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Preparation method of DL-lysine

A technology of lysine and lysine salt, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, etc., can solve the problems of difficult to guarantee product purity, complicated process and high technical difficulty, and achieve production The effect of low cost, simple process and strong operability

Inactive Publication Date: 2010-01-13
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This approach of chemically synthesizing DL-lysine seems simple, but in fact the process is complicated, the technical difficulty is high, and thus the production cost is also high; (2) using L-lysine as raw material, in a lipid DL-lysine is obtained by racemization and refining in the presence of family acids and an aldehyde (see European Patent EP57092; Japanese Patent 81 / 938)
But this method still has the shortcoming that the technological process is complicated, and needs free L-lysine as raw material, because free L-lysine stability is relatively poor, the price is more expensive, so this method directly uses free L-lysine Amino acid is limited as a raw material
At the same time, due to the backwardness of the post-processing method, that is, the purification method, by-products often exist, and the product purity is difficult to guarantee

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] ①Add 100kg of feed grade L-lysine hydrochloride to the reaction kettle, then add 75kg of glacial acetic acid, 25kg of purified water, heat to 100°C with steam, and stir until completely dissolved.

[0029] ②Add 1,500ml of salicylaldehyde to the above reaction kettle, heat it with steam to 100°C and keep it warm for racemization reaction for 4 hours until the racemization is completed.

[0030] ③Reduce the temperature of the solution in "②" in an ice bath. When the temperature drops to 0°C, start filtering to obtain 90kg of DL-lysine hydrochloride as a solid.

[0031] ④The mother liquor obtained by filtering in "③" is recovered, and the steps "①,②" can be repeated to carry out the mother liquor, and the amount of salicylaldehyde can be halved to increase the yield.

[0032] ⑤ Add 270kg of purified water to the solid obtained in "③" to obtain a dilute solution, add 3kg of activated carbon, heat to 65°C, stir for half an hour to decolorize, and filter.

[0033] ⑥ Put the ...

Embodiment 2

[0037] ①Add 100kg of feed grade L-lysine hydrochloride to the reaction kettle, then add 50kg of glacial acetic acid, 50kg of purified water, heat to 100°C with steam, and stir until completely dissolved.

[0038] ② Add 1600ml of salicylaldehyde to the above reaction kettle, heat it with steam to 100°C and keep it warm for racemization reaction for 4 hours until the racemization is completed.

[0039] ③Reduce the temperature of the solution in "②" in an ice bath, and when the temperature drops to 0°C, start filtering to obtain 85kg of DL-lysine hydrochloride as a solid.

[0040] ④The mother liquor obtained by filtering in "③" is recovered, and the steps "①,②" can be repeated to carry out the mother liquor, and the amount of salicylaldehyde can be halved to increase the yield.

[0041] ⑤ Add 255kg of purified water to the solid obtained in "③" to obtain a dilute solution, add 3kg of activated carbon, heat to 65°C, stir for half an hour to decolorize, and filter.

[0042] ⑥ Put ...

Embodiment 3

[0046] ①Add 100kg of feed grade L-lysine hydrochloride to the reactor, then add 25kg of glacial acetic acid, 75kg of purified water, heat to 100°C with steam, and stir until completely dissolved.

[0047] ② Add 1700ml of salicylaldehyde to the above reaction kettle, heat it with steam to 100°C and keep it warm for racemization reaction for 6 hours until the racemization is completed.

[0048] ③Reduce the temperature of the solution in "②" in an ice bath, and when the temperature drops to 0°C, start filtering to obtain 75kg of DL-lysine hydrochloride as a solid.

[0049] ④The mother liquor obtained by filtering in "③" is recovered, and the steps "①,②" can be repeated to carry out the mother liquor, and the amount of salicylaldehyde can be halved to increase the yield.

[0050] ⑤ Add 225kg of purified water to the solid obtained in "③" to obtain a dilute solution, add 3kg of activated carbon, heat to 65°C, stir for half an hour to decolorize, and filter.

[0051] ⑥Put the decol...

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Abstract

The invention provides a preparation method of DL-lysine, which comprises the following steps: using lysine salt as a raw material and adding the lysine salt to an aqueous solution of glacial acetic acid; steam heating and stirring the obtained mixed solution to be completely dissolved; adding salicylaldehyde to the solution to catalyze; carrying out heat preservation and racemization; after completing racemization, dropping temperature and filtering to obtain solid DL-lysine salt; adding purified water to the solid DL-lysine salt to dissolve and stirring an obtained solute to decolor; adopting ion exchange to desalt; and concentrating and crystallizing obtained resolution liquid to obtain solid DL-lysine. The method has simple process, strong maneuverability, small pollution in a production process, realization of mass production, lower production cost and good racemization effect, and the purity of an obtained DL-lysine product can be maintained higher than 98 percent.

Description

technical field [0001] The invention relates to a method for preparing DL-lysine, in particular to a method for preparing DL-lysine by using lysine salt as a raw material and adopting a certain processing technology. Background technique [0002] DL-lysine is currently being actively discussed at home and abroad, and it has both D and L configurations of lysine. Compared with L-lysine, this DL-lysine has its special purpose. At present, it is widely used as a drug intermediate and is an indispensable and effective composition in medicine, pharmacy and nutrition. [0003] The existing preparation methods of DL-lysine include: (1) One-step synthesis of DL-lysine by chemical methods. This approach of chemically synthesizing DL-lysine seems simple, but in fact the process is complicated, the technical difficulty is high, and thus the production cost is also high; (2) using L-lysine as raw material, in a lipid DL-lysine is obtained by racemization and refining in the presence o...

Claims

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Application Information

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IPC IPC(8): C07C229/26C07C227/36
Inventor 陈文婕江立新张瑾魏珺璇赵辉陈昀李立标胡媛郑爱
Owner BENGBU BBCA MEDICINE SCI DEV
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