Preparation of creatine monohydrate

A technology of creatine and sodium sarcosinate, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of low yield, unavoidable generation of dicyandiamide and creatinine, etc., and achieve high yield , reduce the generation probability, inhibit the effect of decomposition and aggregation

Active Publication Date: 2009-05-20
太仓市新毛涤纶化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This shows that the yield of the preparation method disclosed in this invention is low, and the generation of dicyandiamide and creatinine cannot be avoided equally.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Get 1300 kilograms (3.92kmol) of an aqueous solution containing 33.5% (w / w) sodium sarcosinate and place it in a reactor, cool to 20°C, and while stirring, slowly add 30% hydrochloric acid to adjust the pH of the aqueous solution of sodium sarcosinate value is 9.5, and then inject 500 kg (3.57 kmol) of cyanamide aqueous solution cooled to 15° C. within 90 minutes. The reaction temperature is controlled at 85°C. During the process of adding the cyanamide aqueous solution, adjust the pH value of the reaction solution between 9 and 10 with 15% (w / w) hydrochloric acid for 5 times. After the cyanamide aqueous solution is added, at this temperature Stir for 60 minutes, then lower the temperature of the feed liquid to below 30°C. After the creatine monohydrate is precipitated, a suspension is formed, and the sodium hydroxide aqueous solution is added dropwise under stirring to make the pH value 13, and the temperature is raised to 55°C, and the temperature is lowered to 15°C a...

Embodiment 2

[0020] Get 1300 kilograms (3.92kmol) of the aqueous solution that contains 33.5% (w / w) sodium sarcosinate and place in the reactor, be cooled to 20 ℃, during stirring, slowly add hydrochloric acid, adjust the pH value of sodium sarcosinate solution to be 9.5, and then inject 500 kg (3.57 kmol) of cyanamide aqueous solution cooled to 15°C within 90 minutes. The reaction temperature is controlled at 75°C. During the process of adding the cyanamide aqueous solution, adjust the pH value of the reaction solution between 9 and 10 with 10% (w / w) hydrochloric acid for 5 times. After the cyanamide aqueous solution is added, at this temperature Stir for 60 minutes, then lower the temperature of the feed liquid to below 30°C. After the precipitation of creatine monohydrate crystals is completed, a suspension is formed, and an aqueous solution of sodium hydroxide is added dropwise under stirring to make the pH value 14, and the temperature is raised to 55°C, and after stirring for 30 minu...

Embodiment 3

[0022] Obtain the suspension containing creatine monohydrate according to the same method as in Example 1, filter to obtain creatine monohydrate, place it in a washing tank, add 500 liters of deionized water, and adjust the suspension with sodium hydroxide under stirring The pH was 13, the temperature was raised to 55°C, the temperature was lowered to 15°C after stirring for 30 minutes, and the mixture was filtered. Gained creatine monohydrate after filtering is placed in washing tank again and washes 2 times with the same example 1 condition, and dry by the drying method shown in embodiment 1, obtains 418.6 kilograms of creatine monohydrate (with cyanamide feeding dosage Yield 78.6%). Detected by HPLC: the purity is 99.94%, creatinine and dicyandiamide are not detected.

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PUM

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Abstract

The invention relates to a preparation method of kreatine monohydrate, wherein, calcium cyanamide and sodium sarcosine react in the water. The specific technological process of the preparation method is as follows: chlorhydric acid is firstly adopted for adjusting the pH value of an aqueous solution of the sodium sarcosine to 9 to 10, and the solution is heated to 60 DEG C to 90 DEG C, and then a calcium cyanamide aqueous solution with temperature below 20 DEG C is slowly added; during the addition of the calcium cyanamide aqueous solution, the chlorhydric acid is continuously used for adjusting the pH value of a reaction solution to between 9 and 10; and after the addition of the calcium cyanamide aqueous solution, kreatine monohydrate is generated in the reaction at the temperature of 60 DEG C to 90 DEG C. In the preparation method, the pH value during the whole reaction is strictly controlled so as to effectively inhibit the decomposition and polymerization of calcium cyanamide, reduce the generation probability of dicyandiamide and improve the purity of the kreatine monohydrate. The kreatine monohydrate obtained by the preparation method has the purity of more than 99.9 percent; in addition, the preparation method has high yield.

Description

technical field [0001] The invention relates to a method for preparing creatine monohydrate. Background technique [0002] Creatine is an energy reserve substance present in muscle tissue, which can be used as a food additive and for the preparation of medicines. It is mainly obtained by removing crystal water from creatine monohydrate. [0003] In the prior art, there are many methods for preparing creatine monohydrate, such as the method for preparing creatine monohydrate by using an aqueous solution of sodium sarcosinate and methylisothiouronium sulfate as described in U.S. Patent No. 6,326,513B1 and Chinese Invention patent CN 1240207A records the use of chloroacetic acid, methylamine and cyanamide to prepare creatine monohydrate. The former has an impact on the environment due to the production of equimolar methyl mercaptan in the process, and the creatine monohydrate produced has to be washed repeatedly with ethanol, and the product must be purified by recrystallizati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/14C07C277/02
Inventor 张建忠陈延全
Owner 太仓市新毛涤纶化工有限公司
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