Creatine phosphate and a method for its preparation

Abstract

This invention proposes a method for preparing creatine phosphate, belonging to the fields of pharmaceutical chemistry and food additives. The method involves dissolving raw materials, dropwise reaction, cooling crystallization, and post-processing to prepare creatine phosphate. The process is short, with mild reaction conditions, requiring no special high-pressure or corrosion-resistant equipment, and eliminating the need for complex purification processes. This significantly reduces energy consumption and labor costs, enabling direct industrial-scale continuous production. Furthermore, this application uses purified water, methanol, and ethanol as reaction solvents, which are low in toxicity and environmentally friendly, eliminating the risk of high-risk solvent residues. The solvents can be recovered and reused through conventional distillation, significantly reducing raw material costs and waste emissions, meeting the requirements of green chemical production. The target product achieves a molar yield of up to 91% and a stable purity of ≥99.8%, directly meeting the high-end application requirements of food and pharmaceutical grades, resulting in strong market competitiveness.

Description

Technical Field

[0001] This invention belongs to the fields of pharmaceutical chemical engineering and food additives, and specifically relates to a creatine phosphate and its preparation method. Background Technology

[0002] Creatine phosphate is an important bioactive compound with high-energy phosphate bonds. In vivo, it can rapidly replenish energy to muscle cells, effectively relieve fatigue, and repair damaged cells, making it a recognized high-efficiency fatigue recovery agent. Based on its excellent physiological activity and safety, creatine phosphate is widely used in various fields such as food and beverage additives, nutritional supplements, pharmaceutical raw materials, pharmaceutical and chemical intermediates, daily chemical raw materials, feed additives, and veterinary drug raw materials, with broad market application prospects.

[0003] Currently, existing processes for preparing creatine phosphate still have many shortcomings: some processes use highly toxic organic solvents, which not only pose a risk of excessive solvent residues in the product but also generate a large amount of hazardous waste, putting significant pressure on environmental protection; some processes involve cumbersome reaction steps and harsh reaction conditions, requiring high-end production equipment and making it difficult to achieve continuous industrial-scale production; and some processes have strict requirements for raw material specifications and poor control of side reactions, resulting in low product yields and insufficient purity, failing to meet the requirements of high-end applications in food and pharmaceutical fields, and severely limiting the large-scale promotion and application of creatine phosphate.

[0004] Therefore, developing a method for preparing creatine phosphate with high product purity, high reaction yield, simple process steps, strong raw material compatibility, environmental friendliness, and suitability for large-scale industrial production has significant economic value and industry significance. Summary of the Invention

[0005] This invention addresses the problems of the prior art by providing a creatine phosphate.

[0006] To achieve the above objectives, the technical solution adopted in this application is as follows: Firstly, a creatine phosphate, wherein the molecular formula of the creatine phosphate is C4H9N3O2·H3PO4, the molecular weight is 229.128, the creatine phosphate is a white crystalline powder, and the product purity is ≥99.8%.

[0007] Preferably, the creatine phosphate has the following structural formula: .

[0008] Secondly, a method for preparing creatine phosphate, the specific steps of which are as follows: Step 1: Adding and dissolving the materials: Add the reaction solvent to the reaction vessel, add creatine monohydrate while stirring, and heat to the preset reaction temperature; Step 2: Dropwise addition reaction: Slowly add phosphoric acid dropwise to the mixture obtained in Step 1. After the addition is complete, maintain the temperature at a constant temperature to carry out the synthesis reaction. Step 3: Cooling and Crystallization: Cool the system from Step 2 to the crystallization temperature and stir at a constant temperature to complete crystallization; Step 4: Post-processing: Filter the system after crystallization in step 3, and dry the filter cake to obtain creatine phosphate product.

[0009] Preferably, in step one, the reaction solvent is selected from any one of purified water, methanol, ethanol, or a mixture of several solvents.

[0010] Preferably, in step one, the mass ratio of the reaction solvent to creatine monohydrate is 3-5:1, preferably 4:1.

[0011] Preferably, the preset reaction temperature is -10~70℃, and more preferably 50~60℃.

[0012] Preferably, in step two, the phosphoric acid is an aqueous solution of phosphoric acid with a mass fraction of 85% to 98%; the molar ratio of creatine monohydrate to phosphoric acid is 1:1.0 to 1.2, preferably 1:1.05.

[0013] Preferably, in step two, the phosphoric acid is added for 2 to 3 hours, and the reaction is kept warm for 1.5 to 3 hours after the addition is completed, preferably for 2 hours.

[0014] Preferably, in step three, the crystallization temperature is -5~10℃, more preferably 0~5℃, and the stirring crystallization time is 1~3 hours, more preferably 2 hours.

[0015] Preferably, in step four, the drying is performed by atmospheric pressure forced air drying or vacuum drying, at a temperature of 40~60℃, until the product moisture content is ≤0.5%.

[0016] Compared with the prior art, the advantages and positive effects of the present invention are as follows: This application discloses a method for preparing creatine phosphate, which involves steps such as dissolving raw materials, dropwise reaction, cooling crystallization, and post-treatment. The process is short, the reaction conditions are mild, and there are no special high-pressure or corrosion-resistant requirements for production equipment. It eliminates the need for complex purification processes, significantly reducing energy consumption and labor costs, and enabling direct industrial-scale continuous production. Furthermore, this application uses purified water, methanol, and ethanol as reaction solvents, which are low in toxicity and environmentally friendly, eliminating the risk of high-risk solvent residues. The solvents can be recovered and reused through conventional distillation, significantly reducing raw material costs and waste emissions, thus meeting the requirements of green chemical production. Furthermore, this application effectively suppresses side reactions by optimizing material ratios, phosphoric acid dropping conditions, reaction temperature, and crystallization process. The target product molar yield can reach up to 91%, and the product purity is stable at ≥99.8%, which can directly meet the high-end application requirements of food and pharmaceutical grades, making the product highly competitive in the market. Finally, the core raw materials of this application are creatine monohydrate and phosphoric acid, both of which are readily available chemical raw materials, convenient to procure, and inexpensive. At the same time, the process has strong adaptability to phosphoric acid concentration, and phosphoric acid with a concentration of 85%~98% can be used directly without the need for raw material pretreatment, further reducing the production threshold and overall cost. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is a flowchart illustrating the preparation process of creatine phosphate according to the present invention. Detailed Implementation To better understand the above-mentioned objectives, features, and advantages of the present invention, the present invention will be further described below in conjunction with the accompanying drawings and embodiments. It should be noted that, unless otherwise specified, the embodiments and features described in these embodiments can be combined with each other.

[0019] Numerous specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways than those described herein, and therefore the invention is not limited to the specific embodiments disclosed in the following specification.

[0020] Example 1, such as Figure 1As shown, the specific preparation steps of a creatine phosphate according to this application are as follows: 600g of purified water is added to a 1000ml reaction flask, stirring is started, 150g of creatine monohydrate is added, the temperature is raised to 50-60℃, and after the system is evenly dispersed, 106g of 98% phosphoric acid is slowly added dropwise, controlling the dropwise addition time to 2.5 hours. After the dropwise addition is completed, the temperature is maintained at 50-60℃ for another 2 hours. After the reaction is completed, the system is cooled to 0-5℃ and stirred at a constant temperature for 2 hours to complete crystallization. The crystallized system is filtered, and the filter cake is placed in a 50℃ forced-air drying oven and dried until the moisture content is ≤0.5%, yielding 202g of white crystalline powder creatine phosphate. The product molar yield is 88% and the purity is 99.9%.

[0021] Example 2 describes the preparation of creatine phosphate as follows: 600g of methanol was added to a 1000ml reaction flask, stirring was started, 150g of creatine monohydrate was added, and the temperature was raised to 50-60℃. After the system was evenly dispersed, 106g of 98% phosphoric acid was slowly added dropwise over a period of 3 hours. After the addition was complete, the temperature was maintained at 50-60℃ for another 2 hours. After the reaction was complete, the system was cooled to 0-5℃ and stirred at a constant temperature for 2 hours to complete crystallization. The crystallized system was filtered, and the filter cake was dried in a 45℃ vacuum drying oven until the moisture content was ≤0.5%, yielding 208g of white crystalline powder creatine phosphate. The product molar yield was 91%, and the purity was 99.8%.

[0022] Example 3 describes the preparation of creatine phosphate as follows: 600g of ethanol was added to a 1000ml reaction flask, stirring was started, 150g of creatine monohydrate was added, and the temperature was raised to 50-60℃. After the system was evenly dispersed, 106g of 98% phosphoric acid was slowly added dropwise over a period of 2 hours. After the addition was complete, the temperature was maintained at 50-60℃ for another 2 hours. After the reaction was complete, the system was cooled to 0-5℃ and stirred at a constant temperature for 2 hours to complete crystallization. The crystallized system was filtered, and the filter cake was dried in a 55℃ forced-air drying oven until the moisture content was ≤0.5%, yielding 204g of white crystalline powder creatine phosphate. The product molar yield was 89%, and the purity was 99.8%.

[0023] Example 4 describes the preparation of creatine phosphate, with the following steps: 600g of a methanol-ethanol mixed solvent (methanol to ethanol mass ratio 1:1) was added to a 1000ml reaction flask. Stirring was started, and 150g of creatine monohydrate was added. The temperature was raised to 55℃. After the system was evenly dispersed, 122g of 85% phosphoric acid was slowly added dropwise over 2.5 hours. After the addition was complete, the temperature was maintained at 55℃ for another 2 hours. After the reaction was complete, the system was cooled to 0-5℃ and stirred at this temperature for 2 hours to complete crystallization. The crystallized system was filtered, and the filter cake was dried in a 50℃ vacuum drying oven until the moisture content was ≤0.5%, yielding 205g of white crystalline powdered creatine phosphate. The product molar yield was 89.5%, and the purity was 99.8%.

[0024] Example 5 describes the preparation of creatine phosphate, with the following steps: 600 kg of purified water was added to a 1000 L reactor, stirring was started, 150 kg of creatine monohydrate was added, and the temperature was raised to 50-60 °C. After the system was evenly dispersed, 106 kg of 98% phosphoric acid was slowly added dropwise over a period of 3 hours. After the addition was complete, the temperature was maintained at 50-60 °C for another 2 hours. After the reaction was completed, the system was cooled to 0-5 °C and stirred at a constant temperature for 2 hours to complete crystallization. The crystallized system was centrifuged and filtered, and the filter cake was dried in a 50 °C double-cone rotary vacuum dryer until the moisture content was ≤0.5%, yielding 205 kg of white crystalline powdered creatine phosphate. The product molar yield was 89.5%, and the purity was 99.8%.

[0025] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any other way. Any person skilled in the art may make changes or modifications to the above-disclosed technical content to create equivalent embodiments that can be applied to other fields. However, any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the protection scope of the present invention.

Claims

1. A creatine phosphate salt, characterized in that, The creatine phosphate has the molecular formula C4H9N3O2·H3PO4 and a molecular weight of 229.

128. It is a white crystalline powder with a purity of ≥99.8%.

2. The creatine phosphate according to claim 1, characterized in that, The structural formula of the creatine phosphate is shown below: 。 3. The method for preparing creatine phosphate according to claim 2, characterized in that, The specific steps are as follows: Step 1: Adding and dissolving the materials: Add the reaction solvent to the reaction vessel, add creatine monohydrate while stirring, and heat to the preset reaction temperature; Step 2: Dropwise addition reaction: Slowly add phosphoric acid dropwise to the mixture obtained in Step 1. After the addition is complete, maintain the temperature at a constant temperature to carry out the synthesis reaction. Step 3: Cooling and Crystallization: Cool the system from Step 2 to the crystallization temperature and stir at a constant temperature to complete crystallization; Step 4: Post-processing: Filter the system after crystallization in step 3, and dry the filter cake to obtain creatine phosphate product.

4. The method for preparing creatine phosphate according to claim 3, characterized in that, In step one, the reaction solvent is selected from any one of purified water, methanol, ethanol, or a mixture of several solvents.

5. The method for preparing creatine phosphate according to claim 4, characterized in that, In step one, the mass ratio of the reaction solvent to creatine monohydrate is 3~5:

1.

6. The method for preparing creatine phosphate according to claim 3, characterized in that, In step one, the preset reaction temperature is -10~70℃.

7. The method for preparing creatine phosphate according to claim 3, characterized in that, In step two, the phosphoric acid is an aqueous solution of phosphoric acid with a mass fraction of 85% to 98%; the molar ratio of creatine monohydrate to phosphoric acid is 1:1.0 to 1.

2.

8. The method for preparing creatine phosphate according to claim 1, characterized in that, In step two, the phosphoric acid is added dropwise over 2 to 3 hours, and the reaction is kept at a constant temperature for 1.5 to 3 hours after the addition is complete.

9. The method for preparing creatine phosphate according to claim 3, characterized in that, In step three, the crystallization temperature is -5~10℃, and the stirring crystallization time is 1~3 hours.

10. A method for preparing creatine phosphate according to claim 3, characterized in that, In step four, the drying is performed by atmospheric pressure forced air drying or vacuum drying at a temperature of 40~60℃ until the product moisture content is ≤0.5%.

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