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气相法制备ZIF-8纳米膜包覆Pt/SiO2催化剂及其炔烃半加氢性能

罗根 张斌 杨新春 武慧斌 孟繁春 翟黎明 覃勇

罗根, 张斌, 杨新春, 武慧斌, 孟繁春, 翟黎明, 覃勇. 气相法制备ZIF-8纳米膜包覆Pt/SiO2催化剂及其炔烃半加氢性能[J]. 燃料化学学报. doi: 10.1016/S1872-5813(21)60075-0
引用本文: 罗根, 张斌, 杨新春, 武慧斌, 孟繁春, 翟黎明, 覃勇. 气相法制备ZIF-8纳米膜包覆Pt/SiO2催化剂及其炔烃半加氢性能[J]. 燃料化学学报. doi: 10.1016/S1872-5813(21)60075-0
LUO Gen, ZHANG Bin, YANG Xin-chun, WU Hui-bin, MENG Fan-chun, ZHAI Li-ming, QIN Yong. The Synthesis of ZIF-8 Nano-Film-coated Pt/SiO2 by Chemical Vapor Deposition for Alkyne Semi-hydrogenation[J]. Journal of Fuel Chemistry and Technology. doi: 10.1016/S1872-5813(21)60075-0
Citation: LUO Gen, ZHANG Bin, YANG Xin-chun, WU Hui-bin, MENG Fan-chun, ZHAI Li-ming, QIN Yong. The Synthesis of ZIF-8 Nano-Film-coated Pt/SiO2 by Chemical Vapor Deposition for Alkyne Semi-hydrogenation[J]. Journal of Fuel Chemistry and Technology. doi: 10.1016/S1872-5813(21)60075-0

气相法制备ZIF-8纳米膜包覆Pt/SiO2催化剂及其炔烃半加氢性能

doi: 10.1016/S1872-5813(21)60075-0
基金项目: 本文得到国家自然科学基金(22072172, 21872160),中国科学院青年创新促进会(2017204),山西省自然科学基金(201901D211591),国家杰出青年科学基金(21825204)等项目的支持
详细信息
    通讯作者:

    Tel/Fax: 0351–4040420. Email: zhangbin2009@sxicc.ac.cn

  • 中图分类号: O643.38

The Synthesis of ZIF-8 Nano-Film-coated Pt/SiO2 by Chemical Vapor Deposition for Alkyne Semi-hydrogenation

Funds: The project was financially supported by the National Natural Science Foundation of China (22072172, 21872160), the Youth Innovation Promotion Association CAS (2017204), and Natural Science Foundation of Shanxi Province (201901D211591), The National Science Fund for Distinguished Young Scholars (21825204)
  • 摘要: 以原子层沉积技术与气相转晶法相结合的方法,制备出ZIF-8/Pt/SiO2催化剂。该催化剂中Pt纳米颗粒沉积在SiO2纳米线表面,进一步通过气相法被厚度可控的ZIF-8纳米薄膜包覆后形成三明治结构。通过XRD、TEM、BET、ICP–MS、XPS、CO–DRIFT等表征对催化剂结构进行了系统的分析,以1–庚炔加氢为探针反应研究了ZIF-8薄膜对Pt催化性能的影响。结果表明,Pt颗粒高度分散在SiO2纳米线上,所制备的ZIF-8薄膜厚度可控,能够实现Pt/SiO2纳米催化剂表面的均一、保形性包覆。ZIF-8薄膜改变了Pt电子状态,提高了 Pt表面电子密度。在1-庚炔加氢反应中,ZIF-8包覆后, Pt催化庚炔加氢制庚烯的选择性由14%增加到70%。此外,降低ZIF-8纳米薄膜厚度能够提高反应的活性,几乎不影响烯烃的选择性。
  • 图  1  ZIF-8/Pt/SiO2催化剂制备示意图

    Figure  1.  Schematic diagram of preparation of ZIF-8/Pt/SiO2 catalyst.

    图  2  载体和催化剂的XRD图谱

    Figure  2.  XRD patterns of support and catalysts

    图  3  (a)20Pt/SiO2,(b)100ZnO/20Pt/ SiO2,(c) 30ZIF-8/20Pt/SiO2,(d)、(e) 50ZIF-8/20Pt/SiO2和 (f)100ZIF-8/20Pt/SiO2的TEM图

    Figure  3.  TEM image of 20Pt/SiO2 (a), 100ZnO/20Pt/ SiO2 (b), 30ZIF-8/20Pt/SiO2(c), 50ZIF-8/20Pt/SiO2 (d-e) and 100ZIF-8/20Pt/SiO2 (f)

    图  4  (a) SiO2和30ZIF-8/20Pt/SiO2的氮气吸脱附曲线;(b) SiO2和30ZIF-8/20Pt/SiO2的孔径分布图

    Figure  4.  (a) Nitrogen absorption and desorption curve of SiO2 and 30ZIF-8/20Pt/SiO2; (b) Pore size distribution diagram of SiO2 and 30ZIF-8/20Pt/SiO2

    图  5  20Pt/SiO2和30ZIF-8/20Pt/SiO2催化剂的XPS图谱

    Figure  5.  XPS spectra of 20Pt/SiO2 and 30ZIF-8/20Pt/SiO2 catalyst

    图  6  20Pt/SiO2xZIF-8/20Pt/SiO2催化剂CO原位红外谱图

    Figure  6.  In-situ CO-DRIFT study of 20Pt/SiO2, xZIF-8/20Pt/SiO2 catalyst

    图  7  反应时间对20Pt/SiO2(a)、10ZIF-8/20Pt/SiO2(b)、30ZIF-8/20Pt/SiO2(c)、50ZIF-8/20Pt/SiO2(d)催化1–庚炔加氢反应性能的影响

    Figure  7.  Effect of reaction time on the catalytic performance of 20Pt/SiO2 (a), 10ZIF-8/20Pt/SiO2 (b), 30ZIF-8/20Pt/SiO2 (c) and 50ZIF-8/20Pt/SiO2 (d) in the hydrogenation of 1–heptyne

    图  8  1–庚炔 (a) 和1–庚烯 (b) 在Pt/SiO2和30ZIF-8/20Pt/SiO2表面的红外吸附对比图

    Figure  8.  Comparison of infrared adsorption of 1–heptyne (a) and 1–heptene (b) on Pt/SiO2 and 30ZIF-8/20Pt/SiO2 surfaces

    图  9  30ZIF-8/20Pt/SiO2催化剂1–庚炔加氢的稳定性测试

    Figure  9.  Stability test of 30ZIF-8/20Pt/SiO2 in the hydrogenation of 1–heptyne

    表  1  催化剂的比表面积和孔道结构

    Table  1.   The surface area and pore structure of the catalysts

    SampleABET
    (cm2·g−1)
    Vmicro
    (cm3·g−1)
    dmicro
    (nm)
    Vmeso
    (cm3·g−1)
    dmaso
    (nm)
    SiO272.0000.16.6
    10ZIF-8/20Pt/SiO2290.40.061.20.13.6
    30ZIF-8/20Pt/SiO2320.20.101.20.13.6
    50ZIF-8/20Pt/SiO2420.10.111.20.13.5
    ABET:BET表面积;Vmicro:使用HK方法得到微孔体积;dmicro:使用HK方法得到微孔平均直径;Vmeso:使用BJH方法得到介孔体积;dmaso:使用BJH方法得到介孔平均直径
    下载: 导出CSV

    表  2  不同样品上Pt、Zn元素的负载量

    Table  2.   Pt and Zn loading on different samples

    Sample20Pt/SiO210ZIF-8/20Pt/SiO230ZIF-8/20Pt/SiO2
    wt(Pt)/%2.91.81.6
    wt(Zn)/%06.927.3
    下载: 导出CSV

    表  3  不同催化剂的1-庚炔加氢反应性能a

    Table  3.   Catalytic performance of different catalysts for 1-heptyne hydrogenation

    SampleReaction time (min)Conversion (%)Selectivity (%)CO adsorption (mmol·g−1)bTOF c(10−4·h−1)
    20Pt/SiO230100140.1051.6
    10ZIF-8/20Pt/SiO2235100650.041.62
    30ZIF-8/20Pt/SiO2445100700.022.36
    50ZIF-8/20Pt/SiO21155100670.0060.66
    a. 反应条件:100 μL1–庚炔,15 mg催化剂,10 mL异丙醇,反应温度60 ℃,1 MPa氢气。b. CO吸附数据。c. TOF = Nconversed heptyne /(NCO × t),其中N表示摩尔数,t表示反应时间(h)。
    下载: 导出CSV
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