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Synthesis and Characterization of MgO-Doped / Acid Modified Metakaolin Supported Ni-Based Catalysts

Received: 21 October 2021    Accepted: 15 November 2021    Published: 13 July 2022
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Abstract

Catalytic steam reforming of bioethanol is an endothermic reaction for hydrogen production with high tendency of complete conversion at high temperature, but the catalyst is susceptible to deactivation due to the sintering of based metal and carbon deposition. MgO-doped/acid modified metakaolin supported nickel-based catalysts (with 5-25wt% nickel loading) were synthesized using wetness impregnation method and characterized. The physicochemical properties of the catalysts were examined using XRD, BET, SEM-EDX, XRF, FTIR and TG/DTA techniques. XRD patterns show the presence of nickel oxide, spinel MgAl2O4, NiAl2O4 in all the calcined catalyst samples, via characteristic peaks. Most of the crystallite sizes of the NiO particles in the synthesized catalysts were within 20.1-38nm, far less than the size effect threshold of 100nm, except CAT II, with crystallite size of 132.5nm, which could be attributed to the high tendency of NiO particles to agglomerate with MgO. Based on BET results, all the synthesized catalysts have pore diameter in the mesopore diameter range. SEM-EDX results show that there is nuclear interaction among MgO, NiO and Al2O3, as confirmed by XRD and XRF analyses. The FTIR analyses show that nickel phyllosilicate bond, Si-O-Al stretching vibration, OH stretching and metal-oxygen bond exist within the synthesized catalysts. The formation of MgAl2O4 and NiAl2O4 spinel phases is due to the interaction of active oxide components with acid modified metakaolin and MgO, which contributes to the catalyst thermal stability, as confirmed by TG/DTA analyses. These spinel structures would contribute to the catalysts’ activity and selectivity, as their structures could remain unchanged under severe reaction conditions. The mesoporous structure of the synthesized catalysts would aid the reactant gases to adsorb on its surface and easy diffusion through the catalyst’s channel after reaction. With better interaction among the support, promoter and based metal in the synthesized catalysts and available surface OH group, the formation and conversion of adsorbed formate intermediate during steam reforming reactions would be facilitated, and in turn reduce carbon deposition.

Published in Journal of Energy, Environmental & Chemical Engineering (Volume 7, Issue 3)
DOI 10.11648/j.jeece.20220703.12
Page(s) 54-65
Creative Commons

This is an Open Access article, distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium or format, provided the original work is properly cited.

Copyright

Copyright © The Author(s), 2024. Published by Science Publishing Group

Keywords

Synthesis, Catalyst, Impregnation, Physicochemical, Reforming, Carbon Deposition

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    Abdullahi Nwaha Isah, Elizabeth Jumoke Eterigho, Moses Aderemi Olutoye, Mohammed Umar Garba. (2022). Synthesis and Characterization of MgO-Doped / Acid Modified Metakaolin Supported Ni-Based Catalysts. Journal of Energy, Environmental & Chemical Engineering, 7(3), 54-65. https://doi.org/10.11648/j.jeece.20220703.12

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    Abdullahi Nwaha Isah; Elizabeth Jumoke Eterigho; Moses Aderemi Olutoye; Mohammed Umar Garba. Synthesis and Characterization of MgO-Doped / Acid Modified Metakaolin Supported Ni-Based Catalysts. J. Energy Environ. Chem. Eng. 2022, 7(3), 54-65. doi: 10.11648/j.jeece.20220703.12

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    Abdullahi Nwaha Isah, Elizabeth Jumoke Eterigho, Moses Aderemi Olutoye, Mohammed Umar Garba. Synthesis and Characterization of MgO-Doped / Acid Modified Metakaolin Supported Ni-Based Catalysts. J Energy Environ Chem Eng. 2022;7(3):54-65. doi: 10.11648/j.jeece.20220703.12

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  • @article{10.11648/j.jeece.20220703.12,
      author = {Abdullahi Nwaha Isah and Elizabeth Jumoke Eterigho and Moses Aderemi Olutoye and Mohammed Umar Garba},
      title = {Synthesis and Characterization of MgO-Doped / Acid Modified Metakaolin Supported Ni-Based Catalysts},
      journal = {Journal of Energy, Environmental & Chemical Engineering},
      volume = {7},
      number = {3},
      pages = {54-65},
      doi = {10.11648/j.jeece.20220703.12},
      url = {https://doi.org/10.11648/j.jeece.20220703.12},
      eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.jeece.20220703.12},
      abstract = {Catalytic steam reforming of bioethanol is an endothermic reaction for hydrogen production with high tendency of complete conversion at high temperature, but the catalyst is susceptible to deactivation due to the sintering of based metal and carbon deposition. MgO-doped/acid modified metakaolin supported nickel-based catalysts (with 5-25wt% nickel loading) were synthesized using wetness impregnation method and characterized. The physicochemical properties of the catalysts were examined using XRD, BET, SEM-EDX, XRF, FTIR and TG/DTA techniques. XRD patterns show the presence of nickel oxide, spinel MgAl2O4, NiAl2O4 in all the calcined catalyst samples, via characteristic peaks. Most of the crystallite sizes of the NiO particles in the synthesized catalysts were within 20.1-38nm, far less than the size effect threshold of 100nm, except CAT II, with crystallite size of 132.5nm, which could be attributed to the high tendency of NiO particles to agglomerate with MgO. Based on BET results, all the synthesized catalysts have pore diameter in the mesopore diameter range. SEM-EDX results show that there is nuclear interaction among MgO, NiO and Al2O3, as confirmed by XRD and XRF analyses. The FTIR analyses show that nickel phyllosilicate bond, Si-O-Al stretching vibration, OH stretching and metal-oxygen bond exist within the synthesized catalysts. The formation of MgAl2O4 and NiAl2O4 spinel phases is due to the interaction of active oxide components with acid modified metakaolin and MgO, which contributes to the catalyst thermal stability, as confirmed by TG/DTA analyses. These spinel structures would contribute to the catalysts’ activity and selectivity, as their structures could remain unchanged under severe reaction conditions. The mesoporous structure of the synthesized catalysts would aid the reactant gases to adsorb on its surface and easy diffusion through the catalyst’s channel after reaction. With better interaction among the support, promoter and based metal in the synthesized catalysts and available surface OH group, the formation and conversion of adsorbed formate intermediate during steam reforming reactions would be facilitated, and in turn reduce carbon deposition.},
     year = {2022}
    }
    

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  • TY  - JOUR
    T1  - Synthesis and Characterization of MgO-Doped / Acid Modified Metakaolin Supported Ni-Based Catalysts
    AU  - Abdullahi Nwaha Isah
    AU  - Elizabeth Jumoke Eterigho
    AU  - Moses Aderemi Olutoye
    AU  - Mohammed Umar Garba
    Y1  - 2022/07/13
    PY  - 2022
    N1  - https://doi.org/10.11648/j.jeece.20220703.12
    DO  - 10.11648/j.jeece.20220703.12
    T2  - Journal of Energy, Environmental & Chemical Engineering
    JF  - Journal of Energy, Environmental & Chemical Engineering
    JO  - Journal of Energy, Environmental & Chemical Engineering
    SP  - 54
    EP  - 65
    PB  - Science Publishing Group
    SN  - 2637-434X
    UR  - https://doi.org/10.11648/j.jeece.20220703.12
    AB  - Catalytic steam reforming of bioethanol is an endothermic reaction for hydrogen production with high tendency of complete conversion at high temperature, but the catalyst is susceptible to deactivation due to the sintering of based metal and carbon deposition. MgO-doped/acid modified metakaolin supported nickel-based catalysts (with 5-25wt% nickel loading) were synthesized using wetness impregnation method and characterized. The physicochemical properties of the catalysts were examined using XRD, BET, SEM-EDX, XRF, FTIR and TG/DTA techniques. XRD patterns show the presence of nickel oxide, spinel MgAl2O4, NiAl2O4 in all the calcined catalyst samples, via characteristic peaks. Most of the crystallite sizes of the NiO particles in the synthesized catalysts were within 20.1-38nm, far less than the size effect threshold of 100nm, except CAT II, with crystallite size of 132.5nm, which could be attributed to the high tendency of NiO particles to agglomerate with MgO. Based on BET results, all the synthesized catalysts have pore diameter in the mesopore diameter range. SEM-EDX results show that there is nuclear interaction among MgO, NiO and Al2O3, as confirmed by XRD and XRF analyses. The FTIR analyses show that nickel phyllosilicate bond, Si-O-Al stretching vibration, OH stretching and metal-oxygen bond exist within the synthesized catalysts. The formation of MgAl2O4 and NiAl2O4 spinel phases is due to the interaction of active oxide components with acid modified metakaolin and MgO, which contributes to the catalyst thermal stability, as confirmed by TG/DTA analyses. These spinel structures would contribute to the catalysts’ activity and selectivity, as their structures could remain unchanged under severe reaction conditions. The mesoporous structure of the synthesized catalysts would aid the reactant gases to adsorb on its surface and easy diffusion through the catalyst’s channel after reaction. With better interaction among the support, promoter and based metal in the synthesized catalysts and available surface OH group, the formation and conversion of adsorbed formate intermediate during steam reforming reactions would be facilitated, and in turn reduce carbon deposition.
    VL  - 7
    IS  - 3
    ER  - 

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Author Information
  • Department of Chemical Engineering Technology, School of Engineering Technology, Federal Polytechnic Nasarawa, Nasarawa, Nigeria

  • Department of Chemical Engineering, School of Infrastructure, Process Engineering and Technology, Federal University of Technology, Minna, Nigeria

  • Department of Chemical Engineering, School of Infrastructure, Process Engineering and Technology, Federal University of Technology, Minna, Nigeria

  • Department of Chemical Engineering, School of Infrastructure, Process Engineering and Technology, Federal University of Technology, Minna, Nigeria

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