HYDROTHERMAL SYNTHESIS AND CHARACTERIZATION OF ZSM-5 ZEOLITE FROM ANORTHOSITE: IMPACTS OF REACTION TIME AND TEMPERATURE
Keywords:
anorthosite, zeolite, hydrothermal synthesis, ZSM-5
Abstract
Anorthosite was used as the alumina source while applying a hydrothermal method for the synthesis of ZSM-5. The anorthosite sample, obtained from the Soji-Bikilal region of Ethiopia, was pre-treated and activated with NaOH at a 1:2 (wt/wt) ratio. ZSM-5 type zeolites were made from the anorthosite rock utilising hydrothermal synthesis at reaction times of (24, 48, and 96) h at a reaction temperature of 100 °C, in accordance with the alkaline fusion technique. UV-vis spectra, X-ray diffraction, scanning electron microscopy and BET surface area were used to characterize anorthosite and synthesized ZSM-5 zeolite. The highest noticeable reflection peak for the ZSM-5 zeolite synthesised at the reaction temperature of 100 °C and reaction time of 96 h was at 24.7°, showing that the material was extremely crystalline. According to their microstructures, anorthosite features platy crystals and amorphous particles, while ZSM-5 zeolite exhibits spherical crystals with some amorphous gel.
References
1. Wang, S., et al., Tuning the siting of aluminum in ZSM-11 zeolite and regulating its catalytic performance in the conversion of methanol to olefins. Journal of Catalysis, 2019. 377: p. 81-97.
2. Rujiwatra, A., A selective preparation of phillipsite and sodalite from perlite. Materials Letters, 2004. 58(14): p. 2012-2015.
3. Boronat, M. and A. Corma, What is measured when measuring acidity in zeolites with probe molecules? ACS catalysis, 2019. 9(2): p. 1539-1548.
4. Kim, D.J. and H.S. Chung, Synthesis and characterization of ZSM-5 zeolite from serpentine. Applied Clay Science, 2003. 24(1-2): p. 69-77.
5. Serrano, D., et al., Molecular and meso-and macroscopic properties of hierarchical nanocrystalline ZSM-5 zeolite prepared by seed silanization. Chemistry of Materials, 2009. 21(4): p. 641-654.
6. Cheng, Y.T., et al., Production of p‐xylene from biomass by catalytic fast pyrolysis using ZSM‐5 catalysts with reduced pore openings. Angewandte Chemie, 2012. 124(44): p. 11259-11262.
7. Chawla, A., et al., Cooperative effects of inorganic and organic structure-directing agents in ZSM-5 crystallization. Molecular Systems Design & Engineering, 2018. 3(1): p. 159-170.
8. Corma, A., State of the art and future challenges of zeolites as catalysts. Journal of Catalysis, 2003. 216(1-2): p. 298-312.
9. Khaleque, A., et al., Zeolite synthesis from low-cost materials and environmental applications: A review. Environmental Advances, 2020. 2: p. 100019.
10. Sanhueza, V., et al., Synthesis of ZSM‐5 from diatomite: a case of zeolite synthesis from a natural material. Journal of Chemical Technology & Biotechnology: International Research in Process, Environmental & Clean Technology, 2004. 79(7): p. 686-690.
11. Coker, E.N., et al., Zeolite ZSM-5 synthesized in space: catalysts with reduced external surface activity. Microporous and mesoporous materials, 2001. 46(2-3): p. 223-236.
12. Garcıa-Martınez, J., et al., Synthesis and characterisation of MFI-type zeolites supported on carbon materials. Microporous and mesoporous materials, 2001. 42(2-3): p. 255-268.
13. Zhang, H., et al., Nano-crystallite oriented self-assembled ZSM-5 zeolite and its LDPE cracking properties: Effects of accessibility and strength of acid sites. Journal of Catalysis, 2013. 302: p. 115-125.
14. Ding, J., et al., Catalytic properties of a hierarchical zeolite synthesized from a natural aluminosilicate mineral without the use of a secondary mesoscale template. ChemCatChem, 2013. 5(8): p. 2258-2269.
15. Xue, Z., et al., Hierarchical structure and catalytic properties of a microspherical zeolite with intracrystalline mesopores. Acta materialia, 2012. 60(16): p. 5712-5722.
16. Moliner, M., C. Martínez, and A. Corma, Multipore zeolites: synthesis and catalytic applications. Angewandte Chemie International Edition, 2015. 54(12): p. 3560-3579.
17. Firoozi, M., M. Baghalha, and M. Asadi, The effect of micro and nano particle sizes of H-ZSM-5 on the selectivity of MTP reaction. Catalysis Communications, 2009. 10(12): p. 1582-1585.
18. Choi, M., et al., Stable single-unit-cell nanosheets of zeolite MFI as active and long-lived catalysts. Nature, 2009. 461(7261): p. 246-249.
19. Rownaghi, A.A. and J. Hedlund, Methanol to gasoline-range hydrocarbons: influence of nanocrystal size and mesoporosity on catalytic performance and product distribution of ZSM-5. Industrial & Engineering Chemistry Research, 2011. 50(21): p. 11872-11878.
20. Konno, H., et al., Effectiveness of nano-scale ZSM-5 zeolite and its deactivation mechanism on catalytic cracking of representative hydrocarbons of naphtha. Microporous and mesoporous materials, 2013. 175: p. 25-33.
21. Wdowin, M., et al., The conversion technology of fly ash into zeolites. Clean Technologies and Environmental Policy, 2014. 16: p. 1217-1223.
22. Park, M., et al., Molten-salt method for the synthesis of zeolitic materials: I. Zeolite formation in alkaline molten-salt system. Microporous and Mesoporous Materials, 2000. 37(1-2): p. 81-89.
23. Mondragon, F., et al., New perspectives for coal ash utilization: synthesis of zeolitic materials. Fuel, 1990. 69(2): p. 263-266.
24. Ojha, K., N.C. Pradhan, and A.N. Samanta, Zeolite from fly ash: synthesis and characterization. Bulletin of Materials Science, 2004. 27: p. 555-564.
25. Hong, J.L.X., et al., Conversion of coal fly ash into zeolite materials: synthesis and characterizations, process design, and its cost-benefit analysis. Industrial & Engineering Chemistry Research, 2017. 56(40): p. 11565-11574.
26. Wang, P., B. Shen, and J. Gao, Synthesis of ZSM-5 zeolite from expanded perlite and its catalytic performance in FCC gasoline aromatization. Catalysis Today, 2007. 125(3-4): p. 155-162.
27. de la Villa Mencia, R.V., et al., Synthesis of zeolite type analcime from industrial wastes. Microporous and Mesoporous Materials, 2020. 293: p. 109817.
28. Knudsen, C., J. Wanvik, and H. Svahnberg, Anorthosites in Greenland: a possible raw material for aluminium? GEUS Bulletin, 2012. 26: p. 53-56.
29. Osmanlioglu, A.E., Immobilization of radioactive waste by cementation with purified kaolin clay. Waste Management, 2002. 22(5): p. 481-483.
30. Arai, T. and S. Maruyama, Formation of anorthosite on the Moon through magma ocean fractional crystallization. Geoscience Frontiers, 2017. 8(2): p. 299-308.
31. Ashwal, L.D. and G.M. Bybee, Crustal evolution and the temporality of anorthosites. Earth-Science Reviews, 2017. 173: p. 307-330.
32. Hodge, J., Fractures, Fluids, and Metamorphism: Shear Zone Initiation in the Marcy Anorthosite Massif, Adirondacks, New York, USA. 2019, The University of Maine.
33. Woldemichael, B.W. and J.-I. Kimura, Petrogenesis of the Neoproterozoic Bikilal-Ghimbi gabbro, Western Ethiopia. Journal of mineralogical and petrological sciences, 2008. 103(1): p. 23-46.
34. He, Y., et al., Research progress on green synthesis of various high-purity zeolites from natural material-kaolin. Journal of Cleaner Production, 2021. 306: p. 127248.
35. Król, M., Natural vs. Synthetic zeolites. Crystals, 2020. 10(7): p. 622.
36. Blasco, T., A. Corma, and J. Martínez-Triguero, Hydrothermal stabilization of ZSM-5 catalytic-cracking additives by phosphorus addition. Journal of catalysis, 2006. 237(2): p. 267-277.
37. Xue, N., et al., Synergistic effects of tungsten and phosphorus on catalytic cracking of butene to propene over HZSM-5. Applied Catalysis A: General, 2009. 352(1-2): p. 87-94.
38. Mgbemere, H., et al., Synthesis of zeolite-a using kaolin samples from Darazo, Bauchi state and Ajebo, Ogun state in Nigeria. Nigerian Journal of Technology, 2018. 37(1): p. 87-95.
39. Ríos, C.A., C.D. Williams, and O.M. Castellanos, Crystallization of low silica Na-A and Na-X zeolites from transformation of kaolin and obsidian by alkaline fusion. Ingeniería y competitividad, 2012. 14(2): p. 125-137.
40. Smail, H.A., et al., Synthesis of uniform mesoporous zeolite ZSM-5 catalyst for friedel-crafts acylation. ChemEngineering, 2019. 3(2): p. 35.
41. Yang, L., et al., Role of hydrochloric acid treated HZSM-5 zeolite in Sm2Ti2O7/nHZSM-5 composite for photocatalytic degradation of ofloxacin. Journal of Materials Research and Technology, 2020. 9(5): p. 10585-10596.
42. Singh, B.K., et al., Synthesis of Mesoporous Zeolites and Their Opportunities in Heterogeneous Catalysis. Catalysts, 2021. 11(12): p. 1541.
43. Guo, Y.-P., et al., Fabrication and characterization of hierarchical ZSM-5 zeolites by using organosilanes as additives. Chemical engineering journal, 2011. 166(1): p. 391-400.
44. Klobes, P. and R.G. Munro, Porosity and specific surface area measurements for solid materials. 2006.
45. Anuwattana, R., et al., Conventional and microwave hydrothermal synthesis of zeolite ZSM-5 from the cupola slag. Microporous and mesoporous materials, 2008. 111(1-3): p. 260-266.
46. Kumar, M.S., et al., On the nature of different iron sites and their catalytic role in Fe-ZSM-5 DeNOx catalysts: new insights by a combined EPR and UV/VIS spectroscopic approach. Journal of catalysis, 2004. 227(2): p. 384-397.
47. Schwidder, M., et al., Selective reduction of NO with Fe-ZSM-5 catalysts of low Fe content: I. Relations between active site structure and catalytic performance. Journal of Catalysis, 2005. 231(2): p. 314-330.
2. Rujiwatra, A., A selective preparation of phillipsite and sodalite from perlite. Materials Letters, 2004. 58(14): p. 2012-2015.
3. Boronat, M. and A. Corma, What is measured when measuring acidity in zeolites with probe molecules? ACS catalysis, 2019. 9(2): p. 1539-1548.
4. Kim, D.J. and H.S. Chung, Synthesis and characterization of ZSM-5 zeolite from serpentine. Applied Clay Science, 2003. 24(1-2): p. 69-77.
5. Serrano, D., et al., Molecular and meso-and macroscopic properties of hierarchical nanocrystalline ZSM-5 zeolite prepared by seed silanization. Chemistry of Materials, 2009. 21(4): p. 641-654.
6. Cheng, Y.T., et al., Production of p‐xylene from biomass by catalytic fast pyrolysis using ZSM‐5 catalysts with reduced pore openings. Angewandte Chemie, 2012. 124(44): p. 11259-11262.
7. Chawla, A., et al., Cooperative effects of inorganic and organic structure-directing agents in ZSM-5 crystallization. Molecular Systems Design & Engineering, 2018. 3(1): p. 159-170.
8. Corma, A., State of the art and future challenges of zeolites as catalysts. Journal of Catalysis, 2003. 216(1-2): p. 298-312.
9. Khaleque, A., et al., Zeolite synthesis from low-cost materials and environmental applications: A review. Environmental Advances, 2020. 2: p. 100019.
10. Sanhueza, V., et al., Synthesis of ZSM‐5 from diatomite: a case of zeolite synthesis from a natural material. Journal of Chemical Technology & Biotechnology: International Research in Process, Environmental & Clean Technology, 2004. 79(7): p. 686-690.
11. Coker, E.N., et al., Zeolite ZSM-5 synthesized in space: catalysts with reduced external surface activity. Microporous and mesoporous materials, 2001. 46(2-3): p. 223-236.
12. Garcıa-Martınez, J., et al., Synthesis and characterisation of MFI-type zeolites supported on carbon materials. Microporous and mesoporous materials, 2001. 42(2-3): p. 255-268.
13. Zhang, H., et al., Nano-crystallite oriented self-assembled ZSM-5 zeolite and its LDPE cracking properties: Effects of accessibility and strength of acid sites. Journal of Catalysis, 2013. 302: p. 115-125.
14. Ding, J., et al., Catalytic properties of a hierarchical zeolite synthesized from a natural aluminosilicate mineral without the use of a secondary mesoscale template. ChemCatChem, 2013. 5(8): p. 2258-2269.
15. Xue, Z., et al., Hierarchical structure and catalytic properties of a microspherical zeolite with intracrystalline mesopores. Acta materialia, 2012. 60(16): p. 5712-5722.
16. Moliner, M., C. Martínez, and A. Corma, Multipore zeolites: synthesis and catalytic applications. Angewandte Chemie International Edition, 2015. 54(12): p. 3560-3579.
17. Firoozi, M., M. Baghalha, and M. Asadi, The effect of micro and nano particle sizes of H-ZSM-5 on the selectivity of MTP reaction. Catalysis Communications, 2009. 10(12): p. 1582-1585.
18. Choi, M., et al., Stable single-unit-cell nanosheets of zeolite MFI as active and long-lived catalysts. Nature, 2009. 461(7261): p. 246-249.
19. Rownaghi, A.A. and J. Hedlund, Methanol to gasoline-range hydrocarbons: influence of nanocrystal size and mesoporosity on catalytic performance and product distribution of ZSM-5. Industrial & Engineering Chemistry Research, 2011. 50(21): p. 11872-11878.
20. Konno, H., et al., Effectiveness of nano-scale ZSM-5 zeolite and its deactivation mechanism on catalytic cracking of representative hydrocarbons of naphtha. Microporous and mesoporous materials, 2013. 175: p. 25-33.
21. Wdowin, M., et al., The conversion technology of fly ash into zeolites. Clean Technologies and Environmental Policy, 2014. 16: p. 1217-1223.
22. Park, M., et al., Molten-salt method for the synthesis of zeolitic materials: I. Zeolite formation in alkaline molten-salt system. Microporous and Mesoporous Materials, 2000. 37(1-2): p. 81-89.
23. Mondragon, F., et al., New perspectives for coal ash utilization: synthesis of zeolitic materials. Fuel, 1990. 69(2): p. 263-266.
24. Ojha, K., N.C. Pradhan, and A.N. Samanta, Zeolite from fly ash: synthesis and characterization. Bulletin of Materials Science, 2004. 27: p. 555-564.
25. Hong, J.L.X., et al., Conversion of coal fly ash into zeolite materials: synthesis and characterizations, process design, and its cost-benefit analysis. Industrial & Engineering Chemistry Research, 2017. 56(40): p. 11565-11574.
26. Wang, P., B. Shen, and J. Gao, Synthesis of ZSM-5 zeolite from expanded perlite and its catalytic performance in FCC gasoline aromatization. Catalysis Today, 2007. 125(3-4): p. 155-162.
27. de la Villa Mencia, R.V., et al., Synthesis of zeolite type analcime from industrial wastes. Microporous and Mesoporous Materials, 2020. 293: p. 109817.
28. Knudsen, C., J. Wanvik, and H. Svahnberg, Anorthosites in Greenland: a possible raw material for aluminium? GEUS Bulletin, 2012. 26: p. 53-56.
29. Osmanlioglu, A.E., Immobilization of radioactive waste by cementation with purified kaolin clay. Waste Management, 2002. 22(5): p. 481-483.
30. Arai, T. and S. Maruyama, Formation of anorthosite on the Moon through magma ocean fractional crystallization. Geoscience Frontiers, 2017. 8(2): p. 299-308.
31. Ashwal, L.D. and G.M. Bybee, Crustal evolution and the temporality of anorthosites. Earth-Science Reviews, 2017. 173: p. 307-330.
32. Hodge, J., Fractures, Fluids, and Metamorphism: Shear Zone Initiation in the Marcy Anorthosite Massif, Adirondacks, New York, USA. 2019, The University of Maine.
33. Woldemichael, B.W. and J.-I. Kimura, Petrogenesis of the Neoproterozoic Bikilal-Ghimbi gabbro, Western Ethiopia. Journal of mineralogical and petrological sciences, 2008. 103(1): p. 23-46.
34. He, Y., et al., Research progress on green synthesis of various high-purity zeolites from natural material-kaolin. Journal of Cleaner Production, 2021. 306: p. 127248.
35. Król, M., Natural vs. Synthetic zeolites. Crystals, 2020. 10(7): p. 622.
36. Blasco, T., A. Corma, and J. Martínez-Triguero, Hydrothermal stabilization of ZSM-5 catalytic-cracking additives by phosphorus addition. Journal of catalysis, 2006. 237(2): p. 267-277.
37. Xue, N., et al., Synergistic effects of tungsten and phosphorus on catalytic cracking of butene to propene over HZSM-5. Applied Catalysis A: General, 2009. 352(1-2): p. 87-94.
38. Mgbemere, H., et al., Synthesis of zeolite-a using kaolin samples from Darazo, Bauchi state and Ajebo, Ogun state in Nigeria. Nigerian Journal of Technology, 2018. 37(1): p. 87-95.
39. Ríos, C.A., C.D. Williams, and O.M. Castellanos, Crystallization of low silica Na-A and Na-X zeolites from transformation of kaolin and obsidian by alkaline fusion. Ingeniería y competitividad, 2012. 14(2): p. 125-137.
40. Smail, H.A., et al., Synthesis of uniform mesoporous zeolite ZSM-5 catalyst for friedel-crafts acylation. ChemEngineering, 2019. 3(2): p. 35.
41. Yang, L., et al., Role of hydrochloric acid treated HZSM-5 zeolite in Sm2Ti2O7/nHZSM-5 composite for photocatalytic degradation of ofloxacin. Journal of Materials Research and Technology, 2020. 9(5): p. 10585-10596.
42. Singh, B.K., et al., Synthesis of Mesoporous Zeolites and Their Opportunities in Heterogeneous Catalysis. Catalysts, 2021. 11(12): p. 1541.
43. Guo, Y.-P., et al., Fabrication and characterization of hierarchical ZSM-5 zeolites by using organosilanes as additives. Chemical engineering journal, 2011. 166(1): p. 391-400.
44. Klobes, P. and R.G. Munro, Porosity and specific surface area measurements for solid materials. 2006.
45. Anuwattana, R., et al., Conventional and microwave hydrothermal synthesis of zeolite ZSM-5 from the cupola slag. Microporous and mesoporous materials, 2008. 111(1-3): p. 260-266.
46. Kumar, M.S., et al., On the nature of different iron sites and their catalytic role in Fe-ZSM-5 DeNOx catalysts: new insights by a combined EPR and UV/VIS spectroscopic approach. Journal of catalysis, 2004. 227(2): p. 384-397.
47. Schwidder, M., et al., Selective reduction of NO with Fe-ZSM-5 catalysts of low Fe content: I. Relations between active site structure and catalytic performance. Journal of Catalysis, 2005. 231(2): p. 314-330.
Published
2025-02-06
How to Cite
1.
BizualemYD, Shah MA, Ibrahimi S, Gasmi A, Elboughdiri N. HYDROTHERMAL SYNTHESIS AND CHARACTERIZATION OF ZSM-5 ZEOLITE FROM ANORTHOSITE: IMPACTS OF REACTION TIME AND TEMPERATURE. MatTech [Internet]. 2025Feb.6 [cited 2025Mar.25];59(1):105–112. Available from: https://mater-tehnol.si/index.php/MatTech/article/view/1283
Section
Articles
