1 [PCR-03] Proceeding the Regional Conference on Chemical Engineering 2014 Yogyakarta, December 2-3, 2014 ISBN: 978-602-71398-0-0 Synthesis and characterization of highly ordered solid acid catalyst from kaolin 1 Peter Adeniyi Alaba, 1,2 Yahaya Muhammad Sani & 1 Wan Mohd Ashri Wan Daud 1 Department of Chemical Engineering, University of Malaya, 50603 Kuala Lumpur, Malaysia. 2 Department of Chemical Engineering, Ahmadu Bello University, 870001 Nigeria. Email: ashri@um.edu.my, adeniyipee@live.com & ymsani@siswa.um.edu.my Abstract. Crystalline solidacid catalysts exhibit higher catalytic activity and hydrothermal stability in catalytic cracking compared with their amorphous counterparts. This is because of the presence of stronger Brönsted acid sites on their surfaces. Thus, we report the synthesis of crystalline solidacid material by impregnating NaOH into the pores of thermal and acid-treated amorphous aluminosilicate. NH3-TPD, XRD, TGA and DSC revealed the surface acidity, structural and textural properties of the materials. All the kaolinites peaks in the starting material disappeared after the thermal and acid activation. Interestingly, most of the crystalline peaks reappeared with greater intensities at the (0211) band after NaOH impregnation. Further, the crystallinity index calculated by weighted intensity ratio index (WIRI) at (0211) band showed superior crystallinity for the synthesized material than the starting kaolin. This is in consonant with reemerging crystalline peaks. The acidity … This work demonstrates that impregnation of NaOH on amorphous aluminosilicate is a novel route for synthesizing of crystalline superacid catalysts. Keywords: Solidacid catalyst; kaolinite; acid activation; alkali activation; crystallinity. 1. Introduction Biodiesel is renewable, sustainable and nonfossil based fuel with various advantages such as renewability, sustainability, biodegradability, lower GHG-emissions and enhanced lubricity [9]. Further, the prospect of producing biodiesel from existing refineries is promising. However, robust and active solidacid catalysts are essential for ensuring smooth transition into the refineries for commercial productions. Evidently, solidacid catalysts have gained wide acceptance in catalytic conversion processes such as bulk chemistry and petrochemical processes [1, 2]. However, cost of producing such catalysts remains major challenge hindering catalysis from ensuring the prominence of biodiesel. Hence, cheaper starting materials with equally high catalytic properties will help in alleviating the economic constraints. Interestingly, kaolinites clay minerals catalysts found industrial applications since the early 1930s. Significant progress in several industrial processes such as petrochemistry; especially catalytic refining and bulk chemistry became possible with kaolinite as precursor in active catalyst synthesis. This is because of the unique structure and pore size which are suitable for conversion of bulky molecules [3]. These explain the renewed interests that aluminosilicates from clay are receiving towards solidacid catalyst synthesis. However, kaolinites resist acid attack during activation because of higher octahedral alumina contents. Calcining at temperatures between 550 and 950 ° C subdues this resistance by transforming the clay to metakaolin. Nonetheless, this transformation deforms the crystalline structure of the clay material. A process for alleviating these issues is acid leaching of metakaolin. Development of porosity, acidity and surface area are the major significance of acid leaching. The process also dealuminates and purifies the octahedral layers to facilitate formation of surface structure. However, materials synthesized by this procedure are amorphous in nature. Therefore, there is a need to make the catalytic material crystalline for higher catalytic performances. This is