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整体型微孔-大孔Silicalite-1@SiO_2的制备与表征 被引量:1

Preparation and Characterization of Monolithic Micro-macroporous Silicalite-1@SiO_2
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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.
作者 陶凯 程文静 吴燕飞 李笑迎 梁云霄 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)
出处 《硅酸盐通报》 CAS CSCD 北大核心 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)
关键词 整体型 大孔SiO2 Silicalite-1纳米颗粒 多级孔 苯酚吸附 monolithic macroporous SiO2 Silicalite-1 nanoparticle hierarchical porous phenol adsorption
作者简介 陶凯(1995-),男,硕士研究生.主要从事无机多孔材料的制备及应用的研究.;通讯作者:梁云霄,博士,教授.
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