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Method for preparing monopotassium L-aspartate dihydrate by separation process

A technology of aspartic acid and chelated potassium, applied in the field of chemistry, can solve the problem of large fixed cost plant and equipment investment, large difference in product moisture, and difficulty in producing stable and uniform potassium L-aspartate hemihydrate. things, etc.

Active Publication Date: 2012-04-11
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

In the prior art, L-aspartic acid chelated potassium dihydrate cannot be obtained when direct spray drying method is used to prepare L-aspartic acid chelated potassium
[0009] The product produced by this method is a powdery solid, and it is impossible to obtain a product with a very good particle size; moreover, it is difficult to control the moisture of each batch of products, and the moisture of each part of the product in the drying chamber varies greatly, so it is difficult to produce stable, uniform, Qualified potassium L-aspartate hemihydrate; at the same time, the humidity and temperature of the production environment are required to be controlled very low to prevent deliquescence of the material
This method has relatively large fixed cost plant and equipment investment, relatively low yield, and very high energy consumption.
Most importantly, this method cannot produce L-aspartic acid chelated potassium dihydrate

Method used

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  • Method for preparing monopotassium L-aspartate dihydrate by separation process
  • Method for preparing monopotassium L-aspartate dihydrate by separation process
  • Method for preparing monopotassium L-aspartate dihydrate by separation process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 500ml of deionized water into a 1000ml beaker, heat and stir on a magnetic stirrer, when the temperature rises to 70℃~75℃, add 100g of L-aspartic acid, K 2 CO 3 52g. After the reaction solution was clarified, samples were taken to measure the pH, and the pH of the corrected end point was 6.0-8.0. Add activated carbon 0.01Kg / L, decolorize, press filter, concentrate to 200ml, cool down to 16°C, add 2g of L-aspartic acid chelated potassium dihydrate as seed crystal, stir and cool to crystallize, add 50ml of absolute ethanol to soak for 2 Suction filter after hours. The solid material obtained by suction filtration was put into a single-necked flask, and then poured out after 4 hours of vacuum drying at room temperature and reduced pressure on a rotary evaporator to obtain 125g of finished product, with a yield of 79.61%. The test was qualified. The test results are shown in Table 1.

Embodiment 2

[0029] Add 500ml of deionized water into a 1000ml beaker, heat and stir on a magnetic stirrer, when the temperature rises to 75°C, add 100g of L-aspartic acid, K 2 CO 3 52g. After the reaction solution is clarified, take a sample to measure the pH, and correct the end point to pH=6.0-8.0. Add activated carbon 0.01Kg / L, decolorize, filter with suction, concentrate to 200ml, cool down to 16°C, add 3g of seed crystal L-potassium glutamate, stir and cool to crystallize, add 50ml of absolute ethanol to soak for 2 hours, and then filter with suction. The solid material obtained by suction filtration was packed into a single-necked flask, and then poured out after 4 hours of vacuum drying at room temperature and reduced pressure on a rotary evaporator to obtain 132g of finished product, with a yield of 83.54%. The test was qualified, and the test results are shown in Table 1.

Embodiment 3

[0031] Add 500ml of deionized water into a 1000ml beaker, heat and stir on a magnetic stirrer, when the temperature rises to 75°C, add 100g of L-aspartic acid, K 2 CO 3 52g. After the reaction solution is clarified, take a sample to measure the pH, and correct the end point to pH=6.0-8.0. Add activated carbon 0.01Kg / L, after decolorization, suction filtration, concentration to 200ml, after cooling down to 16°C, add 4g of seed crystal L-potassium glutamate, stir and cool to crystallize, add 50ml of absolute ethanol to soak for 2 hours and then suction filtration. The solid material obtained by suction filtration was put into a single-necked flask, and then poured out after 4 hours of vacuum drying at room temperature and reduced pressure on a rotary evaporator to obtain 132g of finished product, with a yield of 83.01%. The test was qualified. The test results are shown in Table 1.

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Abstract

The invention discloses a method for preparing a monopotassium L-aspartate dihydrate by a separation process. The method taking L-aspartic acid and potassium carbonate or potassium hydroxide as raw materials comprises the following steps of: adding the raw materials to a reaction vessel; allowing the blended materials to react in the presence of a solvent-deionized water, and then correcting the pH value; decolorizing, filter-pressing, concentrating and cooling the obtained reaction solution; adding a monopotassium L-aspartate dihydrate crystal as a seed crystal to the reaction solution; inducing the monopotassium L-aspartate in the reaction solution to be crystallized so as to form the monopotassium L-aspartate dihydrate crystal with a stable water content; and adding an organic solvent for soaking the monopotassium L-aspartate dihydrate crystal, then directly filtering out a mother liquid, and finally drying to obtain the monopotassium L-aspartate dihydrate. The monopotassium L-aspartate dihydrate obtained by the method has the advantages of large and uniform crystallization granularity and stable water content (based on each batch of the products), thus meeting the requirements for the dihydrate.

Description

technical field [0001] The invention belongs to the field of chemistry, and relates to a method for separating and preparing L-aspartic acid chelated potassium dihydrate, in particular to a method for separating and preparing L-aspartic acid chelated potassium dihydrate by inducing crystallization combined with solvent extraction Methods. Background technique [0002] Monopotassium L-Aspartate Dihydrate, alias: L-aspartic acid potassium salt, molecular formula: C 4 h 6 KNO 4 2H 2 O, molecular weight: 207.19, molecular structure formula: [0003] [0004] It has a wide range of applications in the fields of food additives and pharmaceutical raw materials. [0005] L-Aspartic Acid Chelated Potassium has significant curative effects in regulating myocardial function and electrophysiology, and treating cardiovascular and cerebrovascular diseases, hypokalemia and other arrhythmias, hepatitis, and liver insufficiency. It is a pharmaceutical intermediate, which can be used...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/24C07C227/18C07C227/42
Inventor 席日新李海涛杨龙震
Owner 宜兴市前成生物有限公司
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