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
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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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