高等学校化学学报 ›› 2011, Vol. 32 ›› Issue (3): 613.

• 研究论文 • 上一篇    下一篇

硬模板法高温水热合成微孔-介孔二氧化硅及掺铝介孔二氧化硅

南海明1,2,齐娟娟1,蔡强1,孙乾耀2,徐春明2,李恒德1   

  1. 1. 清华大学材料科学与工程系,   先进材料重点实验室, 北京  100084;
    2.  中国石油大学(北京)化学化工学院, 重质油加工国家重点实验室, 北京  102249
  • 收稿日期:2010-10-18 修回日期:2010-12-12 出版日期:2011-03-10 发布日期:2011-02-23
  • 通讯作者: 蔡强;孙乾耀 E-mail:caiqiang@mail.tsinghua.edu.cn;qysun@cup.edu.cn
  • 基金资助:

    国家自然科学基金(批准号: 20676149)和中国石油大学(北京)重质油加工国家重点实验室开放基金资助.

High Temperature Synthesis of Hydrothermally Stable Micro-mesoporous Silica and Al-Doped Mesoporous Silica via Rigid Template

NAN Hai-Ming1,2, QI Juan-Juan1, CAI Qiang1*, SUN Qian-Yao2*, XU Chun-Ming2, LI Heng-De1   

  1. 1.  Key Laboratory of Advanced Materials,  Department of Materials Science and Engineering, Tsinghua University,  Beijing 100084,    China;
    2.  State Key Laboratory of Heavy Oil Processing,  Faculty of Chemical Science and Engineering, China University of Petroleum,  Beijing 102249,  China
  • Received:2010-10-18 Revised:2010-12-12 Online:2011-03-10 Published:2011-02-23
  • Contact: CAI Qiang;SUN Qian-Yao E-mail:caiqiang@mail.tsinghua.edu.cn;qysun@cup.edu.cn
  • Supported by:

    国家自然科学基金(批准号: 20676149)和中国石油大学(北京)重质油加工国家重点实验室开放基金资助.

摘要: 摘要 采用高温水热合成的方法有利于得到具备高水热稳定性的介孔二氧化硅.本研究中,我们利用α-亚麻酸在加热条件下通过胶束内聚合转化为能够耐受高温水热环境的介观模板,利用此硬模板在高温水热条件下直接合成了微孔-介孔二氧化硅及掺铝介孔二氧化硅.采用了不同的表征手段如X射线衍射(XRD),氮气吸附,透射电镜等手段对材料进行了表征. 实验结果表明,制得的材料在沸水中处理5天后,仍能保持670m2 g-1的比表面积.透射电镜结果和NLDFT孔径分析结果显示,材料同时具备介孔和微孔结构.29Si MAS NMR谱图显示,完全缩聚的Q4型硅为材料中主要的硅组分,这解释了材料的高水热稳定性.

关键词: 关键词 胶束内聚合, 水热稳定, α-亚麻酸, 微介孔材料

Abstract: Abstract: High temperature condition is helpful to obtain hydrothermally stable mesoporous silica. In this paper, we synthesized micro-mesoporous silica (designated as TCM-1) and Al-doped mesoporous silica (Al-TCM-1) under high temperature. The self-assembly of α-linolenic acid, which transformed to a rigid mesophase template via inter-micelle polymerization, were successfully leveraged to fabricate hydrothermally stable mesoporous silicas that retained a BET surface area of 678 m2g-1 after hydrothermal treatment in boiling water for 5 days. The 29 Si MAS NMR spectras of as calcined TCM-1 indicates Q4 silicons (Qn= Si(OSi)n(OH)4-n) are dominating, which can explain the high hydrothermal stability of the material.

Key words: Key words: α-linolenic acid, Hydrothermal stable, Inter-molecular polymerization, Micro-mesoporous materials

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