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-FAN WONG1, KRITTANUN DEEKAMWONG2,
JATUPORN WITTAKAYUN2*, TAU CHUAN LING3, OKI MUZARA4,
HOOI LING LEE1, FAROOK ADAM1, ENG-POH NG1*
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
Diserahkan: 21 April 2017/Diterima:
17 Ogos 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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*Pengarang untuk surat-menyurat; email: epng@usm.my