溶胶-凝胶法制备纳米二氧化硅及原位改性  

Preparation and in situ modification of nano-SiO_2 by sol-gel method

作　　者：阙永生[1] 杨辉[1] 汪海风[1] 吴春春[1] 潘崇根[1] 陈远[1] 

机构地区：[1]浙江大学浙江加国际纳米技术研究院,浙江杭州310058

出　　处：《无机盐工业》2015年第9期13-17,共5页Inorganic Chemicals Industry

基　　金：浙江省科技计划项目公益性项目(2014C31120);中央高校基本科研业务费专项资金资助(2014QN81006);浙江省教育厅科研计划项目(Y201225468);浙江省博士后基金(Bsh1201017)资助

摘　　要：采用溶胶-凝胶法制备了纳米二氧化硅,并成功进行了γ-甲基丙烯酰氧丙基三甲氧基硅烷（KH570）原位改性。采用X射线衍射（XRD）、红外光谱（FT-IR）、透射电镜（TEM）、激光粒度仪等方法对产物的结构和形貌进行了表征。结果表明：制备的纳米二氧化硅粒径大小为25-40 nm,类球形,粒度分布均匀,且有一定的结晶度;正硅酸乙酯（TEOS）8 mL/min的进料速度为该体系条件下二氧化硅转化率达到100%的最大进料速度;酸性（pH=3）与碱性（pH=9）改性条件相比,前者改性后的纳米二氧化硅边界不清晰,易粘连和团聚,而后者相反;KH570与二氧化硅物质的量比为20%时改性效果最佳,改性后物质在老化温度为60℃条件下在二甲苯中能够稳定750 h,并对相关反应机理进行了探讨。Nano-Si O2 was prepared and successfully in situ modified with KH570 by sol-gel method.XRD,FT-IR,TEM,and laser particle size analyzer were employed to characterize the structure and morphology.Results showed that： the size of nanoSi O2 prepared was mainly within 25 -40 nm,spherical-like,uniform in particle size distribution,and there was a certain degree of crystallinity;the feed flow rate of 8 mL/min of ethyl orthosilicate（TEOS） was the maximum feed rate to reach 100%conversion rate for the system;the modification conditions between acidic（pH=3） and alkaline（pH=9）,the former modified nano-Si O2′ boundary was not clear,and prone to cohere and agglomerate,while,the latter was just on the opposite; the amount-of-substance ratio of KH570/Si O2 was equal to 20%,which was the optimal conditions for coupling agent modification,and the modified nano-Si O2 can be stable for 750 h in xylene at aging temperature of 60 ℃.The related reaction mechanism was also discussed.

关 键 词：溶胶-凝胶 纳米二氧化硅 原位改性 

分 类 号：TQ127.2[化学工程—无机化工]