贻贝壳在不同方法下合成羟基磷灰石多孔微球的性能研究

Study on the synthesis and properties of porous hydroxyapatite microspheres from mussel shells with various methods

选用舟山市贻贝壳为原料制备羟基磷灰石(HA)多孔微球,球形HA较其他形状的HA有更多的药物和金属负载量,可以合成特殊的功能性材料.实验过程为:采用贻贝壳提取CaCO_(3),以贻贝壳的CaCO_(3)为原料,用水热法、沉淀法、十六烷基三甲基溴化铵模板剂法及反相微乳液法制备HA,经比较确定可行方案,并对制备出的样品进行银离子吸附实验.研究结果表明:通过扫描电子显微镜表征观察得出水热法制备的产物为球形;X射线粉末衍射仪和傅里叶红外光谱仪测得水热法制得的产物为HA,其他产物为方解石型CaCO_(3)/HA复合材料;比表面积及微孔孔隙分析表征得出水热法制备的产物介孔结构和比表面积最优;电感耦合等离子体发射光谱仪检测产物的钙磷比及载银量,确定水热法制备的样品为缺磷型HA,该HA的银离子吸附率达75.10%.表明贝壳制备HA多孔微球是可行的,采用水热法可将贝壳CaCO_(3)合成球形多孔HA,且在转化程度和载银效果方面较其他方法更有优势.

Mussel shells of Zhoushan City were selected as raw materials for preparing hydroxyapatite(HA)porous microspheres.Compared with HA in other shapes,spherical HA possesses more drug and metal loading capacities,and can be used to synthesize materials with special functions.The experimental process was as follows:CaCO_(3)was extracted from mussel shells and used as raw material to prepare HA with hydrothermal method,pecipitation method,sixteen alkyl three methyl ammonium bromide template method and inverse micro-emulsion method.The study was aimed to determine the feasible method and implement the silver loading experiment on prepared samples.Shown by scanning electron microscopy,HA prepared by hydrothermal method was spherical.Shown by X-ray powder diffractometer and fourier transform infrared spectrometer(FTIR),one product prepared by hydrothermal method was HA and the other products were calcite type CaCO_(3)/HA composites.The micro pore analysis showed that the product prepared by hydrothermal method was provided with optimal mesoporous structure.Inductively coupled plasma emission spectrometer was used to detect the ratio of calcium to phosphorus and silver loading capacity of the product.The sample prepared by hydrothermal method was phosphorus deficient HA and the silver ion adsorption rate was 75.10%.The results show that it is feasible to prepare HA porous microspheres from shells.Using hydrothermal method,shell CaCO_(3)can be fully utilized and synthesized into spherical porous HA with great silver loading effect.