Sains Malaysiana 47(2)(2018): 337-345

http://dx.doi.org/10.17576/jsm-2018-4702-16

Nanocrystalline K-F Zeolite from Rice Husk Silica as an Eco-friendly Solid Base Catalyst for the Synthesis of Jasminaldehyde under Microwave Irradiation

(Nanohablur K-F Zeolit daripada Silika Sekam Padi sebagai Mangkin Bes Pepejal  Mesra Alam untuk Sintesis Jasminaldehid di bawah Sinaran Gelombang Mikro)

SIEW-FANG WONG¹, KRITTANUN DEEKAMWONG², JATUPORN WITTAKAYUN², TAU CHUAN LING³, OKI MUZARA⁴, HOOI LING LEE¹, FAROOK ADAM¹ & ENG-POH NG^1*

¹School of Chemical Sciences, Universiti Sains Malaysia, 11800 USM, Pulau Pinang, Malaysia

²School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000, Thailand

³Institute of Biological Sciences, Faculty of Science, University of Malaya, 50603 Kuala Lumpur, Federal Territory, Malaysia

⁴Center of Research Excellence in Nanotechnology and Chemical Engineering Department, King Fahd University of Petroleum & Minerals, Dhahran 31261, Saudi Arabia

  Received: 21 April 2017/Accepted: 17 August 2017

ABSTRACT

Nanocrystalline aluminosilicate F-type zeolite (K-F, EDI-type structure) was synthesized in an organic template-free system using rice husk ash (RHA) silica source and microwave energy. The morphology, crystallite size, chemical composition, crystallographic and basicity properties of the nanocrystals were studied by using various characterization techniques. The results showed that fully crystalline K-F zeolite (Si/Al ratio = 1.26) with flattened cuboid-like shaped could be obtained within 2 min of crystallization which was considerably very fast. In addition, K-F zeolite nanocrystals was also tested as a solid base catalyst in the microwave-enhanced Aldol condensation reaction of heptanal with benzaldehyde and the six catalytic parameters were studied and optimized. The nanosized K-F zeolite crystals showed good catalytic performance in the studied reaction with 77.1% heptanal conversion and 69.5% jasminaldehyde selectivity under optimum reaction condition. The nanocatalyst was reusable and no significant loss in its catalytic reactivity was observed even after five consecutive reaction cycles.

Keywords: Aldol condensation; K-F; nanozeolite; microwave synthesis; organotemplate free

ABSTRAK

Nanohablur aluminosilikat jenis F zeolite (K-F, jenis struktur EDI) telah disintesis dalam sistem bebas templat organik menggunakan sumber silika sekam padi (RHA) dan tenaga gelombang mikro. Morfologi, saiz hablur, komposisi kimia, sifat hablurgrafi dan sifat dasar nanohablur dikaji dengan menggunakan pelbagai teknik pencirian. Keputusan menunjukkan bahawa zeolit ​​K-F menghablur sepenuhnya (nisbah Si / Al = 1.26) dengan bentuk membentuk kuboid rata diperolehi dalam masa 2 minit penghabluran. Selain itu, nanohablur zeolit K-F juga diuji sebagai pemangkin asas pepejal dalam tindak balas pemeluwapan Aldol yang dipertingkatkan oleh gelombang mikro heptanal dengan benzaldeid dan enam ukuran pemangkin dikaji dan dioptimumkan. Zeolit ​​K-F nanohablur menunjukkan prestasi pemangkin yang baik dalam tindak balas yang dikaji dengan penukaran 77.1% heptanal dan jasminaldehid memilih 69.5% di bawah keadaan tindak balas optimum. Nanopemangkin boleh digunakan semula dan tiada kehilangan ketara dalam tindakbalas pemangkinnya selepas lima kitaran reaksi berturut-turut.

Kata kunci: K-F; kodensasi aldol; sintesis gelombang mikro; templat organo bebas; zeolit hablur

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*Corresponding author; email: epng@usm.my