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

Inactive Publication Date: 2015-06-10
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

Furthermore, for the product loss caused by recrystallization, as described in the patent example, 2 moles of anhydrous creatine were added to obtain 186 grams of creatine nitrate, which should theoretically be 388 grams, and the yield was less than 50%.
Due to the small amount of water, the reaction product is in a supersaturated state in the solut

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a preparation method for creatine nitrate. The preparation method comprises the following steps: adding water and creatine monohydrate into a reaction container, and stirring and mixing at a temperature lower than 20 DEG C; then, adding nitric acid into the reaction container and controlling the reaction temperature to be lower than 40 DEG C, filtering reaction liquor after the reaction liquor is clarified, cooling the filtered reaction liquor to be lower than 5 DEG C within 0.5-1.5 hours under stirring, standing for 0.5-1.5 hours, centrifuging to separate out mother liquor and creatine nitrate wet crystals; drying the creatine nitrate wet crystals for 5-7 hours under reduced pressure at a temperature lower than 55 DEG C to obtain the creatine nitrate, and replacing mother liquor with water as raw materials for producing next batch of the creatine nitrate. According to the preparation method disclosed by the invention, the creatine nitrate with purity of 99.8% and creatinine lower than 30PPM and without creatine dinitrate and trinitrate can be obtained without re-crystallization, the yield of the creatine nitrate is higher than 83.8%, the energy consumption is reduced, and the cost is low. The whole preparation process is environmentally friendly.

Description

technical field [0001] The invention relates to a preparation method of creatine nitrate. Background technique [0002] It is an indisputable fact that creatine is an important muscle supplement nutrient for the body to improve and enhance muscle performance and strength. At the same time, creatine also has the effect of treating heart disease, enhancing cognitive function and treating asthma. The market demand for it is increasing. However, creatine is not easily soluble in water. This feature seriously affects oral administration and absorption. For this, people have prepared a variety of inorganic acid salts, organic acid salts and esters of creatine. Studies have found that creatine nitrate With good water solubility, it also has the effects of increasing blood vessel relaxation and improving blood circulation after oral administration. [0003] At present, the preparation method of creatine nitrate has been reported in China, such as the published CN102391157A, ...

Claims

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Application Information

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IPC IPC(8): C07C279/14C07C277/08
Inventor 张建忠
Owner 太仓市新毛涤纶化工有限公司
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