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Preparation method of high-suspension-degree hydroxyapatite

A floating hydroxyapatite and drying technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of unfavorable environmental protection, inconvenient storage and transportation, and high reaction temperature of organic solvents, and achieve low cost and uniformity. Good performance and stable reaction system

Active Publication Date: 2020-08-28
连云港东泰食品配料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, patent document CN101407316 discloses a method for preparing highly dispersed nano-hydroxyapatite, which uses phosphorus-containing compounds and calcium-containing compounds as raw materials to prepare nano-hydroxyapatite by solvothermal method, and uses organic diamines as solvent, the reaction temperature is 180°C, and the reaction time is 24 hours. By changing the reaction parameters to achieve the purpose of controlling the particle size of the product, high-dispersion nano-hydroxyapatite is prepared, but the organic solvent used is not conducive to environmental protection, and the reaction temperature is high. There are safety hazards in the use of pressure vessels; in addition, the reaction time is too long and the efficiency is low
Patent literature CN101185771 also provides a method for preparing highly dispersed nano-hydroxyapatite sol, but the method utilizes sodium citrate and sodium hexametaphosphate as dispersants, and adopts a two-step process to obtain nano-hydroxyapatite sol , a large amount of absolute ethanol is needed in the reaction treatment process, the recovery cost is high, and the final product is a sol, which is not convenient for storage and transportation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Slurry: Weigh 25 kg of calcium hydroxide powder, add 300 liters of deionized water and stir evenly, add 0.5 kg of citric acid, pump the mixed solution to the 500L reaction kettle, and pass it into the steam clamp jacket heating;

[0025] (2) Acid addition: the phosphoric acid solution of 15% concentration is added dropwise in the reactor at a constant speed, and the acid addition time is controlled for 1 hour, and the terminal pH is controlled to be 6.5;

[0026] (3) Reaction: after adding acid, add 0.5 kg of sodium citrate, control the reaction temperature at 70° C., and react for 2 hours;

[0027] (4) Drying: cool down after the reaction time is over, spray-dry the slurry to control the product moisture below 2.5%, and obtain a high-suspension hydroxyapatite product with a particle size of 0.1-2um, which does not settle for 24 hours.

Embodiment 2

[0029] (1) Slurry: Weigh 25 kg of calcium oxide powder, add 200 liters of deionized water and stir evenly, add 1 kg of citric acid, pump the mixed solution to the 500L reaction kettle, and pass it into the steam jacket heating;

[0030] (2) Acid addition: 10% concentration of phosphoric acid solution was added dropwise to the reactor at a constant speed, the acid addition time was controlled for 1 hour, and the pH at the end point was controlled to be 7.0;

[0031] (3) Reaction: After adding acid, add 1 kg of sodium citrate, control the reaction temperature to 60°C, and react for 3 hours;

[0032] (4) Drying: cool down after the reaction time is over, spray-dry the slurry to control the product moisture below 2.5%, and obtain a high-suspension hydroxyapatite product with a particle size of 0.1-2um, which does not settle for 24 hours.

Embodiment 3

[0034] (1) Slurry: Weigh 25 kg of calcium hydroxide powder, add 400 liters of deionized water and stir evenly, add 0.3 kg of citric acid, pump the mixed solution to the 500L reaction kettle, and pass it into the steam clamp jacket heating;

[0035] (2) Acid addition: 12% concentration of phosphoric acid solution was added dropwise to the reactor at a constant speed, the acid addition time was controlled for 1 hour, and the pH at the end point was controlled to be 7.5;

[0036] (3) Reaction: After adding acid, add 0.3 kg of sodium citrate, control the reaction temperature to 80°C, and react for 4 hours;

[0037] (4) Drying: cool down after the reaction time is over, spray-dry the slurry to control the product moisture below 2.5%, and obtain a high-suspension hydroxyapatite product with a particle size of 0.1-2um, which does not settle for 24 hours.

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Abstract

The invention belongs to the field of inorganic chemical synthesis, and discloses a preparation method of high-suspension-degree hydroxyapatite. The method comprises (1) size mixing: preparing calciumhydroxide or calcium oxide into a solution with the mass fraction of 5-15%, adding citric acid, and heating in a reaction kettle; (2) acid adding: preparing phosphoric acid into a solution with the mass fraction of 10%-15%, slowly dropwise adding the solution into the reaction kettle, and controlling the end point pH to be 6.5-7.5; (3) reaction: after dropwise adding the phosphoric acid solution,adding a citrate solution with the mass fraction of 1%-5%, and continuously reacting; and (4) drying: after the reaction is finished, cooling and drying to obtain the high-suspension-degree hydroxyapatite product. According to the method, by constructing a citric acid-citrate buffer system, the prepared hydroxyapatite product is good in homogeneity, narrow in particle size distribution and high in suspension degree (the effect of no sedimentation within 24 hours can be achieved).

Description

technical field [0001] The invention relates to the field of inorganic chemical synthesis, in particular to a preparation method of high-suspension hydroxyapatite. Background technique [0002] Hydroxyapatite, also known as hydroxyapatite, basic calcium phosphate. Hydroxyapatite (HAP) is the main inorganic component of vertebrate bones and teeth. It can chemically bond with body tissues on the interface, and it has a certain solubility in the body, and can release ions that are harmless to the body. It can participate in metabolism in the body, stimulate or induce bone hyperplasia, and promote the repair of defective tissue, showing biological activity. Therefore, hydroxyapatite has been widely used in bone substitute materials, plastic and cosmetic surgery, dentistry, chromatographic purification, calcium supplements and other fields. In addition, hydroxyapatite also has the characteristics of organic compatibility, strong protein adsorption capacity, and temperature-sens...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32
CPCC01B25/32C01B25/322C01B25/327C01P2004/61C01P2004/62
Inventor 卞其华杨威周洺阳舒峰纪玉英
Owner 连云港东泰食品配料有限公司