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Production method of medicinal anhydrous calcium hydrogen phosphate

An anhydrous calcium hydrogen phosphate, production method technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry and other directions, can solve the problems of unreachable, calcium hydrogen phosphate into calcium hydrogen pyrophosphate, and many impurities, etc. The effect of low equipment requirements, low production cost and simple process

Active Publication Date: 2016-10-12
HUZHOU ZHANWANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation of traditional anhydrous calcium hydrogen phosphate, such as the production process of a kind of calcium hydrogen phosphate disclosed by CN201210562254.3, but generally has the following problems: 1. low yield, many impurities, and unsatisfactory purity; 2. easy to produce By-products, especially in the process of high-temperature treatment from calcium hydrogen phosphate dihydrate to sewage calcium hydrogen phosphate, calcium hydrogen phosphate will undergo intermolecular dehydration and become calcium hydrogen pyrophosphate; 3. It does not meet the current version of the Pharmacopoeia And the requirements of the European and American Pharmacopoeia, etc., these problems largely limit the application of anhydrous calcium hydrogen phosphate in the pharmaceutical field

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A production method of medicinal anhydrous calcium hydrogen phosphate, comprising the steps of:

[0029] (1) Prepare a phosphoric acid solution with a concentration of 15%, add it to the reaction kettle, and raise the temperature to 40°C;

[0030] (2) Prepare a calcium carbonate slurry with a concentration of 25%, add it to the reactor at a rate of 1.5L / min, and at the same time raise the temperature of the solution in the reactor to 65°C, and keep stirring at a rate of 200rpm to react calcium carbonate with phosphoric acid solution After adding the calcium carbonate slurry, continue to stir until the pH of the solution is 5.0, stop stirring, drop the temperature to 60° C., and keep it for 1.5 hours to obtain slurry 1;

[0031] (3) Prepare milk of lime with a concentration of 15%, add it to the slurry obtained in step (2) at a rate of 2.5L / min, stir at a rate of 150rpm while adding the milk of lime, and continue stirring for 20 minutes after adding the milk of lime Unt...

Embodiment 2

[0035] A production method of medicinal anhydrous calcium hydrogen phosphate, comprising the steps of:

[0036] (1) Prepare a phosphoric acid solution with a concentration of 20%, add it to the reaction kettle, and raise the temperature to 45°C;

[0037] (2) Prepare a calcium carbonate slurry with a concentration of 20%, add it to the reactor at a rate of 3.5L / min, and at the same time raise the temperature of the solution in the reactor to 70°C, and keep stirring at a rate of 250rpm to react calcium carbonate with phosphoric acid solution After adding the calcium carbonate slurry, continue to stir until the pH of the solution is 5.5, stop stirring, drop the temperature to 55° C., and keep it for 0.5 h to obtain slurry 1;

[0038] (3) Prepare milk of lime with a concentration of 10%, add it to the slurry obtained in step (2) at a rate of 1.0L / min, stir at a rate of 130rpm while adding the milk of lime, and continue stirring for 15 minutes after adding the milk of lime Until t...

Embodiment 3

[0043] A production method of medicinal anhydrous calcium hydrogen phosphate, comprising the steps of:

[0044] (1) Prepare a phosphoric acid solution with a concentration of 30%, add it to the reaction kettle, and raise the temperature to 50°C;

[0045] (2) Prepare a calcium carbonate slurry with a concentration of 21%, add it to the reactor at a rate of 2.0L / min, and at the same time raise the temperature of the solution in the reactor to 68°C, and keep stirring at a rate of 225rpm to react calcium carbonate and phosphoric acid solution After adding the calcium carbonate slurry, continue to stir until the pH of the solution is 5.3, stop stirring, drop the temperature to 50° C., and keep it for 1.0 h to obtain a slurry 1;

[0046] (3) Prepare milk of lime with a concentration of 12%, add it to the slurry 1 obtained in step (2) at a rate of 2.0L / min, stir at a rate of 200rpm while adding the milk of lime, and continue stirring for 16 minutes after adding the milk of lime Unti...

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Abstract

The invention relates to preparation of calcium hydrogen phosphate, in particular to a production method of medicinal anhydrous calcium hydrogen phosphate. The method comprises the following steps: (1) preparing a phosphoric acid solution; (2) preparing calcium carbonate slurry, and enabling the prepared calcium carbonate slurry to react with the phosphoric acid solution to obtain slurry I; (3) preparing 10-15% lime milk, adding the prepared lime milk into the slurry I obtained in the step (2) at the speed of 1.0-2.5L / min, stirring at the speed of 130-200rpm while adding the lime milk, continuously stirring for 5-20min until the pH of the solution is 6.0-7.0 after the lime milk is added, standing and carrying out heat preservation for 1-1.5h to obtain slurry II; (4) carrying out solid-liquid separation on the slurry II obtained in the step (3), recovering solid and drying to obtain the anhydrous calcium hydrogen phosphate. The production method is simple in technology and low in requirements for equipment; the reaction raw materials are treated by special processes, so that the obtained anhydrous calcium hydrogen phosphate is high in yield and purity, can meet the requirements of pharmaceutical grade, and is low in production cost.

Description

technical field [0001] The invention relates to the preparation of calcium hydrogen phosphate, in particular to a production method of pharmaceutical grade anhydrous calcium hydrogen phosphate, which belongs to the field of production of pharmaceutical auxiliary materials. Background technique [0002] Calcium hydrogen phosphate anhydrous is a white, odorless, tasteless powder or crystal, which exists as a triclinic crystal. Pharmaceutical grade anhydrous calcium hydrogen phosphate is mainly used as a diluent for hydrophobic drug tablets and capsules. It is not only a pharmaceutical excipient but also a calcium supplement nutrient. [0003] The preparation of traditional anhydrous calcium hydrogen phosphate, such as the production process of a kind of calcium hydrogen phosphate disclosed by CN201210562254.3, but generally has the following problems: 1. low yield, many impurities, and unsatisfactory purity; 2. easy to produce By-products, especially in the process of high-te...

Claims

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Application Information

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IPC IPC(8): C01B25/32
CPCC01B25/322C01P2006/80
Inventor 潘继成
Owner HUZHOU ZHANWANG PHARMA
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