Method of preparing hydroxyapatite by mechanochemical method

A mechanochemical method and hydroxyapatite technology, applied in chemical instruments and methods, inorganic chemistry, phosphorus compounds, etc., can solve problems such as unsuitability for industrial production, impact on purity, long heat treatment time, etc., and achieve easy large-scale industrialization Effects of production, improvement of crystallinity and purity, and reduction of reaction activation energy

Inactive Publication Date: 2016-02-03
HANGZHOU DIANZI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction temperature of this method is relatively high, the heat treatment time is relatively long, and the performance after sintering is relatively poor, so it is not suitable for industrial production
The preparation temperature of the wet method is lower than that of the dry method, but there are also some insurmountable shortcomings
The chemical process of the sol-gel method is relatively complicated, the price of the alkoxide raw material is quite expensive, the toxicity of the organic solvent is high, and it is easy to cause pollution to the environment, etc.
In terms of morphology control of hydroxyapatite powder, nano-hydroxyapatite with various structures (nanometer microspheres, nanofibers, nanocolumns) has been synthesized, but during the synthesis process, templates or surfactants need to be added , these additives can easily pollute the final product and affect the purity of hydroxyapatite
In summary, the current preparation of hydroxyapatite is mostly limited to the use of chemical raw materials and organic templates, and the synthesis temperature is high and the process is complicated. In addition, to obtain hydroxyapatite powder with specific morphology and structure, it is necessary to add Extraneous substances, affecting purity

Method used

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  • Method of preparing hydroxyapatite by mechanochemical method
  • Method of preparing hydroxyapatite by mechanochemical method
  • Method of preparing hydroxyapatite by mechanochemical method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Put 100g of scallop shells and 124.2g of anhydrous disodium hydrogen phosphate into a planetary ball mill according to the molar ratio of Ca / P=1, set the speed of the ball mill to 100r / min, and the ball milling time to 30h. 2) After the reaction is over, mix 200g of the mixture with 6000g of water, and feed high-purity CO 2 Gas, react for 120min; or transfer 200g of the mixture and 6000g of water into the reactor, set the reaction temperature to 50°C, and the reaction time to 30h. After the reaction, filter and dry to obtain hydroxyapatite powder. Scanning electron microscopy of hydroxyapatite figure 1 shown.

Embodiment 2

[0021] 1) Put 100g of oyster shells and 71.9g of anhydrous sodium dihydrogen phosphate into a stirring ball mill according to the molar ratio of Ca / P=1.5, set the speed of the ball mill to 600r / min, and the ball milling time to 6h. 2) After the reaction is over, mix 150g of the mixture with 750g of water, and feed high-purity CO 2 Gas, react for 20 minutes; or transfer 150g of the mixture and 750g of water into the reactor, set the reaction temperature to 150°C, and the reaction time to 5h. After the reaction, filter and dry to obtain hydroxyapatite powder. Scanning electron microscopy of hydroxyapatite figure 2 shown.

Embodiment 3

[0023] 1) Put 100g of mussel shells and 61.1g of diamine hydrogen phosphate into a stirring ball mill according to the molar ratio of Ca / P=2, set the speed of the ball mill to 200r / min, and the ball milling time to 25h. 2) After the reaction is over, mix 150g of the mixture with 1500g of water, and feed high-purity CO 2 Gas, react for 30 minutes; or transfer 150g of the mixture and 1500g of water into the reactor, set the reaction temperature to 60°C, and the reaction time to 26h. After the reaction, filter and dry to obtain hydroxyapatite powder. Scanning electron microscopy of hydroxyapatite image 3 shown.

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Abstract

The invention discloses a method of preparing hydroxyapatite by a mechanochemical method. The method comprises the steps that according to a mole ratio that Ca / P is equal to 1 to 2, adding a calcareous material and microcosmic salt into a ball miller, and ball-milling to obtain a mixture; then mixing the mixture with water, introducing CO2 gas, and reacting for 20 to 120min; or transferring the mixture and the water into a reaction kettle, and reacting for 5 to 30h under the temperature of 50 to 150 DEG C; after the reaction is ended, filtering and drying to obtain hydroxyapatite powder. The calcareous material is pretreated by means of a mechanical activation technology, so that a defected is generated on a structure, reaction activation energy is reduced, reactivity is enhanced, and reaction with the microcosmic salt is promoted; the mixture after the reaction is ended reacts with CO2 or is subjected to heat reaction with water for further edulcoration and crystallization, the crystallinity and the purity of the hydroxyapatite are improved, the technological process is simple, the reaction conditions are mild, and large-scale industrial production is easy.

Description

technical field [0001] The invention belongs to the field of inorganic synthesis, in particular to a method for preparing hydroxyapatite by mechanochemical method. Background technique [0002] Hydroxyapatite (HAP) is a high value-added bio-inorganic material with good biocompatibility and bioactivity. It has been extensively studied and applied in the field of hard tissue repair or replacement. In addition, HAP also has the characteristics of high surface activity, selective adsorption, unique pore structure, and high chemical stability. It has broad application prospects in the fields of sewage treatment, drug carriers, separation and purification, and industrial catalysis, and has great research. Develop and exploit value. [0003] At present, the preparation methods of HAP mainly include chemical precipitation method, sol-gel method, hydrothermal synthesis method, microemulsion method, solid phase reaction method and template method. The dry method usually uses tricalc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32
Inventor 姚志通赵红挺唐俊红谢正苗叶炜宗代银平王雪莹吕挺韩伟黄进刚
Owner HANGZHOU DIANZI UNIV
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