高等学校化学学报

高等学校化学学报

• 研究论文 • 上一篇    下一篇

蒸气促进干胶法合成硅胶负载的TS-1纳米晶

柯学斌1, 徐莉1, 曾昌凤2, 张利雄1, 徐南平1   

    1. 南京工业大学化学化工学院, 材料化学工程国家重点实验室,
    2. 南京工业大学机械与动力工程学院, 南京 210009
  • 收稿日期:2007-01-22 修回日期:1900-01-01 出版日期:2007-08-10 发布日期:2007-08-10
  • 通讯作者: 张利雄

Synthesis of TS-1 Nanocrystals on Silica Gel via Steam-assisted Dry Gel Conversion Method

KE Xue-Bin1, XU Li1, ZENG Chang-Feng2, ZHANG Li-Xiong1*, XU Nan-Ping1   

    1. State Key Laboratory of Materials-oriented Chemical Engineering, College of Chemistry and Chemical Engineering;
    2. College of Mechanical and Power Engineering, Nanjing University of Technology, Nanjing 210009, China
  • Received:2007-01-22 Revised:1900-01-01 Online:2007-08-10 Published:2007-08-10
  • Contact: ZHANG Li-Xiong

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被引次数

15

摘要： 采用蒸气促进的干胶法, 在工业硅胶上原位合成出TS-1纳米晶. 先用TS-1合成液浸渍硅胶, 再于130 ℃下和水蒸气作用2 d, 得到硅胶上负载的TS-1纳米晶. 采用XRD, FTIR, UV-Vis和NMR谱以及N2吸附、 ICP、 SEM和TEM等对所得样品进行了表征. 结果表明, 将TS-1纳米晶负载在硅胶上, 其晶粒大小为20 nm左右, Ti进入了分子筛的骨架; 所得的TS-1/silica gel复合材料的比表面积为113.2 m2/g, 平均中孔孔径达到23.7 nm. 将其用于苯的羟基化反应, 以n(C6H6)/n(H2O2)=3进料, 环丁砜为溶剂, 于100 ℃下反应2 h, 苯的转化率达到8.7%, 苯酚的选择性超过99%, 苯的氧化速率(TOF)为11.37, 其催化活性明显高于传统水热合成的TS-1.

关键词: 纳米晶, TS-1, 干胶转化法, 硅胶

Abstract: TS-1 nanocrystals were synthesized on silica gel via dry gel conversion method, at first silica gel was impregnated with TS-1 synthesis solution and then followed by steam treatment at 130 ℃ for 2 d. The product was characterized with XRD, FTIR, UV-Vis, NMR, N2 adsorption, ICP, SEM and TEM. The results indicate that TS-1 crystals were grown on silica gel with a size of ca. 20 nm, a BET specific surface area of 113.2 m2/g and a mesopore size of 23.7 nm. The product exhibited a higher catalyst performance than TS-1 powders, which was prepared by conventionally hydrothermal synthesis, for benzene hydroxylation with n(benzene)/n(H2O2)=3 and sulfolane as the solvent at 100 ℃ for 2 h. The benzene conversion and TOF were 8.7% and 11.37, respectively, with more than 99% of phenol selectivity.

Key words: Nanocrystal, TS-1, Dry gel conversion method, Silica gel

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