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硅酸盐通报 ›› 2018, Vol. 37 ›› Issue (4): 1404-1410.

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整体型微孔-大孔Silicalite-1@SiO2的制备与表征

陶凯;程文静;吴燕飞;李笑迎;梁云霄   

  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
  • 出版日期:2018-04-15 发布日期:2021-01-18
  • 基金资助:
    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)

Preparation and Characterization of Monolithic Micro-macroporous Silicalite-1@SiO2

TAO Kai;CHENG Wen-jing;WU Yan-fei;LI Xiao-ying;LIANG Yun-xiao   

  • Online:2018-04-15 Published:2021-01-18

摘要: 以整体型柱撑式大孔聚合物为模板,制备出由SiO2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SiO2,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@SiO2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@SiO2的大孔孔径主要分布在0.5~1 μm之间,大孔SiO2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SiO2孔壁通过化学键结合到一起.水热晶化10 h的Silicalite-1@SiO2样品在保证整体型SiO2机械稳定性的同时达到最高结晶度,其比表面积(352 m2/g)和微孔体积(0.088 cm3/g)与整体型大孔SiO2相比均明显提高,并且Silicalite-1@SiO2具有很好的苯酚吸附性能.

关键词: 整体型;大孔SiO2;Silicalite-1纳米颗粒;多级孔;苯酚吸附

Abstract: The monolithic macroporous SiO2 with three-dimensional (3D) interconnected channel structure constructed by SiO2 nano-film was prepared by pillared monolithic macroporous polymer as template.Then, the various regular shaped monolithic Silicalite-1 @ SiO2 was prepared under hydrothermal condition by immersing the macroporous SiO 2 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@SiO2 is 0.5-1 μm, and the Silicalite-1 nanoparticles with a diameter between 100 and 200 nm are in situ grown on the wall of the macroporous SiO 2 .Silicalite-1 nanoparticles are combined with the wall of macroporous SiO 2 through chemical bonds.Silicalite-1@SiO2 shows highest crystallinity when the hydrothermal crystallization time is 10 h and the Silicalite-1@SiO2 sample maintains the structure stability of macroporous SiO 2.Compared with monolithic macroporous SiO2 , the specific surface area (352 m2 /g) and micropore volume (0.088 cm3 /g) of Silicalite-1@SiO2 are significantly increased.Meanwhile, Silicalite-1@SiO2 exhibits excellent phenol adsorption property .

Key words: monolithic;macroporous SiO2;Silicalite-1 nanoparticle;hierarchical porous;phenol adsorption

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