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Hydrothermal preparation of ultrafine calcium silicon-phosphate powder and application thereof

A technology of fine silicon calcium phosphate and silicon calcium phosphate is applied in the field of medical materials, which can solve the problems of long process cycle and difficult sintering of powder, and achieves the effect of meeting application requirements, easy availability of raw materials and less agglomeration

Active Publication Date: 2019-03-22
上海积力威尔生物科技合伙企业(有限合伙)
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] Aiming at the problem that the sol-gel method is difficult to sinter the powder and the process cycle is long in the preparation of silicon calcium phosphate powder, the present invention provides a method of synthesizing the precursor by hydrothermal method, and calcining the precursor at a lower temperature to prepare super Method for Fine Silicon Calcium Phosphate Powder Material

Method used

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  • Hydrothermal preparation of ultrafine calcium silicon-phosphate powder and application thereof
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  • Hydrothermal preparation of ultrafine calcium silicon-phosphate powder and application thereof

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preparation example Construction

[0056] The present invention provides a kind of preparation method of superfine silicon calcium phosphate powder in the first aspect, comprises the steps:

[0057] (1) Mix calcium source, phosphorus source, silicon source and dispersant to obtain a mixture; wherein, the molar ratio of Ca in the calcium source, P in the phosphorus source and Si in the silicon source is 5:2:1;

[0058] In this step, the calcium source can be any one or more of easily soluble calcium source, soluble calcium source or slightly soluble calcium source; preferably, the calcium source is calcium nitrate, calcium chloride, calcium phosphate , any one or more of calcium dihydrogen phosphate, calcium hydrogen phosphate, and calcium hydroxide. Described phosphorus source can select the commonly used phosphorus source reagent for use, comparatively suitably has any in phosphoric acid, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, sodium phosphate, calcium phosphate, calcium dihydrogen phosp...

Embodiment 1

[0106] (1) Weigh 2.842gNa respectively 2 SiO 3 9H 2 O powder, 2.3405gCa(H 2 PO 4 ) 2 Powder, 2.9636gCa(OH) 2 powder, respectively poured into three small beakers, and dissolved in 15mL deionized water, Na 2 SiO 3 9H 2 O dissolved into a transparent solution, Ca(H 2 PO 4 ) 2 Slightly soluble, white suspension, Ca(OH) 2 Slightly soluble, white suspension. Observe Na 2 SiO 3 9H 2 After O is completely dissolved, the Ca(H 2 PO 4 ) 2 Slowly pour the suspension into the sodium silicate solution, stir with a magnetic stirrer while pouring, and then add Ca(OH) 2 The suspension was poured, and the resulting mixture was white, and stirred with a magnetic stirrer for 1 to 2 hours.

[0107] (2) Transfer 60mL of the mixed liquid to a 100mL hydrothermal reaction kettle, and the hydrothermal reaction is carried out in a homogeneous reactor, and the reaction conditions are 180°C, 24h, 15 rpm.

[0108] (3) After the reaction, the white precipitated solution in the hydrother...

Embodiment 2

[0112] (1) With embodiment 1.

[0113] (2) With embodiment 1.

[0114] (3) with embodiment 1.

[0115](4) The finished precursor is calcined at a high temperature of 950°C under conventional atmospheric pressure, the heating rate is 5°C / min, and the temperature is kept at 950°C for 6 hours to obtain calcium silicon phosphate (Ca 5 (PO 4 ) 2 SiO 4 ) powder.

[0116] Carry out XRD test to the prepared silicon calcium phosphate powder, the phase is pure phase silicon calcium phosphate, consistent with the standard card (PDFNo.73-1181) (such as Figure 5 ). Scanning electron microscope observes the morphology of the silicon calcium phosphate powder of preparation (such as Figure 6 ), the particle size of the powder is between 200nm and 300nm, and the particle shape of the powder is irregular, which increases compared to the particle size of the powder calcined at 950°C / 3h.

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Abstract

The invention relates to a hydrothermal preparation of ultrafine calcium silicon-phosphate powder and application thereof. The preparation method comprises the following steps that a calcium source, aphosphorus source, a silicon source and a dispersing agent are mixed to obtain a mixture; wherein a molar ratio of Ca in the calcium source, P in the phosphorus source and Si in the silicon source is5:2:1; the mixture is sealed in a hydrothermal device for hydrothermal reaction to obtain a crude precursor; the crude precursor is treated to obtain a precursor product; and the precursor product iscalcined to obtain a calcium silicon-phosphate powder. The invention also relates to a calcium silicon-phosphate powder material prepared by the method and a use of calcium silicon-phosphateceramic material in repair materials that repairs bone tissue or other hard tissues. The method has the advantages of low cost, simple operation cycle and short particle size, and the prepared calcium silicon-phosphate material has potential application value in biomedical materials, especially in the application of defect repair of human hard tissue.

Description

technical field [0001] The invention relates to the technical field of medical materials, in particular to the hydrothermal preparation and application of superfine silicon calcium phosphate powder. Background technique [0002] There are tens of thousands of patients with bone defects every year in the world, and the repair and regeneration of defective bones is still an important problem in the field of biomedicine. Existing methods of bone repair include xenograft, allograft, autograft and implantation of artificial materials. These methods are limited in clinical application and cannot meet the needs. Therefore, the research and development of bone repair and replacement materials is an important topic in the field of biomedical materials, and has great social significance and huge economic benefits. [0003] In the current research and use of bone repair and replacement materials, calcium phosphate bioceramics account for a large proportion, mainly because calcium phos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/447C04B35/22C04B35/626
CPCC04B35/22C04B35/447C04B35/62605C04B2235/3208
Inventor 宁聪琴刘晓丹寇华敏
Owner 上海积力威尔生物科技合伙企业(有限合伙)
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