pH of the reaction solution to 10.4; decolorize and filter the reaction solution, concentrate in vacuum to the solution Baume degree: 42.8°Bé, stir the solution and cool it to room temperature, at this time the material is very viscous Thick, but no crystals separated out.

[0035] (2), transfer the solution to a vacuum freeze dryer, pre-freeze at -25°C for 3 hours, then s...

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PUM

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Abstract

The invention discloses a method for preparing L-asparaginic acid disodium. The method comprises the following steps of performing a reaction at the temperature of 70-80 DEG C by using sodium carbonate or sodium hydroxide, and L-asparaginic acid as raw materials, and by using water as a solvent, after the reaction is finished, adjusting the pH value of reaction liquid to 9.0-12.0, decoloring the reaction liquid, performing filtration, performing concentration until the Baume degree of a solution is 40-45 degree Be, and reducing temperature; transferring the solution after temperature reduction is completed to a vacuum freeze drier, maintaining the pressure of the vacuum freeze drier to be 20-40Pa, performing pre-freezing at the temperature of minus 30 to minus 20 DEG C for 2-4h, and then maintaining the temperature to be at minus 25 to minus 15 DEG C for 3-5h; and drying materials after vacuum freeze-drying at the temperature of 70-80 DEG C for 3-6 hours, so as to obtain L-asparaginic acid disodium products. According to the method disclosed by the invention, an organic solvent is not used, so that the safety coefficient of production environment is increased; and the products are free from solvent residues, so that the quality of the products is improved, and the water content is easy to control.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing disodium L-aspartate. Background technique [0002] Disodium L-aspartate is a pharmaceutical intermediate, which can be used as food additive and biochemical research preparation. There is no report on the production process of this product at present. Due to the difficulty in crystallization of disodium L-aspartate and the particularity of easy water absorption, the inventor has tried spray drying and direct drying at room temperature. Because the product in spray drying is easy to become soft and sticky under high temperature conditions, it has extremely fluidity. Poor, easy to block equipment. Direct drying is difficult to remove moisture, and the appearance of the product will turn yellow seriously under the condition of high temperature and long time. Contents of the invention [0003] The object of the present invention is to provide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/18C07C227/38C07C229/24
CPCC07C227/18C07C227/38C07C229/24
Inventor 席日新
Owner 宜兴市前成生物有限公司
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