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Process for synthesizing hydroxylapatite

A technology for synthesizing hydroxyapatite and hydrothermal synthesis, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of harsh reaction conditions, high acquisition cost, and limited quantity, and achieve fast reaction speed, The effect of abundant resources and low reaction temperature

Inactive Publication Date: 2008-11-19
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is found through summary that the mineral phases of biological raw materials (except sea urchin) are all calcium carbonate aragonite, and these reaction conditions are relatively harsh, such as high temperature (100 ° C ~ 260 ° C), high pressure (usually more than ten atmospheres), reaction It takes a long time (usually several hours to several months), and some synthesis will produce many by-products, etc.
On the other hand, coral is a national key protected natural resource, and its quantity is limited; although sea urchins and cuttlefish bones are renewable resources, the cost of obtaining them is high; It is difficult to enter its interior for ion exchange, so it is difficult to completely convert into HA

Method used

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  • Process for synthesizing hydroxylapatite
  • Process for synthesizing hydroxylapatite
  • Process for synthesizing hydroxylapatite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Weigh 1.0g of the dried chalk layer, put it into a 50ml reaction test tube with 1.0g of diammonium hydrogen phosphate, add about 50ml of water to completely dissolve the diammonium hydrogen phosphate, and then plug the mouth of the test tube with medical cotton. Stand in the air at room temperature 30°C, stop the reaction after 120h, take out the sample and wash it thoroughly, dry it at 80°C and grind it into powder for FTIR test, as shown in Figure-2, from the infrared spectrum in Figure-2, it can be seen that the chalk layer (calcium carbonate calcite) and diammonium hydrogen phosphate aqueous solution at room temperature 30 ℃, the characteristic absorption peak of hydroxyapatite does not appear after 120h (υ 1 960.5cm -1 ; 3 1035.4cm -1 , 1091cm -1 ; 4 564.4cm -1 , 603cm -1 ), that is, no hydroxyapatite is produced.

Embodiment 2

[0041] Take by weighing 1.0g (0.01 mole) dry chalk layer, put into the reaction test tube that has the reflux condenser tube of 50ml with 1.0g (0.0076 mole) diammonium hydrogen phosphate, add 50ml water, make diammonium hydrogen phosphate Dissolve completely, and then place it in a constant temperature water bath at 60°C and heat it. After 48 hours of reaction, samples were taken, washed and dried, and the test results of FTIR and XRD were shown in Figure-3 and Figure-4 respectively.

[0042] It can be seen from Figure-3 that the chalk layer reacted with diammonium hydrogen phosphate aqueous solution at 60°C for 48 hours to convert hydroxyapatite, but the CO of calcite calcium carbonate 3 2- Characteristic absorption peak (879.35cm -1 ,712.75cm -1 ) still exists, indicating that there is a surplus of calcite. The same conclusion can also be drawn from the XRD analysis of the product (Figure-4), and it can be seen that there is more calcite remaining (the relative intensity...

Embodiment 3

[0044]Take by weighing two parts of each 1.0g dry chalk layer, put into the reaction test tube that has the reflux condensation tube of 50ml with 1.0g diammonium hydrogen phosphate respectively, add 50ml water, make diammonium hydrogen phosphate dissolve completely, then Placed in a 75°C constant temperature water bath for heating. Take one of the samples in 24 hours, wash, dry, and grind for FTIR test as shown in Figure-5. The reaction of another sample stopped after 48 hours, and the sample was washed and dried for XRD analysis as shown in Figure-6.

[0045] It can be seen from Figure-5 that the characteristic absorption peak of hydroxyapatite (υ 1 960cm -1 ; 3 1035cm -1 , 1090cm -1 ; 4 564cm -1 , 603cm -1 ), indicating the generation of hydroxyapatite. From the XRD pattern in Figure-6, it can be seen that after 48 hours of reaction, the calcite is still partially unreacted (the weaker peaks of calcite and tricalcium phosphate are not marked).

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Abstract

The invention discloses a method for synthesizing hydroxyapatite with chalk (calcium carbonate) as a raw material, which comprises the step of allowing hydrothermal synthesis reaction between chalk and ammonium hydrogen phosphate aqueous solution under normal pressure in a 60-95 DEG C water bath for 24-96 hours to obtain a hydroxyapatite product. The inventive method has the advantages of normal pressure reaction, rapid reaction speed, low reaction temperature, high yield, and rich raw material resources. The obtained product retains the microstructure original chalk, can be used as an active bioceramic layer, a metal-based or glass-based biomaterial layer, or a matrix or an enhancement body of biological composite materials, can absorb toxic positive ions in wastewater, and can be used as a catalyst carrier or a drug sustained-release carrier.

Description

technical field [0001] The invention relates to a preparation technology of phosphate, in particular to a method for hydrothermally synthesizing hydroxyapatite from biological raw materials. Background technique [0002] Hydroxyapatite [Hydroxyapatite, HA] [Ca 10 (PO 4 ) 6 (OH) 2 ], belonging to phosphate-based inorganic non-metallic materials. Its chemical composition and crystal structure are very close to the mineral composition of vertebrate bones and teeth. After implanted in the human body, it forms an organic combination with living tissue through the biochemical reaction on the surface, and has good biocompatibility and affinity. It is an ideal active bioceramic material. Generally, it can be used as the matrix or reinforcement of active bioceramics, metal-based or glass-based biomaterial coatings and biocomposites; because hydroxyapatite has a strong ability to absorb chemical substances, it can absorb toxic cations in wastewater , It can also be used as a cat...

Claims

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Application Information

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IPC IPC(8): C01B25/32
Inventor 汪港张刚生张伟钢
Owner GUANGXI UNIV
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