Preparation method of lysine acetate bulk drug

A technology of lysine acetate and lysine hydrochloride, which is applied in the field of amino acid preparation, can solve the problems of insufficient environmental protection of ammonia gas, high energy consumption of ammonia, and environmental pollution, and facilitate industrial scale-up, reduce water consumption, and shorten concentration time Effect

Active Publication Date: 2018-11-06
WUXI JINGHAI AMINO ACID
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the whole process, elution of lysine consumes a large amount of ammonia water, and the subsequent heating and vacuum concentration to catch ammonia consumes high energy consumption, and the volatilization of a large amount of ammonia gas is not environmentally friendly; the elution and regeneration process of the detachable column requires strong alkali and strong acid solution, and the elution of lysine also requires the use of a large amount of ammonia solution
Strong alkali, strong acid and ammonia solution are not environmentally friendly and can easily cause environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The preparation of embodiment 1 lysine acetate

[0043] (1) After dissolving 10kg of lysine hydrochloride in water, the diluted solubility is 20% (g / 100ml water). The aqueous solution of lysine hydrochloride is electrodialyzed with a special heterogeneous metal film (EPL4016C of Hangzhou Lanran Environmental Technology Co., Ltd. ) Dechlorination, the volume of the clear solution after dechlorination is twice the volume of the concentrated solution, the conductivity of the clear solution after dechlorination is ≤400μs / cm, and the yield is ≥99%;

[0044] (2) Add the concentrated lysine solution into a 100L reaction kettle, add glacial acetic acid with the same number of moles as lysine, adjust the pH value to 7.0, and react at 70-80°C for 2 hours to obtain a lysine acetate solution ;

[0045] (3) adjust the pH of the lysine acetate aqueous solution to be 4.0, and obtain the lysine acetate feed liquid;

[0046] (4) Ammonium acetate is first added in the lysine acetate fe...

Embodiment 2

[0051] The preparation of embodiment 2 lysine acetate

[0052](1) After lysine hydrochloride 10kg is dissolved in water, the solubility after dilution is 20%. The aqueous solution of lysine hydrochloride is dechlorinated by electrodialysis special heterogeneous metal membrane. 2 times, the clear night conductivity after dechlorination is ≤350μs / cm, and the yield is ≥98%;

[0053] (2) Add the lysine solution into a 100L reaction kettle, add glacial acetic acid with 1.1 times the molar number of lysine, and adjust the pH value to 7.0, and react at 70-80°C for 2 hours to obtain a lysine acetate solution;

[0054] (3) Regulate the pH of the lysine acetate aqueous solution to be 3.0 to obtain the lysine acetate feed liquid;

[0055] (4) Ammonium acetate is first added in the lysine acetate feed solution, so that the mass ratio of the inorganic salt to the final concentration is 20%, and then ethanol is added so that the mass ratio of the organic solvent to the final concentration ...

Embodiment 3

[0060] The preparation of embodiment 3 lysine acetate

[0061] (1) After lysine hydrochloride 10kg is dissolved in water, the solubility after dilution is 20%. The lysine hydrochloride aqueous solution is dechlorinated by electrodialysis special heterogeneous metal membrane. The clear volume after dechlorination is 2% of the dope volume times, the clear night conductivity after dechlorination is ≤300μs / cm, and the yield is ≥97%;

[0062] (2) Add the lysine solution into a 100L reaction kettle, add glacial acetic acid with 1.2 times the molar number of lysine, and adjust the pH value to 7.0, and react at 70-80°C for 2 hours to obtain a lysine acetate solution;

[0063] (3) Regulate the pH of the lysine acetate aqueous solution to be 5.0 to obtain the lysine acetate feed liquid;

[0064] (4) Ammonium acetate is first added in the lysine acetate feed solution, so that the mass ratio of the inorganic salt to the final concentration is 20%, and then ethanol is added so that the ma...

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Abstract

The invention discloses a preparation method of a lysine acetate bulk drug, and belongs to the technical field of amino acid preparation. According to the preparation method, a conventional method ofusing an ion exchange column to remove chlorine is not used any more, thus acid, alkali, or ammonia water is not used, and the environmental pollution is reduced. An organic solvent / inorganic salt dual water phase system is established to separate and extract lysine acetate, and compared with a conventional ion exchange extraction method, the wastewater amount and consumed acid and alkali are further reduced. The recovery rate of provided preparation method can reach 99.8%, the product purity can reach 99.7%, and the light transmittance can reach 99.8%.

Description

technical field [0001] The invention relates to a preparation method of a lysine acetate bulk drug, belonging to the technical field of amino acid preparation. Background technique [0002] L-Lysine is one of the essential amino acids for the human body, because it is not only a basic nutrient for human health, but also has anti-inflammatory and analgesic effects, liver cell protection, immunity enhancement, and anti-tumor effects in disease treatment. . Medical compound amino acid injection can not only provide patients with essential nutrients, but also has good effects in treating burns, liver diseases, kidney diseases, encephalopathy, etc. Lysine is one of the main raw materials for compound amino acid injection. Due to the poor chemical stability of lysine, it was often used as lysine hydrochloride in the early stage. The compound amino acid infusion prepared with lysine hydrochloride has high chloride ion content, and some patients are not suitable for it. Therefore...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C227/40C07C229/26C07C51/41C07C51/42C07C53/10
CPCC07C51/412C07C51/42C07C227/18C07C227/40C07C229/26C07C53/10
Inventor 陈晓双蔡立明宁健飞
Owner WUXI JINGHAI AMINO ACID
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