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Potassium aspartate preparation method

A technology of potassium aspartate and aspartic acid is applied in the preparation of organic compounds, preparation of cyanide reaction, chemical instruments and methods, etc. question

Active Publication Date: 2013-06-05
山西国润制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has improved the yield, but because the concentration of water in the system takes a long time and consumes a lot of energy, and the vacuum drying effect is also time-consuming and energy-consuming, the overall cost is high
Therefore, it cannot meet the needs of industrial production.
In the existing preparation technology of potassium aspartate, or in the preparation process, water is used to dissolve the raw material and then an organic solvent is added to make it crystallized, and then vacuum drying is carried out. This process consumes a large amount of organic solvent, has low yield and high cost ; Or the reaction solution is initially concentrated, and the concentrated solution is subjected to solvent crystallization treatment. This concentration method takes a long time and consumes a lot of energy; These disadvantages have become a difficult problem to be solved in the production of this product

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Dissolve 133.1g of aspartic acid in 80g of purified water and stir at 30°C until completely dissolved. Add 80g of potassium hydroxide to react. At this time, the pH of the system is 8.0. Add 8.55g of activated carbon to the reaction solution at a temperature of 40°C to decolorize for 30 minutes at 30°C. Filter while it is hot, and filter through a carbon filter, a 1μm filter membrane (the material is PTFE), 0.45μm filter membrane (material is PTFE) three-stage filtration to obtain filtrate.

[0036] The filtrate was transferred to a crystallization tank (triangular flask, 1000ml in size), and an aqueous solution of 95% ethanol as an organic solvent three times the amount of water was slowly added, the solution gradually became cloudy, and the temperature was controlled at -10 to -8°C until the addition was complete. Keep the temperature at -25°C for 2 hours, then filter. The white product was obtained by filtration, washed with a small amount of ethanol solution (30ml)...

Embodiment 2

[0037] Dissolve 133.1g of aspartic acid in 93g of purified water and stir at 30°C until completely dissolved. Add 100g of potassium hydroxide to react, the pH of the system is 7.5, add 8.55g of activated carbon to the reaction solution at 40°C for decolorization at 30°C for 30 minutes, filter while hot, and pass through three stages of filtration of activated carbon, 1μm filter membrane, and 0.45μm filter membrane respectively. A filtrate was obtained.

[0038] Slowly add an aqueous solution of organic solvent 95% ethanol three times the amount of water to the filtrate, the solution becomes cloudy gradually, and the temperature is controlled at -9°C until the addition is complete. Keep the temperature at -20°C for 2.5 hours, then filter. The white product was obtained by filtration, washed with 30 ml of ethanol as a solvent, and then dried under reduced pressure at 30° C. for 8.5 hours. The weight loss on drying was 6.8%, and the finished product yield of potassium aspartate...

Embodiment 3

[0040] Dissolve 133.1 g of aspartic acid in 106 g of purified water and stir at 30°C until completely dissolved. Add 93g of potassium hydroxide to react, the pH of the system is 7.0, and the reaction solution is filtered while hot at a temperature of 40°C, and is filtered through three stages of activated carbon, 1 μm filter membrane and 0.45 μm filter membrane respectively to obtain the filtrate.

[0041] Slowly add an aqueous solution of organic solvent 95% ethanol three times the amount of water to the filtrate, the solution becomes cloudy gradually, and the temperature is controlled at -9°C until the addition is complete. Keep the temperature at -20°C for 2.5 hours, then centrifuge and filter. The white product was obtained by filtration, and the filter cake was washed with 30 ml of ethanol, and then dried under reduced pressure at 30° C. for 9 hours. The weight loss on drying was 7.0%, and the finished product yield of potassium aspartate was 96.1%, and the content was 9...

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Abstract

The invention provides a potassium aspartate preparation method. The method comprises the following steps: 1, reacting aspartic acid with potassium hydroxide according to a mass ratio of 1:0.6-0.75; 2, carrying out three-stage filtration of a product obtained after the reaction in step 1 through one-time filtration by active carbon and two-time filtration by a filter membrane, and taking the obtained filtrate; 3, adding an organic solvent to the filtrate at -10-0DEG C, and cooling at -30 - -20DEGC; and 4, filtering, taking the obtained filter cake, and drying. The method allows the optimum water application amount to be obtained through the difference of the solubility of aspartic acid in water at different temperatures in order to reduce the solvent application amount and improve the yield. A filter system is increased to reduce impurities. A drying method is changed to select a best boiling drying method in order to reach the purposes comprising working hour saving, energy consumption reduction and effective water control. The method has the advantages of short production operation steps, low cost, short time consumption, high yield, and high content, and is very suitable for the industrialized production.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a preparation method of a salt of aspartic acid. Background technique [0002] Potassium aspartate, the chemical name is L-potassium aspartate, and the molecular formula is C 4 h 6 KNO 4 , the molecular weight is 171, and the structural formula is [0003] [0004] Potassium aspartate is the potassium salt of aspartic acid and is an electrolyte supplement. Potassium magnesium aspartate is a mixed double salt composed of potassium aspartate and magnesium salt, which can improve myocardial contractility, reduce oxygen consumption, and improve energy metabolism of myocardial cells. Aspartic acid has a strong affinity with cells, and can be used as a carrier for potassium ions to enter cells, allowing potassium ions to return to cells, promoting cell depolarization and cell metabolism, maintaining myocardial contractility, thereby improving myocardial contractility...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/24C07C227/18C07C227/40
CPCY02P20/10
Inventor 杨立志杨育平
Owner 山西国润制药有限公司
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