Preparation method of high energy phosphoric acid compound

Abstract

The invention discloses a preparation method of a high energy phosphoric acid compound, which comprises the following steps: uniformly mixing phosphoric pentoxide and industrial phosphoric acid, slowly adding organic acid anhydride in a mixing system and stirring for reaction; after reacting, adding carbonate and / or a bicarbonate precipitating agent in a reaction solution, stirring and precipitating deposition, and filtering and then obtaining the high energy phosphoric acid compound with high yield. The method has the advantages of simple operation, high utilization rate of raw materials, low production cost, safety and environmental protection, and can satisfy industrialization production.

Description

technical field

[0001] The invention relates to a preparation method of a high-energy phosphoric acid compound, belonging to the field of chemical synthesis. Background technique

[0002] High-energy phosphate compounds are phosphate compounds that appear during the metabolism of organisms. When hydrolyzed, they can release a large amount of free energy, enabling organisms to complete various physiological activities. High-energy phosphate compounds generally have high-energy phosphate bonds, which can be transferred to other compounds such as ADP under the action of enzymes, thereby realizing the in situ regeneration of the expensive cofactor ATP, which has a wide range of application values.

[0003] Jinan Weierkang Biochemical Pharmaceutical Co., Ltd. disclosed the preparation and content determination of dilithium acetyl phosphate (2003 "Chinese Journal of Biochemical Medicine"). The synthesized high-energy phosphoric acid compound is dilithium acetyl phosphate, which is...

Examples

Embodiment 1

[0026] 1. Take 200mL of 85% phosphoric acid in a glass beaker, add 16.0g of phosphorus pentoxide powder, and stir in a water bath at 55°C for 1 hour;

[0027] 2. Lower the temperature of the mixture in step 1 to 25°C, take propionic anhydride that is 1.1 times the moles of phosphoric acid, and slowly add it dropwise to the phosphoric acid mixture, and the process lasts for 1.5 hours;

[0028] 3. Add 274.0g of magnesium carbonate, stir in an ice bath for 2 hours, and obtain a solid granular precipitate;

[0029] 4. The above granular precipitate was collected by filtration, vacuum filtered and dried to obtain 564.5 g of magnesium propionyl phosphate, the purity was 90.2%, the conversion rate of phosphoric acid was 98.7%, and the conversion rate of propionic anhydride was 90.9%.

Embodiment 2

[0031] 1. Take 120mL of 85% phosphoric acid in a glass beaker, add 7.8g of phosphorus pentoxide powder, and stir in a water bath at 60°C for 1.5 hours;

[0032] 2. Cool the mixture in step 1 to 15°C, take propionic anhydride that is 1.05 times the moles of phosphoric acid, add it dropwise to the phosphoric acid mixture, and stir and mix for 2.5 hours;

[0033] 3. Add 163.3g calcium bicarbonate, stir in ice bath for 2 hours, and get precipitate;

[0034] 4. The precipitate was collected by filtration, vacuum filtered and dried to obtain 347.6 g of calcium propionyl phosphate, with a purity of 94.96%, a conversion rate of phosphoric acid of 98.5%, and a conversion rate of propionic anhydride of 95.2%.

Embodiment 3

[0036] 1. Take 300mL of 85% phosphoric acid in a glass beaker, add 15.6g of phosphorus pentoxide powder, and stir in a water bath at 65°C for 1 hour;

[0037] 2. Cool down the temperature of the mixture in step 1 to 3°C, take 1.1 times the mole number of acetic anhydride, slowly add it dropwise to the phosphoric acid mixture, stir and react, and the process lasts for 1.5 hours;

[0038] 3. Add 440.6g of calcium carbonate, stir in an ice bath for 2.5 hours, and obtain a solid granular precipitate;

[0039] 4. The above granular precipitate was collected by filtration, vacuum filtered and dried to obtain 829.3 g of calcium acetylphosphate with a purity of 93.19%. The conversion rate of phosphoric acid was 98.6%, and the conversion rate of acetic anhydride was 90.6%.

technical field

[0001] The invention relates to a preparation method of a high-energy phosphoric acid compound, belonging to the field of chemical synthesis. Background technique

[0002] High-energy phosphate compounds are phosphate compounds that appear during the metabolism of organisms. When hydrolyzed, they can release a large amount of free energy, enabling organisms to complete various physiological activities. High-energy phosphate compounds generally have high-energy phosphate bonds, which can be transferred to other compounds such as ADP under the action of enzymes, thereby realizing the in situ regeneration of the expensive cofactor ATP, which has a wide range of application values.

[0003] Jinan Weierkang Biochemical Pharmaceutical Co., Ltd. disclosed the preparation and content determination of dilithium acetyl phosphate (2003 "Chinese Journal of Biochemical Medicine"). The synthesized high-energy phosphoric acid compound is dilithium acetyl phosphate, which is...

Examples

Embodiment 1

[0026] 1. Take 200mL of 85% phosphoric acid in a glass beaker, add 16.0g of phosphorus pentoxide powder, and stir in a water bath at 55°C for 1 hour;

[0027] 2. Lower the temperature of the mixture in step 1 to 25°C, take propionic anhydride that is 1.1 times the moles of phosphoric acid, and slowly add it dropwise to the phosphoric acid mixture, and the process lasts for 1.5 hours;

[0028] 3. Add 274.0g of magnesium carbonate, stir in an ice bath for 2 hours, and obtain a solid granular precipitate;

[0029] 4. The above granular precipitate was collected by filtration, vacuum filtered and dried to obtain 564.5 g of magnesium propionyl phosphate, the purity was 90.2%, the conversion rate of phosphoric acid was 98.7%, and the conversion rate of propionic anhydride was 90.9%.

Embodiment 2

[0031] 1. Take 120mL of 85% phosphoric acid in a glass beaker, add 7.8g of phosphorus pentoxide powder, and stir in a water bath at 60°C for 1.5 hours;

[0032] 2. Cool the mixture in step 1 to 15°C, take propionic anhydride that is 1.05 times the moles of phosphoric acid, add it dropwise to the phosphoric acid mixture, and stir and mix for 2.5 hours;

[0033] 3. Add 163.3g calcium bicarbonate, stir in ice bath for 2 hours, and get precipitate;

[0034] 4. The precipitate was collected by filtration, vacuum filtered and dried to obtain 347.6 g of calcium propionyl phosphate, with a purity of 94.96%, a conversion rate of phosphoric acid of 98.5%, and a conversion rate of propionic anhydride of 95.2%.

Embodiment 3

[0036] 1. Take 300mL of 85% phosphoric acid in a glass beaker, add 15.6g of phosphorus pentoxide powder, and stir in a water bath at 65°C for 1 hour;

[0037] 2. Cool down the temperature of the mixture in step 1 to 3°C, take 1.1 times the mole number of acetic anhydride, slowly add it dropwise to the phosphoric acid mixture, stir and react, and the process lasts for 1.5 hours;

[0038] 3. Add 440.6g of calcium carbonate, stir in an ice bath for 2.5 hours, and obtain a solid granular precipitate;

[0039] 4. The above granular precipitate was collected by filtration, vacuum filtered and dried to obtain 829.3 g of calcium acetylphosphate with a purity of 93.19%. The conversion rate of phosphoric acid was 98.6%, and the conversion rate of acetic anhydride was 90.6%.

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