Method for preparing nano beta-TCP powder through macromolecular network gelling method and nano beta-TCP powder

A technology of polymer network and gel method, which is applied in the field of biomedical ceramic powder to prevent phase separation and dispersion, overcome long reaction time and fast synthesis speed

Inactive Publication Date: 2017-12-22
SOUTH CHINA INST OF COLLABORATIVE INNOVATION
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has been widely used in the synthesis of multi-component oxides and composite powders of high-temperature superconducting materials, oxide thermoelectric materials, nano-fluorescent materials, solid fuel cell materials, glass-ceramic materials, etc., but this method has not yet been used. Synthesis of β-TCP in Bioactive Ceramic Powder

Method used

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  • Method for preparing nano beta-TCP powder through macromolecular network gelling method and nano beta-TCP powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Weigh 0.02mol of calcium nitrate tetrahydrate and citric acid and dissolve them in 100mL of deionized water, stir well, add 0.013mol of diammonium hydrogen phosphate according to the molar ratio of Ca / P=1.5, and use nitric acid and ammonia water as pH regulator, to control the pH of the mixture to 2-3;

[0039] (2) Add 5g of acrylamide, 1g of N,N'-methylenebisacrylamide, 0.1mL of tetramethylethylenediamine and 0.4g of ammonium persulfate to the mixture in step (1) in sequence, and stir well ;

[0040] (3) Treat the mixed solution in step (2) in a water bath, the temperature of the water bath is 80° C., and the time of the water bath is 30 min, to obtain a transparent hydrogel;

[0041] (4) Pre-freeze the wet gel obtained in step (3) in a -20°C refrigerator, and then freeze-dry until the quality of the gel is stable, then directly heat-treat the dry gel at 850°C for 180 minutes to obtain nano-scale β-TCP powder.

Embodiment 2

[0043] (1) Weigh 0.03mol of calcium nitrate tetrahydrate and citric acid and dissolve them in 100mL of deionized water, stir evenly, add 0.02mol of diammonium hydrogen phosphate according to the molar ratio of Ca / P=1.5, and use nitric acid and ammonia water as pH regulator, to control the pH of the mixture to 2-3;

[0044] (2) Add 16g of acrylamide, 2g of N,N'-methylenebisacrylamide, 0.2mL of tetramethylethylenediamine and 0.5g of ammonium persulfate to the mixture in step (1) in sequence, and stir well ;

[0045] (3) Treat the mixed solution in step (2) in a water bath, the temperature of the water bath is 70° C., and the time of the water bath is 60 minutes to obtain a transparent hydrogel;

[0046] (4) Pre-freeze the wet gel obtained in step (3) in a -20°C refrigerator, and then freeze-dry until the quality of the gel is stable, then directly heat-treat the dry gel at 1000°C for 120 minutes to obtain nano-scale β-TCP powder.

[0047] For the powder X-ray diffraction anal...

Embodiment 3

[0049] (1) Weigh 0.045mol of calcium nitrate tetrahydrate and citric acid and dissolve them in 100mL of deionized water, stir evenly, add 0.03mol of diammonium hydrogen phosphate according to the molar ratio of Ca / P=1.5, and use nitric acid and ammonia water as pH regulator, to control the pH of the mixture to 2-3;

[0050] (2) Add 33g of N-methylolacrylamide, 3g of N,N'-methylenebisacrylamide, 0.3mL of tetramethylethylenediamine and 0.6g of 3% hydrogen peroxide, and stir well;

[0051](3) Treat the mixed solution in step (2) in a water bath, the temperature of the water bath is 85° C., and the time of the water bath is 40 minutes to obtain a transparent hydrogel;

[0052] (4) Microwave-dry the wet gel obtained in step (3) until the quality of the gel is stable, and then directly heat-treat the dry gel at 800° C. for 160 min to obtain nano-sized β-TCP powder.

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Abstract

The invention belongs to the technical field of biological medical ceramic powder, in particular to a method for preparing nano beta-TCP powder through a macromolecular network gelling method and nano beta-TCP powder. The method comprises the following steps: (1) uniformly mixing a calcium source and a complexing agent in water, adding a phosphorus source according to a molar ratio that Ca/P is equal to 1.5, and adjusting the pH of the mixed solution to be 2 to 3; (2) adding monomers, a cross-linking agent, a catalyst and an initiator into the system, uniformly stirring, heating the system, and obtaining hydrogel; (3) drying the hydrogel, and thermally treating to obtain nano beta-TCP powder. The method is simple in process, good in repeatability, and high in synthesis speed; by adopting liquid phase reaction, and a gel reaction process is rapid, so that the separation and diffusion phenomenon is effectively prevented, and the weakness of the chemical precipitation method that the reaction time is long can be overcome; moreover, the method has the advantages of low cost, easy control of the process, easy industrialization, and capablility of obtaining nanoscale powder with high purity and good dispersity.

Description

technical field [0001] The invention belongs to the technical field of biomedical ceramic powder, and in particular relates to a method for preparing nanometer β-TCP powder by a polymer network gel method and the nanometer β-TCP powder. Background technique [0002] β-tricalcium phosphate (β-TCP) is the low-temperature phase of tricalcium phosphate, which is mainly composed of calcium and phosphorus. Biocompatibility, bioactivity, and biodegradability are ideal materials for human hard tissue repair and replacement, and have been paid close attention to in the field of biomedical engineering. [0003] The synthesis methods of β-TCP powder mainly include solid-phase method and liquid-phase method, and the liquid-phase method mainly includes chemical precipitation method, hydrothermal method, sol-gel method, etc. The solid-phase method is carried out under anaerobic conditions. The β-TCP powder prepared by this method is often stoichiometric and complete in crystallization, b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32B01J13/00
CPCB01J13/0065C01B25/325C01P2002/72
Inventor 郑华德马艺娟张明
Owner SOUTH CHINA INST OF COLLABORATIVE INNOVATION
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