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Preparation method for nano hydroxylapatite doped with metal ions

A nano-hydroxyapatite and metal ion technology is applied in the fields of biomedicine and nano-material preparation, which can solve the problems of complicated operation, long preparation period, complicated sol-gel process, etc., and achieves easy control of dosage and uniform doping. Effect

Inactive Publication Date: 2010-01-13
SHAANXI UNIV OF SCI & TECH
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Problems solved by technology

[0003] At present, the methods for preparing this kind of material are mainly sol-gel method, hydrothermal synthesis method and co-precipitation method, etc. Among them, the hydrothermal synthesis method requires a high temperature and high pressure reaction environment, and the co-precipitation method does not require a high pressure environment but must strictly control the reaction conditions. The operation is more complicated, the preparation cycle is long, and the sol-gel method also has the disadvantages of complicated process and long preparation cycle.

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  • Preparation method for nano hydroxylapatite doped with metal ions

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Embodiment 1

[0014] Embodiment 1, at first, prepare respectively the Ca(NO 3 ) 2 and (NH 4 ) 2 HPO 4 solution, and by Ca(NO 3 ) 2 and (NH 4 ) 2 HPO 4 The volume ratio is 1.67 mixed with HNO 3 Adjust the pH of the mixed solution to 3 , where AgNO 3 Mass: The volume of solution A is 1×10 -4 (g): 1 (ml), then use HNO 3 Adjust the pH of the mixed solution 2 ) 2 Obtain solution C, wherein, CO(NH 2 ) 2 Quality: The volume of solution B is 0.06 (g): 1 (ml); Finally, under magnetic stirring, solution C was heated and refluxed at 100°C for 4 hours. After the reaction, it was naturally cooled to room temperature, then vacuum filtered and water After washing, it was dried at 100° C. for 24 hours to finally obtain Ag ion-doped nano-hydroxyapatite crystals. see figure 1 , the results show that the obtained sample is a pure nano-hydroxyapatite crystal, and the grain size calculated by the Sherri formula based on the (002) crystal plane is 28.7nm. There is no crystal line of silver and it...

Embodiment 2

[0015] Embodiment 2, at first, prepare respectively the Ca(NO 3 ) 2 and (NH 4 ) 2 HPO 4 solution, and by Ca(NO 3 ) 2 and (NH 4 ) 2 HPO 4 The volume ratio is 1.67 mixed with HNO 3 Adjust the pH of the mixed solution 3 ) 3 , where La(NO 3 ) 3 Mass: The volume of solution A is 3×10 -4 (g): 1 (ml), then use HNO 3 Adjust the pH of the mixed solution 2 ) 2 Obtain solution C, wherein, CO(NH 2 ) 2 Quality: the volume of solution B is 0.03 (g): 1 (ml); finally, under magnetic stirring, solution C was heated to reflux at 100°C for 3 hours, after the reaction was completed, it was naturally cooled to room temperature, then vacuum filtered and washed with water After washing, it was dried at 100° C. for 24 hours, and finally La ion-doped nano-hydroxyapatite crystals were obtained.

Embodiment 3

[0016] Embodiment 3, at first, prepare respectively the Ca(NO of 0.2mol / L 3 ) 2 and (NH 4 ) 2 HPO 4 solution, and by Ca(NO 3 ) 2 and (NH 4 ) 2 HPO 4 The volume ratio is 1.67 mixed with HNO 3 Adjust the pH of the mixed solution 3 ) 2 , where Cu(NO 3 ) 2 Mass: The volume of solution A is 5×10 -4 (g): 1 (ml), then use HNO 3 Adjust the pH of the mixed solution 2 ) 2 Obtain solution C, wherein, CO(NH 2 ) 2 Quality: The volume of solution B is 0.05 (g): 1 (ml); Finally, under magnetic stirring, solution C was heated and refluxed at 100°C for 5 hours. After the reaction, it was naturally cooled to room temperature, then vacuum filtered and water After washing, it was dried at 100° C. for 24 hours to finally obtain Cu ion-doped nano-hydroxyapatite crystals.

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Abstract

The invention relates to a preparation method of nano hydroxylapatite doped with metal ions, which comprises the following steps of: firstly, respectively preparing Ca(NO3)2 and (NH4)2HPO4 solution, mixing the Ca(NO3)2 and (NH4)2HPO4 solution, and obtaining clear and transparent solution A; adding metal nitrate into solution A and obtaining clear and transparent solution B; adding CO(NH2)2 into solution B, and obtaining solution C; finally heating and backflowing the solution C for 3 to 5 hours with the temperature of 100 DEG C under the magnetic force stirring; after the reaction is end, naturally cooling to room temperature; then vacuum-filtering, cleaning with water, drying for 24 hours under the temperature of 100 DEG C; and finally, obtaining nano hydroxylapatite crystal doped with metal ions. The preparation method adopts a metal salt solution heating even precipitation method, and takes inorganic salts containing calcium and phosphate group as raw materials; urea is acidity of a control reaction system of an additive; metal salts are added according to the doped proportion of 1 percent to 5 percent; reaction is carried out under the magnetic force stirring and heating conditions; and the backflowing of reaction liquid is adopted to synthesize nanoscale metal-doped nano hydroxylapatite crystal by one step. The method is obviously characterized by even doping and easy control for added amount.

Description

technical field [0001] The invention belongs to the fields of biomedicine and nanometer material preparation, and in particular relates to a preparation method of metal ion-doped nano-hydroxyapatite. Background technique [0002] Hydroxyapatite (Hydroxyapatite, referred to as HAP) is the main inorganic component of natural bone, its structure is similar to natural bone, so it has good biological activity and biocompatibility (L.HENCH L.Bioceramics[J].Journal of the American Ceramic Society, 1998, 81(7): 1705-1728.). It can induce the formation of new bone in a short time after it is implanted in the body, can form osseointegration with the original damaged bone, and is non-toxic and non-carcinogenic, so it is widely used in the field of biomedical engineering as a good biomaterial. However, the infection caused by the implant material often causes premature loosening and falling off of the implant, and causes infection or even necrosis of adjacent tissues and organs, leadin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L27/12
Inventor 杨辉王栋蔡日强
Owner SHAANXI UNIV OF SCI & TECH
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