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A kind of preparation method of nano-hydroxyapatite

A technology of nano-hydroxyapatite and phosphoric acid, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of long reaction cycle and aging time, and achieve low cost, easy industrialization and wide selection range Effect

Inactive Publication Date: 2014-10-08
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Bose et al. (Bose S, Saha S K. Synthesis and Characterization of Hydroxyapatite Nanopowders by Emulsion Technique, Chem Mater, 2003, 15(23): 4464-4469) the specific surface area of ​​hydroxyapatite prepared by the template method can reach 130m 2 / g, the particle size is 30-50nm, but the reaction cycle and aging time are long

Method used

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  • A kind of preparation method of nano-hydroxyapatite
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  • A kind of preparation method of nano-hydroxyapatite

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Experimental program
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Embodiment 1

[0029] Drugs: phosphoric acid (Sinopharm Chemical Reagent Co., Ltd., AR, purity ≥ 85.0%), absolute ethanol (Sinopharm Chemical Reagent Co., Ltd., AR), calcium hydroxide (Sinopharm Chemical Reagent Co., Ltd., AR, purity ≥ 95.0%) ). The preparation method is as follows:

[0030] 1) Accurately weigh 467.36g of calcium hydroxide and place it in a 250ml beaker, add 60ml of water, stir and disperse to form a 0.1MCa(OH)2 suspension, place the beaker in a water bath, and stir mechanically at a stirring speed of 450rpm. which is:

[0031] Ca(OH) 2(s) +H 2 O→Ca(OH) 2(sus)

[0032] 2) Accurately weigh 4.15g of phosphoric acid and add it to 60ml of water to prepare a 0.06M phosphoric acid solution.

[0033] 3) Heat the water bath to 80°C, use a syringe pump (syringe needle size: 1.2×38mm) to drop 60ml of phosphoric acid solution into the Ca(OH)2 suspension at a constant speed of 60ml / h, and stir to react. After the dropwise addition, the stirring reaction was continued for 1 h to obt...

Embodiment 2

[0041] Drugs: phosphoric acid (Sinopharm Chemical Reagent Co., Ltd., AR, purity ≥ 85.0%), absolute ethanol (Sinopharm Chemical Reagent Co., Ltd., AR), egg shells (provided by Furong Restaurant, Xiamen University).

[0042] Similar to Example 1, the difference is:

[0043] 1. Use eggshells as the calcium source, first use n-hexane to remove the dirt and solid organic matter on the eggshells, then use distilled water and detergent to remove the film and adherents on the eggshells, and finally dry at 80°C and crush to less than 100 mesh. Eggshells react at 950°C for 5 hours to generate CaO. The specific chemical reaction formula is as follows:

[0044]

[0045] 2. The dropping rate of phosphoric acid is 25ml / h.

[0046] 3. After the phosphorus source is added dropwise, continue stirring and the reaction time is 30 minutes.

[0047] The obtained hydroxyapatite was calcined at 700°C and 900°C for 2 hours, and it was still a nanoscale powder. The measurement results of XRD an...

Embodiment 3

[0049] Drugs: phosphoric acid (Sinopharm Chemical Reagent Co., Ltd., AR, purity ≥ 85.0%), absolute ethanol (Sinopharm Chemical Reagent Co., Ltd., AR), egg shells (Furong Restaurant, Xiamen University).

[0050] The present embodiment adopts the same process and equipment as in Embodiment 2, the difference being that the dropping rate of phosphoric acid is 200ml / h.

[0051] The obtained hydroxyapatite was calcined at 700°C and 900°C for 2 hours, and it was still a nanoscale powder. The measurement results of XRD and BET show that the specific surface area, pore volume, pore diameter and grain size of HAp are 160.1m 2 / g, 1.0cm 3 / g, 24.98nm and 10nm.

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Abstract

The invention provides a preparation method of nano-hydroxyapatite, and relates to hydroxyapatite. According to the preparation method, a technology is simple, no additives are added in a reaction process, no byproducts are generated, and the nano-hydroxyapatite can be synthesized at a normal temperature and has high equilibrium temperature, a large specific surface area and large pore volume. The preparation method comprises the steps of: (1) weighing a carbon source, adding distilled water, stirring and dispersing to obtain a Ca(OH)2 suspension liquid; (2) adding phosphoric acid to the Ca(OH)2 suspension liquid, stirring and reacting till the molar ratio of calcium to phosphor is 1.67, stopping adding the phosphoric acid, continuously stirring and reacting to obtain reaction liquid; and (3) filtering and separating the reaction liquid to obtain white precipitates, washing the white precipitates by water and an organic solvent and drying to obtain white powder, namely the nano-hydroxyapatite. The obtained nano-hydroxyapatite has the large specific surface area and a dominant pore structure. The preparation method is simple in technology without special equipment requirements, low in cost and suitable for large-scale industrialization.

Description

technical field [0001] The invention relates to hydroxyapatite, in particular to a method for preparing nano-hydroxyapatite with high specific surface area and high pore diameter. Background technique [0002] Hydroxyapatite (Hydroxyapatite, abbreviated as HAp) widely exists in nature and organisms, has good biocompatibility, biological activity, chemical stability and solid alkalinity, and is widely used in biomedicine, tissue engineering, drug controlled release Therefore, the development and research of nano-scale hydroxyapatite with high purity, thermal stability, especially high specific surface area and high pore volume is of great significance. [0003] At present, the preparation methods of hydroxyapatite mainly include solid phase reaction method, hydrothermal method, sol-gel method, precipitation method, microemulsion method, etc., such as publication numbers CN86108700, CN1760121, CN100999313, CN101486452, CN102491299A, CN102431986A, Chinese patents such as CN101...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32B82Y30/00
Inventor 李军易卜拉辛·阿卜杜勒·拉夫洪燕珍苏玉忠王宏涛
Owner XIAMEN UNIV