Hydrothermal Synthesis and Characterization of ZSM-5 Zeolite from Nigerian-Origin Kaolin: Effects of Crystallization Temperature on Structure and Morphology

Authors

  • Henry E. Mgbemere Metallurgical and Materials Engineering Department, University of Lagos, Akoka-Yaba, Lagos, Nigeria
  • Augustine B. Okoubulu Materials and Metallurgical Engineering Department, Southern Delta University, P.M.B. 5, Ozoro, Nigeria
  • Cynthia C. Nwaeju Department of Mechanical Engineering, Nigeria Maritime University, Okerenkoko, Delta State, Nigeria
  • Pius A. Uzere Department of Mechanical Engineering, Federal University of Petroleum Resources, Effurun, Delta State, Nigeria
  • Francis O. Edoziuno Department of Metallurgical and Materials Engineering, Nnamdi Azikiwe University, P.M.B. 5025 Awka., Nigeria

Keywords:

ZSM-5 Zeolite, Kaolin, Crystallization, Metakaolinization, Hydrothermal synthesis

Abstract

This study investigates the hydrothermal synthesis and characterization of ZSM-5 zeolite from Ajebo kaolin in Nigeria, with a focus on the effects of crystallization temperature on the structure and morphology. ZSM-5 zeolite was synthesized at crystallization temperatures of 100°C, 120°C, and 150°C, with a fixed crystallization time of 6 hours. Characterization techniques, including XRF, FTIR, XRD, EDX, and SEM, were employed to analyze the composition and structure of the synthesized zeolites. The results confirmed the synthesis of ZSM-5 at all temperatures, with the sample crystallized at 150°C achieving the highest crystallinity (85%) and a distinct hexagonal prismatic morphology. XRF analysis revealed high SiO₂ (50–60%) and Al₂O₃ (40–45%) content. FTIR analysis confirmed the absence of -OH vibrations (3600–3700 cm⁻¹) in metakaolin, indicating successful dihydroxylation. A prominent peak at 1078 cm⁻¹ validated the formation of ZSM-5. XRD patterns substantiated the phase transformation from kaolin to ZSM-5, with improved crystallinity at higher temperatures. SEM images showed that the ZSM-5 synthesized at 150°C exhibited well-defined hexagonal prisms. The higher the crystallization temperature, the better the crystallinity of the synthesized zeolites. This study demonstrates Ajebo kaolin as a sustainable and cost-effective source for producing ZSM-5 zeolite, highlighting its potential applications as a catalyst in the breakdown of hydrocarbons and other industrial processes.

Author Biographies

Augustine B. Okoubulu, Materials and Metallurgical Engineering Department, Southern Delta University, P.M.B. 5, Ozoro, Nigeria

okoubulua@gmail.com

Cynthia C. Nwaeju, Department of Mechanical Engineering, Nigeria Maritime University, Okerenkoko, Delta State, Nigeria

cynthianwaeju@gmail.com

Francis O. Edoziuno, Department of Metallurgical and Materials Engineering, Nnamdi Azikiwe University, P.M.B. 5025 Awka., Nigeria

francisedoziuno@gmail.com

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Published

2026-06-05

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Articles