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固相外延生长法制备ZSM-5@Silicalite-1分子筛及其CO2加氢耦合甲苯烷基化反应的影响

贾艺敏 牛鹏宇 贾丽涛 林明桂 郭荷芹 肖勇 侯博 李德宝

贾艺敏, 牛鹏宇, 贾丽涛, 林明桂, 郭荷芹, 肖勇, 侯博, 李德宝. 固相外延生长法制备ZSM-5@Silicalite-1分子筛及其CO2加氢耦合甲苯烷基化反应的影响[J]. 燃料化学学报(中英文). doi: 10.19906/j.cnki.JFCT.2024012
引用本文: 贾艺敏, 牛鹏宇, 贾丽涛, 林明桂, 郭荷芹, 肖勇, 侯博, 李德宝. 固相外延生长法制备ZSM-5@Silicalite-1分子筛及其CO2加氢耦合甲苯烷基化反应的影响[J]. 燃料化学学报(中英文). doi: 10.19906/j.cnki.JFCT.2024012
JIA Yimin, NIU Pengyu, JIA Litao, LIN Minggui, GUO Heqin, XIAO Yong, HOU Bo, LI Debao. Effect of ZSM-5@Silicalite-1 zeolites prepared by solid phase epitaxial growth method on CO2 hydrogenation and toluene alkylation reactions[J]. Journal of Fuel Chemistry and Technology. doi: 10.19906/j.cnki.JFCT.2024012
Citation: JIA Yimin, NIU Pengyu, JIA Litao, LIN Minggui, GUO Heqin, XIAO Yong, HOU Bo, LI Debao. Effect of ZSM-5@Silicalite-1 zeolites prepared by solid phase epitaxial growth method on CO2 hydrogenation and toluene alkylation reactions[J]. Journal of Fuel Chemistry and Technology. doi: 10.19906/j.cnki.JFCT.2024012

固相外延生长法制备ZSM-5@Silicalite-1分子筛及其CO2加氢耦合甲苯烷基化反应的影响

doi: 10.19906/j.cnki.JFCT.2024012
基金项目: 山西省重点研发计划 (202102090301003)资助
详细信息
    通讯作者:

    Tel: 0351-4040428, E-mail: niupy@sxicc.ac.cn

    jialitao910@163.com

  • 中图分类号: O643

Effect of ZSM-5@Silicalite-1 zeolites prepared by solid phase epitaxial growth method on CO2 hydrogenation and toluene alkylation reactions

Funds: The project was supported by the Basic Research Program of Shanxi key research project (202102090301003).
  • 摘要: CO2加氢合成高附加值的芳烃对于缓解CO2排放引起的能源气候问题具有重要意义。本文采用固相法在ZSM-5表面外延生长Silicalite-1,制备出ZSM-5@Silicalite-1分子筛。同时制备高活性氧化物ZnZrOx,并与ZSM-5@Silicalite-1物理混合组成ZnZrOx/ ZSM-5@Silicalite-1双功能催化剂,研究了CO2加氢耦合甲苯烷基化催化性能。相比于ZnZrOx/ZSM-5催化剂,分子筛改性后的双功能催化剂提高了对二甲苯(PX)选择性。研究了晶化条件(硅源、晶化过程、晶化次数)对ZSM-5外延生长Silicalite-1的影响,以及Silicalite-1钝化层厚度对CO2加氢耦合甲苯烷基化反应性能的影响。在400 ℃、3 MPa反应条件下,ZZO/1:3.5Z5-Na-SiO2催化剂的甲苯转化率为12.0%,二甲苯选择性为77.4%,在二甲苯中对二甲苯选择性为73.4%。通过SEM、XRD、N2吸附-脱附、XPS、NH3-TPD、Py-IR等表征,详细研究了分子筛的结构和酸性质。结果表明通过固相外延生长,延长ZSM-5的孔道,增加间二甲苯(MX)、邻二甲苯(OX)的扩散阻力,同时钝化外表面的酸性,可以有效提高对二甲苯(PX)的选择性。固相外延生长法改性ZSM-5分子筛,摒弃了以往堵塞孔以缩小孔口改性分子筛的缺点,在保证催化剂活性的同时提高了产物选择性。
  • 图  1  样品(a)ZSM-5、S1:1Z5-Na-SiO2-1、S1:1Z5-TEOS-1、S1:1Z5-NH3-SiO2-1、S1:1Z5-SiO2-1,(b)S1:1Z5-Na-SiO2-2、S1:1Z5-TEOS-2、S1:1Z5-NH3-SiO2-2、S1:1Z5-SiO2-2,(c)D1:1Z5-Na-SiO2、D1:1Z5-TEOS、D1:1Z5-NH3-SiO2、D1:1Z5-SiO2的XRD谱图;(d)ZSM-5、S1:1Z5-Na-SiO2-1、S1:1Z5-TEOS-1、S1:1Z5-NH3-SiO2-1、S1:1Z5-SiO2-1的N2吸脱附等温线

    Figure  1  (a) XRD patterns of ZSM-5, S1:1Z5-Na-SiO2-1, S1:1Z5-TEOS-1, S1:1Z5-NH3-SiO2-1, and S1:1Z5-SiO2-1; (b) XRD patterns of S1:1Z5-Na-SiO2-2, S1:1Z5-TEOS-2, S1:1Z5-NH3-SiO2-2, and S1:1Z5-SiO2-2; (c) XRD patterns of D1:1Z5-Na-SiO2, D1:1Z5-TEOS, D1:1Z5-NH3-SiO2, and D1:1Z5-SiO2; and (d) N2 adsorption-desorption isotherms of ZSM-5, S1:1Z5-Na-SiO2-1, S1:1Z5-TEOS-1, S1:1Z5-NH3-SiO2-1, and S1:1Z5-SiO2-1

    图  2  样品(a)ZSM-5,(b1-e1)S1:1Z5-Na-SiO2/TEOS/NH3-SiO2/SiO2-1,(b2-e2)S1:1Z5-Na-SiO2/TEOS/NH3-SiO2/SiO2-2,(b3-e3)D1:1Z5-Na-SiO2/TEOS/NH3-SiO2/SiO2的SEM图

    Figure  2  SEM images of samples (a) ZSM-5, (b1-e1) S1:1Z5-Na-SiO2/TEOS/NH3-SiO2/SiO2-1, (b2-e2) S1:1Z5-Na-SiO2/TEOS/NH3-SiO2/SiO2-2, and (b3-e3) D1:1Z5-Na-SiO2/TEOS/NH3-SiO2/SiO2

    图  3  ZSM-5、S1:1Z5-Na-SiO2-1、S1:1Z5-TEOS-1、S1:1Z5-NH3-SiO2-1、S1:1Z5-SiO2-1的(a)XPS Al 2p谱图,(b)NH3-TPD曲线,(c)350 ℃的Py-IR谱图和(d)ZSM-5、S1:1Z5-Na-SiO2-2、S1:1Z5-TEOS-2、S1:1Z5-NH3-SiO2-2和S1:1Z5-SiO2-2的350 ℃ Py-IR谱图

    Figure  3  (a) XPS Al 2p spectra, (b) NH3-TPD curves and (c) Py-IR spectra at 350°C for ZSM-5, S1:1Z5-Na-SiO2-1, S1:1Z5-TEOS-1, S1:1Z5-NH3-SiO2-1, S1:1Z5-SiO2-1, and (d) 350°C Py-IR spectra of ZSM-5, S1:1Z5-Na-SiO2-2,S1:1Z5-TEOS-2, S1:1Z5-NH3-SiO2-2, and S1:1Z5-SiO2-2

    图  4  ZSM-5、1:1Z5-Na-SiO2、1:2Z5-Na-SiO2、1:3Z5-Na-SiO2、1:3.5Z5-Na-SiO2和1:4Z5-Na-SiO2的(a)XRD谱图和(b)N2吸脱附等温线

    Figure  4  (a) XRD patterns and (b) N2 adsorption-desorption isotherms of ZSM-5, 1:1Z5-Na-SiO2, 1:2Z5-Na-SiO2,1:3Z5-Na-SiO2, 1:3.5Z5-Na-SiO2 and 1:4Z5-Na-SiO2

    图  5  催化剂SEM图

    Figure  5  SEM images of catalysts (a) ZSM-5; (b) 1:1Z5-Na-SiO2; (c) 1:2Z5-Na-SiO2; (d) 1:3Z5-Na-SiO2;(e) 1:3.5Z5-Na-SiO2; (f) 1:4Z5-Na-SiO2

    图  6  ZSM-5、1:1Z5-Na-SiO2、1:2Z5-Na-SiO2、1:3Z5-Na-SiO2、1:3.5Z5-Na-SiO2和1:4Z5-Na-SiO2的(a)NH3-TPD曲线和(b)350 ℃的Py-IR谱图

    Figure  6  (a) NH3-TPD curves and (b) Py-IR spectra of ZSM-5, 1:1Z5-Na-SiO2, 1:2Z5-Na-SiO2, 1:3Z5-Na-SiO2,1:3.5Z5-Na-SiO2 and 1:4Z5-Na-SiO2 at 350°C

    图  7  ZnZrOx的(a)SEM图,(b)XRD谱图,(c)Raman曲线和(d)N2吸脱附等温线

    Figure  7  (a) SEM image, (b) XRD patterns, (c) Raman spectra and (d) N2 adsorption-desorption isotherms of ZnZrOx

    图  8  ZnZrOx的(a)H2-TPR曲线,(b)XPS O 1s 谱图,(c)EPR谱图,(d)CO2-TPD曲线和(e)H2-TPD曲线

    Figure  8  (a) H2-TPR curve, (b) XPS O 1s spectra, (c) EPR spectra, (d) CO2-TPD curve and (e) H2-TPD curve of ZnZrOx

    图  9  CO2加H2与甲苯烷基化反应(a)在不同硅源制备的ZSM-5@Silicalite-1和ZnZrOx的双功能催化剂上的液相产物选择性,(b)气相产物选择性,(c)不同晶化次数的ZSM-5@Silicalite-1和ZnZrOx的双功能催化剂上的液相产物选择性和(d)不同钝化层厚度分子筛和ZnZrOx的双功能催化剂上的液相产物选择性,反应条件:400 ℃,3 MPa,H2/CO2为3∶1,GHSV为9000 h−1,甲苯LHSV为2 h−1

    Figure  9  CO2 hydrogenation and toluene alkylation reactions (a) liquid-phase product selectivity over bifunctional catalysts of ZSM-5@Silicalite-1 and ZnZrOx prepared with different silicon sources, (b) gas-phase product selectivity, (c) liquid-phase product selectivity over bifunctional catalysts of ZSM-5@Silicalite-1 and ZnZrOx with different numbers of crystallizations and (d) liquid-phase product selectivity over bifunctional catalysts of zeolites with different shell thicknesses and ZnZrOx. Reaction conditions: 400 ℃, 3 MPa, H2/CO2=3/1, GHSV=9000 h−1, and LHSV of toluene = 2 h−1.

    表  1  ZSM-5和S1:1Z5@Silicalite-1分子筛的织构性质

    Table  1  Textural properties of ZSM-5 and S1:1Z5@Silicalite-1 zeolite

    Catalyst Relative crystallinity/% BET Surface Area S/(m2·g−1) Pore Volume v/(cm3·g−1) Pore Size d/(nm)
    ZSM-5 100 364 0.15 1.92
    S1:1Z5-SiO2-1 87 325 0.13 3.96
    S1:1Z5-SiO2-2 84 443 0.18 5.68
    S1:Z5- Na-SiO2-1 95 337 0.11 3.21
    S1:1Z5-Na-SiO2-2 82 324 0.14 4.95
    S1:1Z5-NH3-SiO2-1 96 258 0.10 3.41
    S1:1Z5-NH3-SiO2-2 73 253 0.10 5.09
    S1:1Z5-TEOS-1 96 413 0.17 2.17
    S1:1Z5-TEOS-2 97 360 0.15 1.96
    下载: 导出CSV

    表  2  350 ℃下从Py-IR得到的ZSM-5和S1:1Z5@Silicalite-1分子筛的B酸和L酸量

    Table  2  Amounts of Brønsted and Lewis acids of ZSM-5 and S1:1Z5@Silicalite-1 zeolite from Py-IR at 350°C

    Catalyst L/(μmol·g−1) B+L/(μmol·g−1) B/(μmol·g−1) B/L Total/(μmol·g−1)
    ZSM-5 2.8 29.6 15.2 5.4 47.5
    S1:1Z5-Na-SiO2-1 1.2 25.1 5.7 4.75 32.0
    S1:1Z5-Na-SiO2-2 0.8 26.0 9.2 11.5 36.0
    S1:1Z5-TEOS-1 3.3 57.5 33.5 10.2 94.3
    S1:1Z5-TEOS-2 2.2 35.6 25.6 11.6 63.3
    S1:1Z5-NH3-SiO2-1 2.2 25.6 10.1 4.6 37.9
    S1:1Z5-NH3-SiO2-2 0.7 30.5 11.7 16.7 43.0
    S1:1Z5-SiO2-1 1.2 24.8 11.0 9.2 37.0
    S1:1Z5-SiO2-2 1.0 28.5 15.5 15.5 45.0
    下载: 导出CSV

    表  3  不同钝化层厚度ZSM@Silicalite-1分子筛的织构性质

    Table  3  Textural properties of ZSM@Silicalite-1 zeolites with different shell thicknesses

    Catalyst BET Surface Area S/(m2·g−1) Pore Volume v/(cm3·g−1) Pore Size d/(nm)
    ZSM-5 383 0.14 1.63
    1:1Z5- Na-SiO2 337 0.11 3.21
    1:2Z5- Na-SiO2 202 0.05 5.13
    1:3Z5- Na-SiO2 165 0.04 5.18
    1:3.5Z5- Na-SiO2 139 0.03 6.5
    1:4Z5- Na-SiO2 143 0.03 6.6
    下载: 导出CSV

    表  4  350 ℃下从Py-IR得到的不同钝化层厚度分子筛的B酸和L酸量

    Table  4  Amounts of Brønsted and Lewis acids of zeolite with different shell thicknesses from Py-IR at 350 ℃

    Catalyst L/(μmol·g−1) B+L/(μmol·g−1) B/(μmol·g−1) B/L Total/(μmol·g−1)
    ZSM-5 2.8 29.6 15.2 5.4 47.5
    1:1Z5-Na-SiO2 1.2 23.1 9.8 8.2 34.1
    1:2Z5-Na-SiO2 0.8 7.5 4.3 5.4 12.6
    1:3Z5-Na-SiO2 0.8 3.9 2.7 3.4 7.5
    1:3.5Z5-Na-SiO2 0.6 3.8 1.9 3.2 6.3
    1:4Z5-Na-SiO2 1.9 2.5 3.8 2 8.2
    下载: 导出CSV

    表  5  ZnZrOx的织构性质

    Table  5  Textural properties of ZnZrOx

    Catalyst BET Surface Area S/(m2·g−1) Pore Volume v/(cm3·g−1) Pore Size d/(nm)
    ZnZrOx 29 0.03 3
    下载: 导出CSV

    表  6  不同晶化条件催化剂上CO2加氢耦合甲苯烷基化反应气相产物分析

    Table  6  Gas-phase products analysis of CO2 hydrogenation and toluene alkylation over catalysts with different crystallization conditions

    CatalystConv.CO2/%C1-C5COSmethy
    ZZO/Z518.633.159.97.0
    ZZO/S1:1Z5-TEOS-115.517.975.46.7
    ZZO/S1:1Z5-Na-SiO2-111.329.459.910.7
    ZZO/S1:1Z5-NH3-SiO2-115.453.139.57.4
    ZZO/S1:1Z5-SiO2-110.126.761.711.6
    下载: 导出CSV

    表  7  不同晶化条件催化剂上CO2加氢耦合甲苯烷基化反应液相产物分析

    Table  7  Liquid phase product analysis of CO2 hydrogenation and toluene alkylation over catalysts with different crystallization conditions

    CatalystConv.
    T/%
    Selectivity/%PX/X
    PXMXOXOther
    ZZO/Z532.428.433.618.419.635.3
    ZZO/S1:1Z5-TEOS-136.327.133.918.220.834.2
    ZZO/S1:1Z5-TEOS-229.033.930.218.417.541.1
    ZZO/D1:1Z5-TEOS29.320.441.018.420.225.5
    ZZO/S1:1Z5-SiO2-126.534.724.213.827.347.7
    ZZO/S1:1Z5-SiO2-229.523.835.217.323.728.4
    ZZO/D1:1Z5-SiO229.118.834.712.733.817.4
    ZZO/S1:1Z5-NH3-SiO2-123.340.421.113.325.254.0
    ZZO/S1:1Z5-NH3-SiO2-225.530.532.515.121.939.0
    ZZO/D1:1Z5-NH3-SiO212.729.728.827.913.634.4
    ZZO/S1:1Z5-Na-SiO2-123.941.919.913.225.055.8
    ZZO/S1:1Z5-Na-SiO2-210.134.926.814.723.645.7
    ZZO/D1:1Z5-Na-SiO21.323.114.024.138.826.2
    下载: 导出CSV
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  • 收稿日期:  2024-01-22
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