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Sains Malaysiana 53(11)(2024): 3731-3744
http://doi.org/10.17576/jsm-2024-5311-15
Highly
Crystalline, Pure ZSM-5 from K2CO3-Treated Mud and Its Catalytic Activity in
Biodiesel Production
(Tinggi Hablur,
ZSM-5 Tulen daripada Lumpur DirawatK2CO3 dan Aktiviti Pemangkinnya dalam Pengeluaran Biodiesel)
HARTATI HARTATI1,*, QURROTA
A’YUNI1, MEDYA AYUNDA FITRI2,
ADIBA NAILA IZZAH1, MELINDA INTAN NOVITALINA1,
PUTRI BINTANG DEA FIRDA1,
TAZKIYATUN NUFUS1, DIDIK PRASETYOKO3,
HARMAMI HARMAMI3,
HASLIZA BAHRUJI4 &
SHAHRUL NIZAM AHMAD5
1Department of Chemistry, Faculty of Science and Technology, Universitas Airlangga, Campus C,
UNAIR, Mulyorejo, Surabaya, 60115, Indonesia
Received: 19
April 2024/Accepted: 27 September 2024
Abstract
Addressing the challenge of clean energy and waste
management for sustainable development goals, ZSM-5 were synthesized from
high-abundance volcano mud (VM) precursor and then utilized as catalyst in
biodiesel production. Unlike conventional alkali treatment, we used the reflux
method to extract the silica-alumina from the VM. K2CO3 alkali salt was utilized as the extractor, activator, and structure-directing
agent. The synthesis was also performed using NaOH as a comparison. Various
analytical techniques were employed including XRD, FTIR, SEM-EDX, TEM, N2 physisorption, and GC-MS to identify the effect of alkali types on the
crystallization rate, morphology, and catalytic activity. Highly crystalline,
pure ZSM-5 was successfully synthesized. It is found that K2CO3 facilitates a slow crystallization rate, requiring a minimum of 5 h of
hydrothermal treatment to produce ZSM-5. Interestingly, slow crystallization
led to homogeneous ZSM-5 particles with a narrow size distribution and a high
mesoporous structure. In contrast, NaOH promoted a faster crystallization rate,
producing inhomogeneous ZSM-5 particles size with a dominant microporosity. Two different feedstock qualities i.e.,
waste cooking oil (WCO) and oleic acid (OA) were used to assess the catalyst’s
versatility. Among all zeolites synthesized using K2CO3,
ZK6 exhibited the highest activity, with an 85.9% yield and 30% selectivity for
FAME in WCO feedstock. In high-quality OA feedstock, ZK6 achieved significantly
higher activity of 97.1% yield with 87.6% selectivity for FAME. ZNa6, the
comparable sample synthesized with NaOH, achieved a 78.2% yield
with 60.4% FAME selectivity in WCO feedstock. A higher catalytic activity of
97.5% yield with 100% selectivity towards FAME was achieved using high-purity
OA feedstock.
Keywords: Biodiesel; K2CO3;
waste cooking oil; ZSM-5
Abstrak
Menangani cabaran tenaga bersih dan pengurusan sisa untuk matlamat pembangunan mampan, ZSM-5 telah disintesis daripada prekursor lumpur gunung berapi (VM) yang memiliki kelimpahan tinggi dan kemudian digunakan sebagai pemangkin dalam pengeluaran biodiesel. Berbeza daripada proses rawatan alkali konvensional, kami menggunakan kaedah refluks untuk mengekstrak alumina silika dalam VM. Garam alkali K2CO3 digunakan sebagai pengekstrak, pengaktif, serta agen pengarah struktur. Sintesis juga dilakukan menggunakan NaOH sebagai perbandingan. Pelbagai teknik analisis digunakan contohnya, XRD, FTIR, SEM-EDX, TEM, N2 fisisorpsi dan GC-MS untuk mengenal pasti kesan jenis alkali ke atas kadar penghabluran, morfologi dan aktiviti pemangkin. ZSM-5 tulen yang sangat kristal telah berjaya disintesis. Didapati bahawa K2CO3 memudahkan kadar penghabluran yang perlahan, memerlukan sekurang-kurangnya 5 jam masa hidroterma untuk menghasilkan ZSM-5. Menariknya, penghabluran perlahan membawa kepada zarah ZSM-5 homogen dengan taburan saiz sempit dan struktur mesoporus yang lebih tinggi berbanding ZSM-5 yang disintesis dengan NaOH. Sebaliknya, NaOH memudahkan kadar penghabluran yang lebih tinggi, menghasilkan saiz zarah ZSM-5 yang tidak homogen dengan struktur mikroporous yang dominan. Dua kualiti bahan mentah yang berbeza iaitu sisa minyak masak (WCO) dan asid oleik (OA) digunakan untuk mengenal pasti kepelbagaian pemangkin. Didapati bahawa antara semua pemangkin yang disintesis dengan K2CO3, ZK6 menunjukkan prestasi tertinggi dengan hasil 85.9% dan selektiviti 30% kepada FAME dalam bahan suapan WCO. Manakala dalam bahan suapan OA, ZK6 menunjukkan 97.1% hasil dengan 87.6% selektiviti kepada FAME. ZNa6, sampel setandingnya mencapai hasil 78.2% dengan selektiviti FAME 60.4% dalam bahan suapan WCO. Aktiviti pemangkin yang lebih tinggi sebanyak 97.5% hasil dengan selektiviti 100% terhadap FAME dicapai menggunakan bahan suapan OA ketulenan tinggi.
Kata kunci: Biodiesel; K2CO3; sisa
minyak masak; ZSM-5
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