【作者】 张家新；

【导师】 金名惠；

【作者基本信息】 华中科技大学 ， 应用化学， 2005， 硕士

【摘要】 本文结合纳米ZnO 和纳米TiO₂的优点,研制得一种在280nm～400nm 全波段均可吸收的防晒剂。以硫酸钛、醋酸锌为原料,用溶胶凝胶法制备了ZnO/TiO₂复合颗粒。应用FT-IR、TEM、UV-Vis 等测试手段对所得粒子的结构和性质进行了表征。结果表明:通过控制锌钛浓度比、锌钛浓度、氨水浓度、络合剂和分散剂用量、煅烧温度等,可以制得致密包覆的纳米ZnO/TiO₂复合颗粒,粒径分布在50nm～100nm 之间,且分散均匀。结合表征结果,对纳米ZnO/TiO₂复合粒子的形成机理进行了初步探讨。本文尝试用有机硅氧烷对复合粒子进行改性:①利用γ-（甲基丙稀酰氧基）丙基三甲氧基硅烷偶联剂（KH-570）对纳米ZnO/TiO₂ 复合颗粒进行表面改性,使其表面接入不饱和双键,接着加入甲基丙烯酸甲酯（MMA）的单体中,使其发生共聚反应,完成纳米ZnO/TiO₂ 复合颗粒的接枝聚合改性; ②采用乳液聚合法用八甲基环四硅氧烷（D4）对ZnO/TiO₂复合颗粒进行表面接枝改性。对改性后的产物进行FT-IR 测试分析,证实了在ZnO/TiO₂ 复合颗粒表面确实接枝了一层有机物。亲水亲油测试结果显示改性后的复合颗粒由亲水性变为亲油性。经UV-Vis、催化性能测试显示:经过KH-570+MMA（KML）和D4（DL）改性后的复合颗粒紫外吸收性能很好,催化性能有明显的下降,特别是经过D4 改性的复合颗粒的催化性能几乎为零。将KML 和DL 应用到化妆品中与市场上的防晒露――雅芳夏日之恋防晒露SPF/FPS30（YFSPF30）和小护士美白防晒露SPF15（XFSPF15）所测得的紫外吸收性能进行对比,发现KML 和DL 的紫外吸收性能差不多,在波长小于355.2595nm 波段内它们的紫外吸收性能要比XFSPF15 强得多,但比YFSPF30 要差一些,在355.2592nm～400nm 波段内,它们的紫外吸收性能比YFSPF30 和XFSPF15 都要强得多。本研究表明经过D4 改性的纳米ZnO/TiO₂复合颗粒可作为一种安全的广谱防晒剂,并且有良好的应用前景。更多还原

【Abstract】 Nanometer ZnO/TiO₂ as broad spectrum sunscreen has been gained combining the strongpoint of nanometer ZnO with nanometer TiO₂. The ZnO/TiO₂ composite particles were prepared by sol-gel with Ti（SO4）2 and Zn（AC）2 as raw materials .The surface structure of samples was characterized by IR/TEM/XRD/UV-vis .The results show that the diameter of the composite particles is 50nm-100nm by controlling the different reaction conditions and they have the structure of TiO₂ as core and ZnO as shell .From the results of the characterization we discussed the formative mechanism of the ZnO/TiO₂ composite particle . Because of the strong polarity the nanometer particles agglomerate easily in the un-polarity solutions. we attempted to modify the composite particles with organosiloxane:①Silane coupling agents（KH-570）and methyl methacrylate（MMA） were initiated to polymerize at the surface of nanometer ZnO/TiO₂ composite particles utilizing the un-saturation bonds and hydroxyl in the surface of ZnO/TiO₂ composite particles and the “bridge”actions of the silane coupling agents. ②Cyclomethicones（D4） modified the ZnO/TiO₂ composite particles via emulsion polymerization .The analysis of FT-IR indicates that there are some graft polymer at the ZnO/TiO₂ composite particles .The surface properties of modified composite particles were studied by dispersability and penetration, the results appear that the modification of composite particles can improve both the lipophilicity and dispersion properties .The result of UV-vis absorption spectroscopy indicates the composite particles have elegant ultraviolet absorption, the photocatalytic experiment reveals that the photocatalysis of the modified particles decrease badly, especially the photocatalysis for D4 modified composite particles can be shielded almost completely. Introduced the composite particles into the cosmetic, we have achieved the fine stability. We compared the ultraviolet absorption of sun block （KML and DL） made by ourselves with the Avon’s day block SPF30（YFSPF30）and Mininurse’s SPF15（XFSPF15）,the results display the ultraviolet absorption of KML is as much as the DL .During 280nm-355.2595nm wavelength the ultraviolet absorption of DL excels to XFSPF15,and less than YFSPF30; In the scope of 355.2595nm-400nm wavelength the ultraviolet absorption of DL is stronger greatly than XFSPF15 and YFSPF30.In a conclusion the effect of the ZnO/TiO2 composite particles on ultraviolet prevention in the whole ultraviolet wavelength is excellent and it is also safe.更多还原