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Preparation process of rear earth yttrium ion doped tetracalcium phosphate

A tetracalcium phosphate, preparation technology, applied in the direction of phosphorus compounds, inorganic chemistry, non-metallic elements, etc., can solve the problems of secondary sintering, lower TTCP quality, increase process difficulty and production cost, etc., to reduce process difficulty and Effects of production cost, lower temperature, and increased ion diffusion speed

Inactive Publication Date: 2014-07-16
HENAN NORMAL UNIV
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Problems solved by technology

[0002] Tetracalcium phosphate (Ca 4 (PO 4 ) 2 O, TTCP) is the main hydration reaction active ingredient in the preparation of calcium phosphate biocement. The most commonly used and classic preparation method is the solid-phase method, that is, calcium carbonate and calcium hydrogen phosphate are used as raw materials at a high temperature of 1500-1550 ° C. Since TTCP is a thermodynamically unstable phase, free calcium oxide (f-CaO) and hydroxyapatite (HA) are easily produced at room temperature, thereby reducing the quality of TTCP
In order to reduce the content of free calcium oxide and inhibit the formation of HA, secondary sintering and quenching operations are required, which increases the process difficulty and production cost

Method used

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  • Preparation process of rear earth yttrium ion doped tetracalcium phosphate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Calcium hydrogen phosphate and analytically pure calcium carbonate were mixed in a molar ratio of 1:2, ball milled on a ball mill with water as a medium for 6 hours, then dried in a drying oven at 80°C for 2 hours, and then the mixture was moved to a high-temperature furnace at 250 The heating rate of ℃ / h is raised to 1380 ℃, and after holding for 4 hours, the sample is directly taken out of the furnace and quenched to obtain tetracalcium phosphate.

Embodiment 2

[0012] Calcium hydrogen phosphate and analytically pure calcium carbonate were mixed in a molar ratio of 1:2, ball milled on a ball mill with water as a medium for 6 hours, then dried in a drying oven at 80°C for 2 hours, and then the mixture was moved to a high-temperature furnace at 250 The heating rate of ℃ / h is raised to 1380 ℃, and after holding for 4 hours, the tetracalcium phosphate is produced in the furnace and cooled with the furnace.

Embodiment 3

[0014] Calcium hydrogen phosphate and analytically pure calcium carbonate were mixed according to a molar ratio of 1:2, and yttrium nitrate with a total mass of calcium hydrogen phosphate and analytically pure calcium carbonate of 1.2% was added and ball milled on a ball mill for 6 hours with water as a medium, and then placed in a drying oven at Dry at 80°C for 2 hours, then move the mixture to a high-temperature furnace to raise the temperature to 1380°C at a rate of 250°C / h, keep it warm for 4 hours, and then cool down with the furnace in the furnace to prepare rare earth yttrium ion-doped tetracalcium phosphate.

[0015] The XRD analysis results of the product calcined at 1380°C for 4 hours showed that in the TTCP sample doped with 1.2wt% yttrium nitrate, the main crystal phase was TTCP, and the diffraction peaks of calcium oxide (CaO) and HA were hardly observed, while no yttrium nitrate doped The diffraction peaks of calcium oxide (CaO) and HA appeared obviously in the sa...

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Abstract

The invention discloses a preparation process of rear earth yttrium ion doped tetracalcium phosphate. According to the technical scheme, the preparation process is technically characterized by comprising the following steps: mixing calcium hydrophosphate and analytically pure calcium carbonate according to a molar ration being 1:2; adding yttrium nitrate the addition of which is 0.6-2.5% of the total mass of calcium hydrophosphate and analytically pure calcium carbonate, carrying out ball milling for 6h by using a ball mill in the presence of water serving as a medium; drying for 2h at 80 DEG C in a drying oven; heating the mixture to 1350-1500 at a heating rate of 250 DEG C / h in a high-temperature furnace; and heating heat for 1-6h and cooling in the furnace to finally prepare the rear earth yttrium ion doped tetracalcium phosphate. A rear earth metallic compound yttrium nitrate is introduced in the raw material system of preparation of tetracalcium phosphate, which is beneficial to the reduction of synthesis temperature of tetracalcium phosphate, stabilization of tetracalcium phosphate phase, inhibition of conversion from tetracalcium phosphate to free calcium oxide and hydroxyapatite; in addition, one-time firing is realized without quenching operation, the process difficulty is lowered, and the product cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of medical biomaterials, and in particular relates to a preparation process of rare earth yttrium ion-doped tetracalcium phosphate. Background technique [0002] Tetracalcium phosphate (Ca 4 (PO 4 ) 2 O, TTCP) is the main hydration reaction active ingredient in the preparation of calcium phosphate biocement. The most commonly used and classic preparation method is the solid-phase method, that is, calcium carbonate and calcium hydrogen phosphate are used as raw materials at a high temperature of 1500-1550 ° C. Under the reaction, since TTCP is a thermodynamically unstable phase, free calcium oxide (f-CaO) and hydroxyapatite (HA) are easily produced at room temperature, thereby reducing the quality of TTCP. In order to reduce the content of free calcium oxide and inhibit the formation of HA, secondary sintering and quenching operations are required, which increases the difficulty of the process and the prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32
Inventor 杨洪吕艳杰张哲亮王佩宁黔冀
Owner HENAN NORMAL UNIV
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