一步溶胶-凝胶法制备乙烯基功能化二氧化硅微球及其表征

Preparation of vinyl-functionalized silica microspheres by one-step sol-gel method and their characterization

以乙烯基三乙氧基硅烷(VTES)为硅源、乙醇和水为溶剂,氨水为催化剂,通过一步溶胶?凝胶法制备了粒径分布为2~11μm的乙烯基功能性二氧化硅微球(V-SiO2)。探究了温度、水硅比、醇硅比、氨硅比和对合成反应及产物形貌的影响,并对产物进行了热重(TG)、扫描电镜(SEM)、傅里叶变换红外光谱(FT-IR)、接触角测量等方面的表征。结果表明:30~50℃时,VTES水解?缩聚反应完全;水硅比越大,体系凝胶时间越长;醇硅比越大,产物球形越规整;氨硅比越大,产物粒径分布范围越窄。产物V-SiO2是具有反应潜能的超疏水材料,可用于分离、检测、陶瓷制造等领域,也可用作引入其他成分的基础材料。

Vinyl-functionalized silica(V-SiO2)microspheres with a size range of 3-11μm were prepared with vinyltriethoxysilane(VTES)as precursor and ammonia as catalyst in ethanol/H2O system by one-step sol–gel method.The effects of reaction temperature as well as the ratios of H2O to VTES,ethanol to VTES,and ammonia to VTES on the synthesis and product morphology were studied.The product was characterized by thermogravimetry(TG),scanning electron microscopy(SEM),Fourier-transform infrared spectroscopy(FT-IR),and contact angle measurement.The results showed that the condensation of VTES was complete at the reaction temperature from 30°C to 50°C.The larger the ratio of H2O to VTES is,the longer the gelation time goes;the larger the ratio of ethanol to VTES is,the more regular the microspheres are;and the larger the ratio of ammonia to VTES is,the narrower the particle size distribution is.The V-SiO2 microspheres are a kind of hydrophobic material with reactivity potential suitable to be used as a basic material for introducing other components,as well as for separation,detection,ceramic production,etc.