The Malaysian Journal of Analytical Sciences, Vol 11, No 1 (2007): 84-92 84 DELAMINATED ZEOLITE, ITQ-6 AS HETEROGENEOUS CATALYST FOR FRIEDEL CRAFTS ALKYLATION Zainab Ramli*, Noor Aishikin Mohd Yusoff and Halimaton Hamdan Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor, Malaysia Keywords : Mesoporous ITQ-6, Microporous FER, alkylation of resorcinol Abstract The ability of ITQ-6, a kind of mesoporous zeolitic material to replace microporous zeolite as catalyst has attracted particular attention. In this study, modification of a precursor of microporous ferrierite, PREFER to mesoporous material, ITQ-6 was carried out by delamination technique. The XRD results show that the crystalline phase of PREFER diminished for the sample after delamination. Porosity study of the ITQ-6 sample shows formation of homogeneous mesopores in the size between 3.5-4.0 nm. The acidity study indicates that ITQ-6 still contains appreciable amounts of Brönsted and Lewis acidities. Catalytic evaluation of the resulting material, ITQ-6 was carried out in the alkylation of resorcinol with methyl tert -butyl ether which gave 4- tert-butyl resorcinol and 4,6-di-tert -butyl resorcinol as main products. The conversion of resorcinol when using ITQ-6 was ten times higher than ferrierite, FER with similar selectivity of disubstituted product. It shows that the mesoporosity of ITQ-6 was responsible for the higher activity of the catalyst in the reaction. Abstrak Kebolehan ITQ-6 sejenis bahan zeolit berliang meso menggantikan zeolit berliang mikro sebagai mangkin telah menarik perhatian. Dalam kajian ini, pengubahsuaian bahan awal ferrierit berliang mikro, PREFER kepada bahan berliang meso ITQ-6 dilakukan melalui teknik penyahlaminan. Keputusan XRD menunjukkan yang fasa hablur PREFER musnah selepas proses penyahlaminan. Kajian keliangan terhadap sampel ITQ-6 menunjukkan pembentukan liang meso yang homogen dengan saiz liang antara 3.5-4.0 nm. Kajian keasidan menunjukkan yang ITQ-6 masih mengandungi keasidan Brönsted dan Lewis dengan amoun yang agak banyak. Kereaktifan bahan yang terhasil, ITQ-6 diuji dalam tindak balas pengalkilan resorsinol dengan metil tert butyl eter yang menghasilan 4-tert-butil resorsinol and 4,6-di- tert -butil resorsinol sebagai hasil utama. Pertukaran resorsinol apabila menggunakan ITQ-6 adalah sepuloh kali lebih tinggi daripada ferrierit, FER, dengan kepilihan yang sama bagi hasil dwitertukarganti. Ini menunjukkan yang ITQ-6 yang berliang meso bertanggungjawab ke atas kereaktifan mangkin dalam tindak balas. Introduction The Friedel Crafts alkylation of resorcinol with methyl tert-butyl ether or equivalent alkylating agents is known to give mono tert-butylated product (4-tert-butyl resorcinol) and further alkylation will lead to the formation of di-tert-butylated product (4,6-di-tert-butyl resorcinol) [1]. The products (butylated dihydroxybenzenes) are useful materials in the synthesis of antioxidants, polymer stabilizer and in the treatment of mitochondrial respiration ailments. Therefore this reaction has become industrially important. Presently, Lewis acid type catalysts for aromatic alkylations include aluminum chloride, ferric chloride, and boron trifluoride. Those of the Bronsted-Lowry acid type are fluoride acid, sulfuric acid and phosphoric acid. However, these traditional catalysts have limitations such as environmental pollution hazards arising from the disposal of potential toxic wastes, reactor corrosion and difficulty in handling. In order to avoid these problems many efforts have been devoted in the search of solid acid and base catalysts more selective, safe, environment friendly, generable, reusable and which need not to be destroyed after reaction. Therefore acidic oxide catalysts of the silica alumina type especially zeolite and cation-exchange resins are becoming increasingly useful as heterogeneous catalysts. Throughout the 1990s, environmentalism remains a foremost concern, with zeolite in the forefront as solutions to new challenges in the generation of “Green Chemistry”. The versatility of zeolite has allowed its application particularly as heterogeneous catalyst in acid [2], base [3] and redox [4] reactions. Over a wide range of solid acids, zeolites hold high acidities on their surface and have received much attention in industry [5] and organic synthesis [6]. Uses of zeolite in the Friedel-Crafts reactions were extensively been studied [7, 8].