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铁基费托催化剂预处理过程的原位表征技术研究进展

韩宇静 王会香 王连成 黄冬梅 王鹏飞 吕宝亮

韩宇静, 王会香, 王连成, 黄冬梅, 王鹏飞, 吕宝亮. 铁基费托催化剂预处理过程的原位表征技术研究进展[J]. 燃料化学学报(中英文), 2023, 51(4): 458-472. doi: 10.19906/j.cnki.JFCT.2022067
引用本文: 韩宇静, 王会香, 王连成, 黄冬梅, 王鹏飞, 吕宝亮. 铁基费托催化剂预处理过程的原位表征技术研究进展[J]. 燃料化学学报(中英文), 2023, 51(4): 458-472. doi: 10.19906/j.cnki.JFCT.2022067
HAN Yu-jing, WANG Hui-xiang, WANG Lian-cheng, HUANG Dong-mei, WANG Peng-fei, LÜ Bao-liang. Research progress on the in-situ characterizations of iron-based FTS catalysts pretreatment process[J]. Journal of Fuel Chemistry and Technology, 2023, 51(4): 458-472. doi: 10.19906/j.cnki.JFCT.2022067
Citation: HAN Yu-jing, WANG Hui-xiang, WANG Lian-cheng, HUANG Dong-mei, WANG Peng-fei, LÜ Bao-liang. Research progress on the in-situ characterizations of iron-based FTS catalysts pretreatment process[J]. Journal of Fuel Chemistry and Technology, 2023, 51(4): 458-472. doi: 10.19906/j.cnki.JFCT.2022067

铁基费托催化剂预处理过程的原位表征技术研究进展

doi: 10.19906/j.cnki.JFCT.2022067
基金项目: 国家自然科学基金(21972158),中国科学院联合基金(2021017),山西省留学基金委科研项目(2020-196),山西省青年科学基金(201901D211583)和山西省博士创业基金(SQ2019006)资助
详细信息
    通讯作者:

    E-mail: wangpf@sxicc.ac.cn

    lbl604@sxicc.ac.cn

  • 中图分类号: O643.36

Research progress on the in-situ characterizations of iron-based FTS catalysts pretreatment process

Funds: The project was supported by the National Natural Science Foundation of China (21972158), Joint Fund of the Yulin University and the Dalian National Laboratory for Clean Energy (2021017), Research Project of Shanxi Scholarship Council of China (2020-196), Shanxi Province Science Foundation for Youths (201901D211583) and Doctoral Start-up Foundation of Shanxi Province (SQ2019006).
  • 摘要:

    铁基费托合成(FTS)催化剂通常以氧化物前驱体α-Fe2O3的形式存在,在不同预处理条件下转变为铁碳化合物FexCy后具有不同的催化活性,因此,研究催化剂预处理过程对费托合成反应具有重要意义。然而该过程中物相体系高度动态复杂,通过常规表征手段无法捕捉到铁基催化剂准确的变化信息。为了深入探究前驱体α-Fe2O3体系在不同预处理过程中的真实变化,需要借助多种原位表征技术获取催化剂物相、形貌及其表面结构和性质的动态变化数据,从而可实现催化剂预处理过程和后续FTS催化性能的有效关联。本工作系统综述了X射线衍射、透射电子显微镜、X射线光电子能谱、红外光谱和拉曼光谱等原位表征技术在铁基FTS催化剂预处理过程中的实验方法以及数据处理方法,以明晰催化剂前驱体复杂的结构性质变化过程,进而促进更高效铁基FTS催化剂的设计和开发。

  • FIG. 2205.  FIG. 2205.

    FIG. 2205.  FIG. 2205.

    图  1  (a)先H2后合成气,(b)CO,(c)合成气气氛下Rietveld精修的铁基催化剂物相相对丰度;在(d)2% CO/He和(e)2% CO/ 8% H2/He气氛下,Rietveld精修的Fe3O4平均晶粒尺寸[33, 35]

    Figure  1  Rietveld refinement of relative abundance of iron oxide in (a) syngas after H2, (b) CO and (c) syngas; Rietveld refinement of average crystal size of Fe3O4 in (d) 2% CO/He and (e) 2% CO/ 8% H2/He [33, 35](with permission from Elsevier and Wiley)

    图  2  α-Fe2O3催化剂的in-situ XRD谱图:(a)高μC条件下预处理及其(b)随后的FTS过程;(d)低μC条件下预处理和及其(e)随后的FTS过程中;(c)高μC催化剂和(f)低μC催化剂在FTS条件下k1傅里叶变换Fe K边原位EXAFS数据[39]

    Figure  2  In-situ XRD patterns of the α-Fe2O3 catalyst evolution during (a) pretreatment in high µC and (b) subsequent FTS condition; (d) pretreatment in low µC and (e) subsequent FTS condition; phase corrected, k1 weighted Fourier-transformed Fe K-edge EXAFS data of the α-Fe2O3 catalyst samples during FTS, (c) high µC catalyst and (f) low µC catalyst [39] (with permission from ACS Publications)

    图  3  (a)常温,(b)400 ℃,(c)700 ℃时Fe/BN的TEM照片和FePt尺寸分布(插图);(d)保持900 ℃15 min后的HRTEM照片;((e)–(g))FePt被h-BN纳米片包裹的HRTEM图像[44]

    Figure  3  TEM images and FePt size distribution (inset) of Fe/BN at (a) RT, (b) 400 ℃, (c) 700 ℃; (d) HRTEM image of FP/BN at 900 ℃ after exposure for 15 min; ((e)–(g)) HRTEM images of FePt nanoparticles enveloped by h-BN nanosheets [44](with permission from Elsevier)

    图  4  (a)α-Fe2O3转变为γ-Fe2O3in-situ HRTEM照片,((b),(c))分别是(a)中红色方框区域b和c的衍射图,((d),(e))b和c区域的EELS光谱,(f)ZnFe2O4@Co3O4在纯H2还原过程中获得的STEM-HAADF图像,插图为EELS光谱图像获得的复合元素图(Co:绿色;Zn-Fe:橙色)[30, 46]

    Figure  4  (a) In-situ HRTEM of the transformation from α-Fe2O3 to γ-Fe2O3, ((b), (c)) The diffractograms from red boxed regions b and c, in (a), respectively, ((d), (e)) EELS spectra from the regions of red boxes b and c in (a), (f) STEM-HAADF images of ZnFe2O4@Co3O4 obtained during the in-situ TEM reduction in pure H2, with inset showing the composite elemental map obtained from the EELS spectrum image (Co: green; Zn-Fe :orange)[30, 46] (with permission from Elsevier and ACS Publications)

    图  5  (a)纳米α-Fe2O3和(b)块状α-Fe2O3在氢气中处理过程中的Fe 2p3/2 XPS谱图,箭头表示纳米颗粒样品中的等吸光点;不同气氛下FeCeNa催化剂的((c), (d))O 1s和((e), (f))Ce 3d in-situ XPS光谱谱图[32, 53]

    Figure  5  (a) Fe 2p3/2 XPS spectra during treatment of (a) the nanoparticles and (b) bulk iron oxide in H2, the arrow indicates the isosbestic point in the nanoparticulate sample; in-situ XPS spectra of ((c), (d)) O 1s and ((e), (f)) Ce 3d of FeCeNa catalysts in different atmospheres[32, 53](with permission from Elsevier and Wiley)

    图  6  (a)(s1)Al2O3/α-Fe2O3 = 1,(s2)SiO2/α-Fe2O3 = 1,(s3)α-Fe2O3活化后催化剂的in-situ CO-DRIFTS光谱谱图;(b)SiO2负载的铁基催化剂的in-situ DRIFTS光谱谱图[18, 64]

    Figure  6  (a) in-situ CO-DRIFTS spectra of (s1) Al2O3/α-Fe2O3 = 1, (s2) SiO2/α-Fe2O3 = 1, (s3) α-Fe2O3; (B) in-situ DRIFTS spectra of SiO2-supported iron based catalyst[18, 64] (with permission from Elsevier and Springer)

    图  7  (a)Fe2O3-C(b)Fe2O3-H(c)Fe2O3-R在350 ℃、10% CO气氛中记录的in-situ Raman光谱谱图[70]

    Figure  7  In-situ Raman spectra of (a) Fe2O3-C, (b) Fe2O3-H, (c)Fe2O3-R at 350 ℃ in 10% CO[70] (with permission from Elsevier)

    图  8  (a)35FeK/m-ZrO2和(b)35FeK/t-ZrO2催化剂的in-situ Raman谱图,实验条件:1 atm、30 mL/min、10% CO/Ar和10 ℃/min的加热速率;(c)350 ℃下CO预处理300 min后35Fe K/m-ZrO2和35FeK/t-ZrO2催化剂的拉曼光谱谱图[72]

    Figure  8  In-situ Raman spectra of (a) 35FeK/m-ZrO2 and (b) 35FeK/t-ZrO2, measurement conditions: 1 atm, 30 mL/min, 10% CO/Ar, and the heating rate of 10 ℃/min, (c) Raman spectra of 35FeK/m-ZrO2 and 35FeK/t-ZrO2 catalysts after the CO prereduction at 350 ℃ for 300 min[72] (with permission from ACS Publications)

    表  1  铁基催化剂的in-situ XPS、FT-IR和Raman表征技术的常用参数

    Table  1  Common parameters of in-situ XPS, FT-IR and Raman characterization techniques for iron-based catalysts

    PhaseXPS[18, 19]/
    eV
    OriginFT-IR[20-22]/
    cm−1
    OriginRaman[23, 24]/
    cm−1
    α-Fe2O3711.0
    529.8
    Fe 2p3/2
    O 1s
    650, 575,
    525, 485,
    440, 400,
    385, 360,
    300
    Fe–O613, 500,
    412, 299,
    247, 225,
    1320
    Fe3O4709.0
    530.2
    Fe 2p3/2
    O 1s
    580
    400
    Fe–O676
    550
    FeO709.0
    530.2
    Fe 2p3/2
    O 1s
    490
    425
    Fe–O210, 390
    480, 652
    α-Fe706.8
    720.3
    Fe 2p3/2
    Fe 2p1/2
    2040−
    1980
    CO
    surface adsorption
    χ-Fe5C2707.0
    719.9
    Fe 2p3/2
    Fe 2p1/2
    2015
    D band:
    1380
    G band:
    1580
    θ-Fe3C707.9
    720.6
    Fe 2p3/2
    Fe 2p1/2
    2030
    下载: 导出CSV
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  • 收稿日期:  2022-07-08
  • 修回日期:  2022-07-28
  • 录用日期:  2022-07-29
  • 网络出版日期:  2022-08-11
  • 刊出日期:  2023-04-15

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