Preparation method for creatine nitrate
A technology of nitrate and creatine, which is applied in the field of preparation of creatine nitrate, can solve problems such as unfavorable formation of pure crystals, yield less than 50%, product loss, etc., and achieve low cost, low energy consumption, and environmental friendliness Effect
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Embodiment 1
[0025] In a 1000L jacketed cooling glass-lined reactor equipped with a stirrer, thermometer, and metering tank, add 400 kg of deionized water and 300 kg of creatine monohydrate (2.01 kmol) in sequence, stir to form a suspension, and keep at 20°C Slowly add 190 kg of 60% nitric acid (2.05 kmol), the reaction temperature is 40°C, after the nitric acid is added, a clear reaction solution is gradually formed, at this reaction temperature, the reaction solution is filtered and then moved to a In a 1000L glass-lined reactor with agitator, thermometer, and jacket cooling function, stir slowly and gradually cool the reaction solution to 5°C within one hour. During this process, crystals of creatine nitrate gradually precipitate, and stand at 5°C for a while. hours later. A centrifuge is used for solid-liquid separation, and the obtained mother liquor is used to replace deionized water to participate in the reaction. The obtained wet crystals of creatine nitrate were transferred to ...
Embodiment 2
[0027] 450 kilograms of the mother liquor that will take out is placed in the reactor of embodiment 1. Add 300 kg of creatine monohydrate (2.01 kmol), stir to form a suspension, and slowly add 190 kg of 68% nitric acid (2.05 kmol) at 15°C. Synthesized, crystallized, and dried under the same conditions as the process parameters in Example 1, and obtained 373 kg of creatine nitrate finished product, with a yield of 95.6%. The product was tested to have a purity of 99.8%, creatinine less than 30PPM, and no creatine dinitrate was detected. and trinitrate.
Embodiment 3
[0029] 450 kg of mother liquor taken out is placed in the reaction kettle of Example 1, 300 kg of creatine monohydrate (2.01 kmol) is added, stirred into a suspension, and at 20° C., 185 kg of nitric acid with a concentration of 68% (2.0 kmol ), synthesized under the same conditions of process parameters as in Example 1, the crystallization temperature was 0°C, and dried under the same conditions as in Example 1 to obtain 382.2 kg of creatine nitrate finished product, with a yield of 98.0% and a purity of 98% after testing. Creatinine was less than 30PPM, creatine dinitrate and trinitrate were not detected.
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