A kind of preparation method of agmatine hydrochloride

A technology of agmatine hydrochloride and agmatine sulfate, which is applied in the field of preparation of agmatine hydrochloride or waste liquid treatment, and can solve problems such as large safety hazards, many side reactions, and cumbersome operations , to achieve the effect of reducing carbon emissions and increasing social benefits

Active Publication Date: 2018-11-09
JING JING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, agmatine is mainly obtained by chemical synthesis in the market. The main raw materials are 1,4-butylene diamine, o-methylisourea sulfate, sulfuric acid, alcohol, etc. The reaction process consumes a lot of energy and the yield is low. , many impurities, great safety hazards, and certain pollution to the environment; at the same time, there are also 1,4-dibromobutane and potassium phthalimide potassium as raw materials, which undergo three-step reactions of substitution, aminolysis, and guanidinylation According to reports on the production of agmatine sulfate, this route has mild reaction conditions, more side reactions, cumbersome operation, unpleasant smell, and more solvents used in the reaction process, which does not meet the clean and efficient production requirements
[0004] Usually, in the later stage of the preparation of agmatine sulfate, there is often a large amount of mother liquor to be treated. There is a large amount of ethanol in the mother liquor that can be recycled and reused, and the content of agmatine is relatively high. Direct discharge causes industrial "three wastes" and does not meet low-carbon requirements. The concept of environmental protection and recycling

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take agmatine sulfate crystallization mother liquor with a content of 10g / L for a total of 5L, concentrate under reduced pressure at a vacuum degree of -0.09mpa, and a temperature of 70±5°C to remove the solvent in the mother liquor, collect and distill under reduced pressure to concentrate 3.5L of solvent, and the remaining Feed liquid passes through anion resin 717 with a flow rate of 25-30ml / min. When 1.5L of the lower column liquid is collected, there is turbidity in spotting with barium chloride at the outlet. Concentrate to 150ml under vacuum conditions, adjust the pH to 3.8 with 20% hydrochloric acid solution, add 2.25g of activated carbon, stir at room temperature for 40min, filter, remove carbon, and pass the filtrate through a fiber resin water-based membrane again with a pore size of 0.45μm. Add ethanol with a concentration of 95% to the 25°C crystallization liquid while stirring. When the feed liquid becomes cloudy, stop adding ethanol dropwise. After growing...

Embodiment 2

[0027] Take agmatine sulfate crystallization mother liquor 15g / L content to be 4L altogether, in vacuum degree be-0.09MPa, temperature is 70 DEG C and concentrates under reduced pressure to remove the solvent in the mother liquor, collects and distills under reduced pressure and concentrates out solvent 3L, and the remaining material liquid is passed through Anion resin 717, the flow rate is 25-30ml / min, when 1.2L of the lower column liquid is collected, there is turbidity in spotting with barium chloride at the outlet, stop the collection, and continue to vacuum the collected lower column liquid at a temperature of 70±5°C Concentrate to 170ml, adjust the pH to 4.2 with hydrochloric acid solution, add 2.55g of activated carbon, stir at room temperature for 40min, filter, remove carbon, and pass the filtrate through a fiber resin water-based membrane again with a pore size of 0.45μm. Add ethanol with a concentration of 95% to the crystallization liquid at 20°C while stirring. Wh...

Embodiment 3

[0030] Take agmatine sulfate crystallization mother liquor with 10g / L content of 4L in total, concentrate under reduced pressure at a vacuum degree of -0.009MPa and a temperature of 68°C to remove the solvent in the mother liquor, collect and distill and concentrate under reduced pressure 2.8L of solvent, and remove the remaining material The liquid passes through anion resin 717 with a flow rate of 25-30ml / min. When 1.5L of the lower column liquid is collected, the barium chloride spotting sample at the outlet is turbid. Stop the collection and continue to concentrate the collected lower column liquid in vacuum at a temperature of 68°C. to 120ml, adjust the pH to 3.8 with hydrochloric acid solution, add 1.8g of activated carbon, stir at room temperature for 40min, filter, remove carbon, and pass the filtrate through a fiber resin water-based membrane to pass 0.45μm again. Add ethanol to the crystallization liquid at 30°C while stirring. When the feed liquid becomes cloudy, sto...

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Abstract

The invention discloses an agmatine hydrochloride preparation method. The method includes steps: concentrating crystallization mother liquor generated in production of agmatine sulfate to remove a solvent and obtain concentrated liquid; allowing the concentrated liquid to overflow regenerated 717 anion resin to adsorb sulfate ions, collecting lower column liquid until sulfate ions flow out through an outlet, and stopping overflowing; concentrating the collected lower column liquid to obtain crystallization liquid; adopting hydrochloric acid for adjusting pH of the crystallization liquid to 3-6; adding activated carbon, stirring to remove impurities, and filtering to remove carbon; crystallizing to obtain an agmatine hydrochloride product. The agmatine hydrochloride preparation method has advantages that the mother liquid obtained after production of agmatine can be completely used, waste of agmatine is avoided while the agmatine hydrochloride product is obtained, the content of effective components of the hydrochloride product is higher than that of effective components of a sulfate product equal to the hydrochloride product in mass, and accordingly carbon emission is reduced, social benefits are increased, and the production requirement on environmental friendliness is met.

Description

technical field [0001] The invention relates to the technical field of preparation of agmatine hydrochloride or waste liquid treatment. Background technique [0002] Agmatine (agmatine) is a substance with multiple biological functions. It belongs to a class of drugs containing guanidine. Benefits, being able to improve body endurance is of certain benefit and satisfaction to athletes and bodybuilding enthusiasts. At the same time, it can speed up body recovery, increase muscle mass, reduce fat and fat, and improve physical performance. A healthy lifestyle helps, and agmatine also increases nitric oxide levels in two ways, stimulating the release of nitric oxide and inhibiting the synthesis of nitric oxide enzyme. [0003] At present, agmatine is mainly obtained through chemical synthesis in the market. The main raw materials are 1,4-butylene diamine, o-methylisourea sulfate, sulfuric acid, alcohol, etc. The reaction process consumes a lot of energy and the yield is low. ,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C277/08C07C279/12
CPCC07C277/08C07C279/12
Inventor 李斌水米造吉张学义何连顺
Owner JING JING PHARMA
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