整体型微孔-大孔Silicalite-1@SiO_2的制备与表征  

Preparation and Characterization of Monolithic Micro-macroporous Silicalite-1@SiO_2

作　　者：陶凯[1] 程文静 吴燕飞[1] 李笑迎[1] 梁云霄[1] TAO Kai;CHENG Wen-jing;WU Yan-fei;LI Xiao-ying;LIANG Yun-xiao(State Ke y Laboratory Base of Novel Functional Materials and Preparation Science,School of Materials Science and Chemical Engineering,Ningbo University ,Ningbo 315211, China)

机构地区：[1]宁波大学材料科学与化学工程学院新型功能材料及其制备科学国家重点实验室培育基地,宁波315211

出　　处：《硅酸盐通报》2018年第4期1404-1410,共7页Bulletin of the Chinese Ceramic Society

基　　金：浙江省公益项目(2014C31130);宁波市科技惠民项目(2017C50033);宁波大学王宽诚幸福基金(XKL072)

摘　　要：以整体型柱撑式大孔聚合物为模板,制备出由SiO_2纳米薄膜构筑的具有三维连续贯通孔道结构的整体型大孔SiO_2,通过Silicalite-1前驱体溶液浸渍,在水热条件下制得不同规则形状的整体型Silicalite-1@SiO_2材料。用SEM、XRD、MIP(压汞法)和BET技术对材料进行了表征。结果表明:Silicalite-1@SiO_2的大孔孔径主要分布在0.5~1μm之间,大孔SiO_2孔壁上原位生长出直径为100~200 nm的Silicalite-1纳米颗粒,Silicalite-1纳米颗粒与大孔SiO_2孔壁通过化学键结合到一起。水热晶化10 h的Silicalite-1@SiO_2样品在保证整体型SiO_2机械稳定性的同时达到最高结晶度,其比表面积(352 m^2/g)和微孔体积(0.088 cm^3/g)与整体型大孔SiO_2相比均明显提高,并且Silicalite-1@SiO_2具有很好的苯酚吸附性能。The monolithic macroporous Si02 with three-dimensional （3D） interconnected channel structure constructed by Si02 nano-film was prepared by pillared monolithic macroporous polymer as template. Then, the various regular shaped monolithic Silicalite-1 @ Si02 was prepared under hydrothermal condition by immersing the macroporous Si02 in the Silicalite-1 precursor solution. All materials were characterized by SEM, XRD, MIP （mercury intrusion porosimetry） and BET. The results show that the macropore size of Silicalite-1 @ Si02 is 0. 5-1 jjim, and the Silicalite-1 nanoparticles with a diameter between 100 and 200 nm are in situ grown on the wall of the macroporous Si02. Silicalite-1 nanoparticles are combined with the wall of macroporous Si02 through chemical bonds. Silicalite-1 @ Si02 shows highest crystallinity when the hydrothermal crystallization time is 10 h and the Silicalite-1 @ Si02 sample maintains the structure stability of macroporous Si02. Compared with monolithic macroporous Si02,the specific surface area （352 m2/g） and micropore volume （0.088 cm3/g） of Silicalite-1 @SiO2 are significantly increased. Meanwhile, Silicalite-1 @ Si02 exhibits excellent phenol adsorption property.

关 键 词：整体型 大孔SiO2 Silicalite-1纳米颗粒 多级孔 苯酚吸附 

分 类 号：O613.7[理学—无机化学]