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不同方法合成钼基氧硫复合物催化剂及其合成气制乙醇性能研究

宇文晓萌 冯文爽 穆晓亮 赵璐 房克功

宇文晓萌, 冯文爽, 穆晓亮, 赵璐, 房克功. 不同方法合成钼基氧硫复合物催化剂及其合成气制乙醇性能研究[J]. 燃料化学学报(中英文). doi: 10.19906/j.cnki.JFCT.2024027
引用本文: 宇文晓萌, 冯文爽, 穆晓亮, 赵璐, 房克功. 不同方法合成钼基氧硫复合物催化剂及其合成气制乙醇性能研究[J]. 燃料化学学报(中英文). doi: 10.19906/j.cnki.JFCT.2024027
YUWEN Xiaomeng, FENG Wenshuang, MU Xiaoliang, ZHAO Lu, FANG Kegong. Study on different synthesis methods of molybdenum-based oxide and sulfide catalyst and its performance in syngas to ethanol[J]. Journal of Fuel Chemistry and Technology. doi: 10.19906/j.cnki.JFCT.2024027
Citation: YUWEN Xiaomeng, FENG Wenshuang, MU Xiaoliang, ZHAO Lu, FANG Kegong. Study on different synthesis methods of molybdenum-based oxide and sulfide catalyst and its performance in syngas to ethanol[J]. Journal of Fuel Chemistry and Technology. doi: 10.19906/j.cnki.JFCT.2024027

不同方法合成钼基氧硫复合物催化剂及其合成气制乙醇性能研究

doi: 10.19906/j.cnki.JFCT.2024027
基金项目: 国家重点研发计划(2023YFB4103201),国家自然科学基金(21978313),中国科学院山西煤炭化学研究所创新基金(SCJC–DT–2022–05),煤转化国家重点实验室自主研究课题项目(2020BWZ002),中国科学院青年创新促进会人才项目(2020181)资助
详细信息
    通讯作者:

    Tel: +86-0351-4041153, E-mail: zhaolu@sxicc.ac.cn

    kgfang@sxicc.ac.cn

  • 中图分类号: O643.3

Study on different synthesis methods of molybdenum-based oxide and sulfide catalyst and its performance in syngas to ethanol

Funds: The project was supported by the National Key Research and Development Program of China (2023YFB4103201), National Natural Science Foundation of China (21978313), the Innovation Foundation of ICC-CAS (SCJC-DT-2022-05), the Autonomous Research Project of SKLCC (2020BWZ002) and the Youth Innovation Promotion Association of CAS (2020181).
  • 摘要: 合成气一步制乙醇是利用非石油资源生产乙醇的重要方法,如何提高乙醇选择性、创制高效催化剂是改善过程经济性的重点。本研究从硫化钼前体出发,分别采用传统热法和射频低温等离子体法制备钼基氧硫复合物催化剂并考察其催化合成气制乙醇反应性能。利用XRD、UV-Visible、HR-TEM、SEM、HAADF-STEM、XPS、CO-TPD、H2-TPD、CO2-TPD和In-situ DRIFTS等表征手段探究不同制备方法下合成的钼基氧硫复合物催化剂的不同物化性质,进而探究特征差异引发的催化反应性能变化。其中,MOS-P催化剂表现出最佳性能,在6 MPa、320 ℃、空速4500 h−1的反应条件下,CO转化率达到22.5%,总醇选择性可达71.4%,其中总醇中乙醇占比为29.1%。有关研究将为合成气定向转化提供理论指导并为新型钼基材料的设计与制备提供借鉴。
  • 图  1  射频低温等离子体装置示意图

    Figure  1  Schematic diagram of radio frequency non-thermal plasma device

    图  2  合成气制乙醇反应流程示意图

    Figure  2  Schematic diagram of reaction device for alcohols synthesis from syngas

    1: Reagent gas; 2: Pre-system pressure setter; 3: Mass flowmeter; 4: Temperature controller; 5: Heating furnace;6: Reactor; 7: Catalytic bed; 8: Heat trap; 9: Cold trap;10: Post-system pressure setter; 11: Gas chromatography;12: Gas outlet

    图  3  不同方法合成的Mo基氧硫复合物催化剂的XRD谱图(a)和UV-visible谱图(b)

    Figure  3  XRD patterns (a) and UV-Visible profiles (b) of the different MOS catalysts synthesized by different methods

    图  4  不同催化剂中MoS2与MoO3的相对含量

    Figure  4  The relative content of MoS2 and MoO3 in different catalysts

    图  5  (a)MS催化剂的SEM图像;(b)MS催化剂的HR-TEM图像;(c)MOS-T催化剂的SEM图像;(d)MOS-T催化剂的HR-TEM图像;(e)MOS-P催化剂的SEM图像;(f)MOS-P催化剂的HR-TEM图像;(g)MO催化剂的SEM图像;(h)MO催化剂的HR-TEM图像;(i)-(n)各催化剂中MoS2和MoO3的平均粒径

    Figure  5  (a) SEM image of the MS catalyst; (b) HR-TEM image of the MS catalyst; (c) SEM image of the MOS-T catalyst; (d) HR-TEM image of the MOS-T catalyst; (e) SEM image of the MOS-P catalyst; (f) HR-TEM image of the MOS-P catalyst; (g) SEM image of the MO catalyst; (h) HR-TEM image of the MO catalyst; (i)-(n) Particle size of MoS2 and MoO3 in each catalyst

    图  6  (a)-(b)MOS-P催化剂的TEM图像;(c)MOS-P催化剂的HAADF-STEM图像

    Figure  6  (a)-(b) TEM images of the MOS-P catalyst; (c) HAADF-STEM images of the MOS-P catalyst

    图  7  不同催化剂的XPS光谱

    Figure  7  XPS spectra of different catalysts

    (a): Full spectrum scanning results; (b): Mo element; (c): O element; (d): S element.

    图  8  不同催化剂的CO-TPD谱图

    Figure  8  CO-TPD profiles of the different catalysts

    图  9  不同催化剂的H2-TPD谱图

    Figure  9  H2-TPD profiles of the different catalysts

    图  10  不同催化剂的CO2-TPD谱图

    Figure  10  CO2-TPD profiles of the different catalysts

    图  11  MOS-T催化剂与MOS-P催化剂的In-situ DRIFTS谱图

    Figure  11  In-situ DRIFTS over the MOS-T catalyst and MOS-P catalyst

    (a): 1000−2300 cm−1; (b): 2300−3800 cm−1.

    表  1  不同催化剂的CO、H2和CO2吸附量

    Table  1  Amount of CO, H2 and CO2 on different catalysts

    CatalystAmount of CO/μmol g−1Amount of H2/μmol g−1Amount of CO2/μmol g−1
    Peak IPeak IITotal
    MS392828376
    MOS-T47116(60%)78(40%)194352
    MOS-P8090(45%)111(55%)201294
    MO211010
    下载: 导出CSV

    表  2  不同催化剂的合成气制乙醇催化反应性能a

    Table  2  The catalytic performance of different catalysts for the synthesis of ethanol from syngas a

    Catalyst
    CO conversion
    /%
    STYEtOH
    /(mg·mL−1·h−1)
    Product selectivity w/% b Alcohol distribution w/% Hydrocarbon distribution w/%
    ROHc CHnd MeOH EtOH C3+OHe C1 C2 C3+
    MS 14.1 13.5 68.8 31.2 66.5 22.5 11.0 57.2 26.1 16.7
    MOS-T 18.9 18.9 69.6 30.4 64.3 23.6 12.1 55.3 27.7 17.0
    MOS-P 22.5 32.0 71.4 28.6 55.2 29.1 15.7 62.5 23.1 14.4
    MO 12.3 14.2 55.9 44.1 53.6 28.3 18.1 61.2 24.2 14.6
    a: Reactions were carried out at 320 ℃, 6.0 MPa, GHSV=4500 h−1, H2/CO =2. STY is space-time yield; b: CO2 free; c: ROH means total alcohols and d: CHn means total hydrocarbons; e: Alcohols with carbon number above 3 were obtained in the product (propanol, butanol and pentanol).
    下载: 导出CSV

    表  3  本研究与文献中合成乙醇Mo基催化剂的催化性能对比

    Table  3  A comparison of the catalytic performance of Mo-based catalysts for ethanol synthesis between this study and the literature

    Catalyst A[22]
    Rh-K-MoP/SiO2
    B[25]
    MoO2-Pla
    C[52]
    β-Mo2C
    D[53]
    K/β-Mo2C/GMC
    E[54]
    Mo-K/MWCNT
    This work
    MOS-P
    CO conversion/% 18.0 16.3 58.6 1.3 19 22.5
    EtOH/ROH/% 27.7 38.0 18 34.6 28 29.1
    STYEtOH/(mg·mL−1·h−1) 22.8 21.6 2.2 11.5 30.8 32.0
    下载: 导出CSV
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  • 收稿日期:  2024-04-09
  • 修回日期:  2024-04-26
  • 录用日期:  2024-04-26
  • 网络出版日期:  2024-06-04

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