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Preparation method of guanidine derivative creatine hydrochloride

A technology for creatine hydrochloride and derivatives, which is applied in the field of preparation of guanidino derivative creatine hydrochloride, can solve the problems of harsh process requirements, difficult post-processing, impact on the environment, etc., and achieves simple and easy operation, The effect is stable and reliable, and the operation is simple and easy.

Active Publication Date: 2012-03-28
沈军
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcomings, defects and disadvantages of this method are: a large amount of waste acid is produced in the production process, which affects the environment, and brings difficulties to the post-treatment of waste acid, increases the cost, and the process requirements are harsh. Once the temperature is too high , the by-product creatinine or creatinine hydrochloride will be high and exceed the standard, which will bring greater difficulties to the post-processing of the product, and more importantly, affect the quality of creatinine hydrochloride products

Method used

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  • Preparation method of guanidine derivative creatine hydrochloride
  • Preparation method of guanidine derivative creatine hydrochloride

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Effect test

specific Embodiment approach 1

[0024] The present invention will be described in detail below in conjunction with the accompanying drawings. As shown in the accompanying drawings:

[0025] A preparation method of creatine hydrochloride, a guanidinium derivative, using creatine monohydrate as raw material, using sulfur oxychloride for acid hydrolysis, and the creatine monohydrate and sulfur oxychloride are carried out at a temperature of 25-35°C Acid hydrolysis into salt, the filtered solution filtered by acid hydrolysis into salt is concentrated by vacuum distillation and concentrated, and then crystallized on standing, and the standing crystals are washed in the state of solvent suction filtration, and the washed standing The crystals are dried until the water content is less than 1% to obtain the guanidine derivative creatine hydrochloride product.

[0026] In the preparation method of the guanidine derivative creatine hydrochloride, the weight ratio of creatine monohydrate to thionyl chloride is 1:1.25-...

specific Embodiment approach 2

[0034] Carry out by specific implementation mode one, just:

[0035]1. Salt formation: Add 500Kg of 97-99% thionyl chloride to a 1000-liter reactor, turn on the stirring and micro-vacuum state, and slowly add 400Kg of creatine monohydrate, creatine The material will slowly dissolve. After the material is added, stir until it becomes clear. The pH value of the liquid should be 0.5-1. If it is too low, add a small amount of thionyl chloride until the pH value is between 0.5-1 and then at 25 At -30°C, keep warm for 5-6 hours.

[0036] 2. Filtration and concentration: the above-mentioned heat preservation liquid is press-filtered into another clean 1000-liter reactor to remove trace impurities and insoluble matter;

[0037] ①. Heat hot water at 50-60°C in the jacket of the reaction kettle, and keep the temperature in the kettle below 40°C for high-vacuum vacuum distillation to remove thionyl chloride. After a small amount of crystals appear in the reaction kettle, stop the concen...

specific Embodiment approach 3

[0043] On the basis of the specific implementation of the specific implementation modes 1 and 2, the specific implementation of multiple and repeated reductions and expansions of various multiples is carried out in proportion, so that the present invention has a principle test, a small-scale test, and a medium-scale test. The solid foundation of , expanded test and productive test has achieved the expected good effect, has practical operability, and has a wide range of popularization and application value.

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Abstract

The invention discloses a preparation method of guanidine derivative creatine hydrochloride, belonging to the technical field of additives. The method adopts a key technology of 'enabling materials to be recyclable and reusable without three wastes by strictly controlling moderate reaction temperature and corresponding conditions'; creatine monohydrate is taken as a material and thionyl chloride is adopted for acidolysis; the creatine monohydrate and the thionyl chloride are subjected to acidolysis salification; filtrate solution after filtering the acidolysis-salified acidolysis solution is subjected to vacuum reduced-pressure distillation and concentration and then standing crystallization is conducted; the standing crystallized substance is washed under the state of solvent extraction filtration; and the washed standing crystallized substance is dried until the water content lowers to below 1%, therefore the guanidine derivative creatine hydrochloride product is obtained. The preparation method is used for the additives in foods and various beverages. The preparation method is scientific and reasonable, simple and feasible to operate, stable and reliable in effect, high in product purity, good in quality and low in cost, and causes no pollution without the three wastes.

Description

technical field [0001] The preparation method of the guanidino derivative creatine hydrochloride of the present invention relates to the technical field of additives; in particular, it relates to the technical field of food additives; in particular, it relates to the technical field of the preparation method of the guanidine derivative creatine hydrochloride. Background technique [0002] Creatine hydrochloride is white crystal or crystalline powder at room temperature, easily soluble in water, but hardly soluble in organic solvents. Its molecular formula is: C4H9N3O2.HCL, and its molecular weight is 167.6. It is highly hydrophilic and can be used in food additives, medicine and health care products, and can promote muscle growth and enhance physical fitness. Because of this, in recent years, creatine hydrochloride has entered the stage of in-depth research, development and utilization. At present, the research, development and utilization of creatine hydrochloride generall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/14C07C277/08
Inventor 沈军
Owner 沈军
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