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Method for synthesizing high-purity alpha-calcium glycerophosphate

A technology of calcium glycerophosphate and synthesis method, applied in the direction of phosphorus organic compounds and the like, can solve the problems of high cost, complex synthesis process, difficult separation and the like, and achieve the effects of less impurity content, high purity and stable quality

Active Publication Date: 2011-04-06
RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complex synthesis process, difficult separation, and high cost, commercially available calcium glycerophosphate is basically a mixture of α-calcium glycerophosphate and β-calcium glycerophosphate.

Method used

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  • Method for synthesizing high-purity alpha-calcium glycerophosphate
  • Method for synthesizing high-purity alpha-calcium glycerophosphate
  • Method for synthesizing high-purity alpha-calcium glycerophosphate

Examples

Experimental program
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preparation example Construction

[0035] Such as figure 1 Shown, a kind of synthetic method of high-purity α-calcium glycerophosphate comprises the following steps:

[0036] One, the synthesis of glycerol acetone

[0037] The synthetic 1 of glycerol acetone comprises a synthetic reaction 11 and underpressure distillation 12, and concrete steps are:

[0038] (i) One synthesis reaction

[0039] The raw materials are medical grade glycerin, reagent grade acetone and water-carrying agent, and the molar ratio is glycerol: acetone = 1: 2-4; the volume is 15-20 times of the theoretical water output, petroleum ether and 8%-10% of glycerin quality The catalyst is added to a three-port reaction kettle with a thermometer, a water separator and a reflux condenser, the magnetic stirring is turned on, the temperature is raised to reflux, and the water-carrying agent takes out the water generated by the reaction from the reaction system. When the amount of water in the water separator reaches the theoretical water output,...

Embodiment 1

[0061] Add 23.6g of glycerin, 38ml of acetone, 67.5ml of petroleum ether and 1.9g of p-toluenesulfonic acid into a three-port reaction kettle equipped with a thermometer, a water separator and a reflux condenser, turn on magnetic stirring, heat up to reflux, and Aqueous petroleum ether takes out the water generated by the reaction from the reaction system. When the amount of water in the water trap reached 4.5ml, the reaction was stopped. The reaction solution was distilled under reduced pressure, and fractions at 80° C. and 1 kPa were collected.

[0062] Add the glycerin acetal collected in the above steps into a three-port reaction kettle, and then add phosphorus pentoxide whose molar number is 3 / 4 of the glycerin acetal in batches under strong stirring, and ultrasonically and vigorously stir for 1 hour under the condition of an ice-water bath . The ultrasound was stopped, and the esterification reaction was carried out for 5 hours under the condition that the temperature ...

Embodiment 2

[0065] Add 23.6g of glycerin, 56ml of acetone, 81ml of petroleum ether and 2.1g of p-toluenesulfonic acid into a three-port reaction kettle equipped with a thermometer, water separator and reflux condenser, turn on magnetic stirring, heat up to reflux, and bring water The agent takes the water produced by the reaction out of the reaction system. When the amount of water in the water trap reached 4.5ml, the reaction was stopped. The reaction liquid was distilled under reduced pressure, and fractions of fractions at 81.5° C. and 1.33 kPa were collected.

[0066] Add the glycerin acetonide collected in the above steps into a three-hole reaction kettle, and then add phosphorus pentoxide whose molar number is 9 / 10 of the glycerol acetonide in batches under strong stirring, and ultrasonically and vigorously stir for 1.2 hours under the condition of an ice-water bath . The ultrasound was stopped, and the esterification reaction was carried out for 4 hours under the condition that the...

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Abstract

The invention discloses a method for synthesizing high-purity alpha-calcium glycerophosphate, which comprises the following steps of: synthesizing glycerol acetonide; (2) synthesizing alpha-glycerophosphate; (3) synthesizing alpha-calcium glycerophosphate; and (4) filtering, drying and the like. The synthesized alpha-calcium glycerophosphate has stable quality and high purity, the interference of difficultly separated beta-calcium glycerophosphate is effectively avoided, and the content of the alpha-calcium glycerophosphate is over 90 percent.

Description

technical field [0001] The invention belongs to a method for synthesizing calcium glycerophosphate, in particular to a method for synthesizing high-purity alpha-calcium glycerophosphate. Background technique [0002] Calcium glycerophosphate is a calcium product that is beneficial to human body absorption. Because it has the effect of preventing dental caries and strengthening teeth, it is widely used in chewing gum and toothpaste additives. In addition, it is also widely used in medicine, food and other industries. In particular, α-calcium glycerophosphate, which has a high solubility, is in great demand in many special fields. However, due to complex synthesis process, difficult separation, high cost and other reasons, commercially available calcium glycerophosphate is basically a mixture of α-calcium glycerophosphate and β-calcium glycerophosphate. Contents of the invention [0003] The present invention is proposed in order to overcome the shortcomings existing in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
Inventor 王晶朱昱王红郑楠
Owner RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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