Malaysian
Journal of Analytical Sciences Vol 24 No 3
(2020): 390 - 404
OPTIMIZATION OF MONTMORILLONITE K10 ION-EXCHANGE
WITH Fe3+ FOR THE APPLICATION OF BIODIESEL PRODUCTION
(Pengoptimuman
Pertukaran Ion Montmorilonit K10 dengan Fe3+ untuk Aplikasi
Penghasilan Biodiesel)
Syahirah Yahya1 and Farah Wahida Harun2, 3*
1Department of Chemistry and Food Technology,
Politeknik Tun Syed Nasir Syed Ismail,
Hab Pendidikan Tinggi Pagoh, KM1 Jalan Panchor, 84600 Pagoh,
Johor, Malaysia
2Faculty of Science and Technology
3Frontier Materials Research Group
Universiti Sains Islam Malaysia, Bandar Baru Nilai, 71800
Nilai, Negeri Sembilan, Malaysia
*Corresponding
author: farahw@usim.edu.my
Received: 20 November
2019; Accepted: 17 April 2020; Published: 9 June 2020
Abstract
The modification of
montmorillonite K10 with Fe3+ was investigated to study the optimum
ion-exchange occurred in the interlayers of clays. Montmorillonite K10 was
modified to be applied as a catalyst in biodiesel production from waste cooking
oil (WCO). Three methods to optimize the ion-exchange process were
investigated. For method 1 and method 2, respective 14% and 27% by mass of Fe
in montmorillonite K10 were stirred in a closed cap system for 7 hours while
method 3 applied 20% of Fe stirred with montmorillonite K10 for 24 hours until
it became mold and slurry. The ability of ion-exchange was tested using
SEM/EDX. It was found that 1.21% Fe composition increased by using method 1
while 2.66% Fe increased using method 2. The highest Fe exchange was detected
using method 3 with 5.23% increment. For more accurate result, 20% Fe-MMT K10
from method 3 was characterized using XRF and it was found that the ion
exchange occurred with interchangeable Ca2+. In correlation, the
effect of Fe increment on acidity was studied by using TPD-NH3.
Naturally, montmorillonite K10 possessed 0.232 mmol/g of acidity. The results
found that the highest acidity was detected for 20% Fe-MMT K10 (14.261 mmol/g).
The application of montmorillonite K10 on biodiesel production increased the
yield up to 38.39% compared to the reaction without catalyst (26.80%). With the
aid of modified montmorillonite K10, 66.54% and 69.32% biodiesel were produced
using catalyst from method 1 and 2 respectively. Amazingly, an outstanding
yield was produced by using catalyst from method 3 (84.58%). Therefore, 20%
Fe-MMT K10 catalyst was selected for further biodiesel optimization via
conventional method. It was found that 96.49% biodiesel was successfully
produced with 28.65% acid conversion at 150 °C, 6 h, 12:1 methanol: oil and 4
wt.% mass of catalyst. The investigations on acid conversion and biodiesel
yield proved that the modification of montmorillonite K10 with 20% Fe is the
optimum and the catalyst can undergo both esterification and
transesterification reactions simultaneously to produce optimum biodiesel
yield.
Keywords:
Montmorillonite K10, Fe3+ ion-exchange,
simultaneous esterification-transesterification, biodiesel, waste cooking oil
Abstrak
Pengubahsuaian montmorilonit K10 dengan Fe3+ telah dijalankan
untuk mengkaji pertukaran ion yang optimum pada lapisan tanah liat.
Montmorilonit K10 diubahsuai untuk dijadikan sebagai pemangkin dalam
pengeluaran biodiesel dari minyak masak terpakai (WCO). Tiga kaedah untuk
mengoptimumkan proses pertukaran ion telah dikaji. Untuk kaedah 1 dan kaedah 2,
masing-masing 14% dan 27% jisim Fe dalam montmorilonit K10 telah dicampur dalam
sistem tertutup selama 7 jam. Manakala kaedah 3 menggunakan 20% Fe dikacau
dengan montmorilonit K10 selama 24 jam sehingga pekat seperti tanah liat.
Keupayaan penukaran ion telah diuji menggunakan SEM/EDX. Hasil kajian mendapati
bahawa komposisi Fe meningkat sebanyak 1.21% dengan menggunakan kaedah 1
manakala 2.66% Fe meningkat dengan menggunakan kaedah 2. Pertukaran Fe tertinggi
telah dikesan menggunakan kaedah 3 dengan kenaikan Fe sebanyak 5.23%. Untuk
hasil yang lebih tepat, 20% Fe-MMT K10 dari kaedah 3 dicirikan dengan
menggunakan XRF dan didapati ion Ca2+ bertukar dengan Fe3+.
Kesan kenaikan Fe terhadap tahap keasidan dikaji dengan menggunakan TPD-NH3.
Pada asalnya, montmorilonit K10 mempunyai tahap keasidan 0.232 mmol/g. Setelah
diubahsuai, keasidan tertinggi dikesan pada sampel 20% Fe-MMT K10 (14.261 mmol
/ g). Penggunaan montmorilonit K10 dalam pengeluaran biodiesel menghasilkan
38.39% produk berbanding tindak balas tanpa pemangkin (26.80%). Dengan bantuan
montmorilonit K10 yang diubahsuai, masing-masing 66.54% dan 69.32% biodiesel
dihasilkan menggunakan pemangkin yang diubahsuai dari kaedah 1 dan 2. Namun,
biodiesel yang paling tinggi dihasilkan dengan menggunakan pemangkin daripada
kaedah 3 (84.58%). Oleh itu, pemangkin 20% Fe-MMT K10 telah dipilih untuk
pengoptimuman biodiesel melalui kaedah konvensional. Hasil kajian mendapati
bahawa 96.49% biodiesel berjaya dihasilkan dengan penukaran asid sebanyak
28.65% pada 150 °C, 6 jam, 12: 1 metanol: minyak dan 4% berat masa pemangkin.
Kajian penukaran asid dan hasil biodiesel telah membuktikan bahawa
pengubahsuaian montmorilonit K10 dengan 20% Fe adalah optimum dan 20% Fe-MMT K10
boleh menjalani tindak balas esterifikasi dan transesterifikasi secara serentak
untuk menghasilkan biodiesel yang optimum.
Kata kunci: Montmorilonit K10, pertukaran ion Fe3+,
esterifikasi-transesterifikasi serentak, biodiesel, minyak masak terpakai
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