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NiW/SAPO-11催化剂对煤焦油加氢尾油模型化合物二十烷加氢异构性能的影响

赵旭红 吴玉起 代正华 钟梅 靳立军 刘洋 亚力昆江·吐尔逊 李建 周玉生

赵旭红, 吴玉起, 代正华, 钟梅, 靳立军, 刘洋, 亚力昆江·吐尔逊, 李建, 周玉生. NiW/SAPO-11催化剂对煤焦油加氢尾油模型化合物二十烷加氢异构性能的影响[J]. 燃料化学学报(中英文), 2024, 52(3): 395-404. doi: 10.19906/j.cnki.JFCT.2023068
引用本文: 赵旭红, 吴玉起, 代正华, 钟梅, 靳立军, 刘洋, 亚力昆江·吐尔逊, 李建, 周玉生. NiW/SAPO-11催化剂对煤焦油加氢尾油模型化合物二十烷加氢异构性能的影响[J]. 燃料化学学报(中英文), 2024, 52(3): 395-404. doi: 10.19906/j.cnki.JFCT.2023068
ZHAO Xuhong, WU Yuqi, DAI Zhenghua, ZHONG Mei, JIN Lijun, LIU Yang, Yalkunjang Tursun, LI Jian, ZHOU Yusheng. Effect of NiW/SAPO-11 catalyst on hydroisomerization performance of model compound eicosane for tail oil hydrogenation of coal tar[J]. Journal of Fuel Chemistry and Technology, 2024, 52(3): 395-404. doi: 10.19906/j.cnki.JFCT.2023068
Citation: ZHAO Xuhong, WU Yuqi, DAI Zhenghua, ZHONG Mei, JIN Lijun, LIU Yang, Yalkunjang Tursun, LI Jian, ZHOU Yusheng. Effect of NiW/SAPO-11 catalyst on hydroisomerization performance of model compound eicosane for tail oil hydrogenation of coal tar[J]. Journal of Fuel Chemistry and Technology, 2024, 52(3): 395-404. doi: 10.19906/j.cnki.JFCT.2023068

NiW/SAPO-11催化剂对煤焦油加氢尾油模型化合物二十烷加氢异构性能的影响

doi: 10.19906/j.cnki.JFCT.2023068
基金项目: 新疆维吾尔自治区重大科技专项(2021A01002-3),国家自然科学基金(22169019,22279110)和“天池英才”引进计划资助
详细信息
    通讯作者:

    Tel: 13669931725, E-mail: zhongmei0504@126.com

    liu_yang0517@126.com

  • 中图分类号: TQ426

Effect of NiW/SAPO-11 catalyst on hydroisomerization performance of model compound eicosane for tail oil hydrogenation of coal tar

Funds: The project was supported by the Major Science and Technology Project of Xinjiang Uygur Autonomous Region (2021A01002-3), the National Natural Science Foundation of China (22169019, 22279110) and “Tianchi Talents” Introduction Plan.
  • 摘要: 以SAPO-11分子筛为载体,采用机械化学法制备Ni系催化剂,引入W调节其电子结构、晶粒尺寸与形态分布以及催化剂的孔结构、酸性与酸量等,基于对XRD、TEM、BET、NH3-TPD、吡啶吸附红外等结果的深入分析,探究催化剂NiW配比对催化剂性质和煤焦油加氢尾油模型化合物正二十烷(n-C20)加氢异构性能的影响规律。结果表明,Ni/SAPO-11负载W后,比表面积不同程度增加,W质量分数为0.5%时比表面积达到最大值149 m2/g;Ni的平均粒径减小,W质量分数为1%时降至最小值4.43 nm,比Ni/SAPO-11减小36%,且Ni0的含量和表面酸量均最高。此外,W促进了Ni的还原,使得还原峰温向低温方向移动。XPS分析表明,随着W含量的增加,Ni0的结合能降低,W5+的结合能升高。二十烷(n-C20)的加氢异构产物分布显示,3Ni1W/SAPO-11作用下n-C20的转化率和异二十烷(i-C20)的收率均最高,分别为88.23%和75.72%,且以单支链异二十烷(Mono-i-C20)为主,收率达71.65%。在线取样结果显示,n-C20在金属位点与酸功能的双重作用下先生成单支链异构体,随着反应的进行向多支链异构体转化,不稳定的多支链异构体会进一步裂解成小分子烷烃。
  • FIG. 3018.  FIG. 3018.

    FIG. 3018.  FIG. 3018.

    图  1  催化剂的XRD谱图(a)和局部放大图(b)

    Figure  1  XRD patterns (a) and local magnification (b) of catalyst

    图  2  催化剂的N2吸附-脱附曲线(a)和孔径分布(b)

    Figure  2  N2 adsorption-desorption curves (a) and pore size distributions (b) of catalysts

    图  3  催化剂的TEM(a1)−(e1)和HRTEM(a2)−(e2)图与Ni的粒径分布(a3)−(e3)

    Figure  3  The TEM (a1)−(e1) and HRTEM (a2)−(e2) images of catalysts and size distribution of Ni (a3)−(e3)

    图  4  3Ni1W/SAPO-11中Ni 2p (a)和W 4f (b)的分峰拟合图

    Figure  4  Peak fitting profiles of Ni 2p (a) and W 4f (b) in 3Ni1W/SAPO-11

    图  5  Ni和W组分的结合能(a)与形态分布(b)

    Figure  5  Binding energy (a) and morphology distribution (b) of Ni and W species

    图  6  催化剂的H2-TPR曲线

    Figure  6  H2-TPR profiles for different catalysts

    图  7  催化剂的NH3-TPD曲线(a)和Py-FTIR谱图(b)

    Figure  7  NH3-TPD profiles (a) and Py-FTIR spectra (b) of catalysts

    图  8  催化剂对n-C20加氢异构反应性能的影响

    Figure  8  Effect of catalyst on hydrogenation isomerization of n-C20

    图  9  n-C20加氢异构行为随时间的变化

    Figure  9  Hydro-isomerism behavior of n-C20 with varied reaction time

    图  10  n-C20在3Ni1W/SAPO-11上主要的加氢异构反应路径

    Figure  10  The main hydro-isomerization reaction pathway of n-C20 on 3Ni1W/SAPO-11

    表  1  催化剂的孔结构参数和相对结晶度

    Table  1  Pore structure parameters and relative crystallinity of catalysts

    SampleSBETa/(m2·g−1)Smicb/(m2·g−1)Sextc/(m2·g−1)d/nmv/(cm3·g−1)Cd/%
    SAPO-11184131536.520.30100
    4Ni/SAPO-1111158538.320.2384.93
    3.5Ni0.5W/SAPO-11149109403.490.1385.80
    3Ni1W/SAPO-1112375484.910.1588.39
    2.5Ni1.5W/SAPO-1111367465.170.1586.83
    4W/SAPO-1113477577.760.2689.28
    a: BET method; b: t-plot method; c: Sext was calculated by subtracting micropore area from BET area; d: The relative crystallinity derived from XRD analysis using the ratio of the sum of zeolite peaks to background with the parent SAPO-11 as reference.
    下载: 导出CSV

    表  2  催化剂的酸性分布

    Table  2  Acid site distribution of catalysts

    SampleWeak acidity/(mmol·g−1)Medium strong acidity/(mmol·g−1)Total/(mmol·g−1)
    SAPO-110.330.550.88
    4Ni/SAPO-110.190.380.57
    3.5Ni0.5W/SAPO-110.280.410.69
    3Ni1W/SAPO-110.300.450.75
    2.5Ni1.5W/SAPO-110.290.400.69
    4W/SAPO-110.250.360.61
    下载: 导出CSV

    表  3  催化剂的理化性质

    Table  3  Physicochemical properties of the catalysts

    SampleAcidity/(μmol·g−1)dNi/nmDNia/%CNib/(μmol·g−1)CNi/CB
    CBCL
    SAPO-1147.28139.03
    4Ni/SAPO-1114.0258.036.9613.9595.086.78
    3.5Ni0.5W/SAPO-1130.8935.235.7816.80100.173.24
    3Ni1W/SAPO-1135.3039.374.4321.92112.033.17
    2.5Ni1.5W/SAPO-1134.2542.434.8520.0293.362.72
    4W/SAPO-1141.34125.81
    a: Ni dispersion (dispersion (%)=97.1/dNi); b: Calculated from the metal content and metal dispersity of Ni.
    下载: 导出CSV

    表  4  不同催化剂在类似反应条件下的催化性能

    Table  4  The catalytic performance of different catalysts under similar reaction conditions

    CarrierMetalLoading/%ReactantTemperature
    /℃
    Pressure
    /MPa
    Conversion
    /%
    Yield
    /%
    Ref.
    SAPO-11NiGa6n-C16360296.7664.90[27]
    ZSM-22Pt0.5n-C163204>80.00>71.00[51]
    ZSM-48Ptn-C163204<87.9<80[49]
    SAPO-11NiW20n-C16340279.571.18[9]
    SAPO-11NiCu4.5n-C8340270.0066.50[21]
    SAPO-11NiW4n-C20320388.2375.72this work
    下载: 导出CSV
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出版历程
  • 收稿日期:  2023-07-24
  • 修回日期:  2023-08-26
  • 录用日期:  2023-08-28
  • 网络出版日期:  2023-09-18
  • 刊出日期:  2024-03-08

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