Malaysian
Journal of Analytical Sciences Vol 26 No 2
(2022): 303 - 317
DIRECT CATALYTIC
CONVERSION OF CELLULOSE INTO FORMIC ACID BY SUPPORTED PHOSPHOTUNGSTIC ACID
CATALYST
(Penukaran
Terus Selulosa Kepada Asid Formik Menggunakan Pemangkin Asid Fosfotungstik yang
Disokong)
Nor
Liyana Zakira Zabidi Adil @ Zaibidai Adil, Farah Wahida Harun, Syaza Azhari,
Lailatun Nazirah Ozair, Shikh
Mohd Shahrul Nizan Shikh Zahari, Tengku Shafazila Tengku Saharuddin*
Faculty
of Science and Technology,
Universiti
Sains Islam Malaysia, Bandar Baru Nilai, 71800 Nilai, Negeri Sembilan
*Corresponding
author: shafazila@usim.edu.my
Received: 15 August 2021; Accepted: 11 January 2022; Published: 28 April 2022
Abstract
This
study aims to prepare phosphotungstic acid supported on hydrotalcite (PTA-HT)
for one-pot hydrothermal cellulose conversion into formic acid (FA). In this
study, different percentages of PTA on HT (1, 5, 10, 15, 20, 25, and 33%) were
prepared and the catalytic activity was observed for two different parameters
such as time (1 to 5 hours) and reaction temperature (160 to 240 °C).
The prepared catalysts were characterized using Fourier transform infrared
(FTIR), X-ray powder diffraction (XRD), Brunauer-Emmet-Teller (BET) and field
emission scanning electron microscopy-energy dispersive X-ray spectrometry
(FESEM-EDX), while the production of FA was determined using ultra
high-performance liquid chromatography (UHPLC). To avoid bias, raw PTA and
calcined HT were compared with varying percentages of supported PTA. PTA-HT was
successfully prepared through the impregnation method as confirmed by XRD,
FTIR, BET and FESEM-EDX. According to the results, the optimum condition for
cellulose conversion into formic acid was when 25% PTA-HT was applied at 220 °C
for 4 hours, with a 30% cellulose conversion and 18 % FA yield. Due to the
acidity and redox properties of PTA, it has been demonstrated that PTA-HT
increased the catalytic activity by two-fold when compared to calcined HT alone
(8%). The significance of this finding opens new suggestion of bifunctional
catalyst in cellulose conversion into FA.
Keywords: catalyst, cellulose, formic acid,
hydrothermal, phosphotungstic acid
Abstrak
Tujuan kajian ini adalah untuk
menyediakan asid fosfotungstik yang disokong dengan oleh hidrotalsit (PTA-HT)
bagi proses hidroterma penukaran selulosa kepada asid formik. Di dalam kajian
ini, perbezaan peratus PTA ke atas HT (1, 5, 10, 15, 20, 25 dan 33%) telah
disediakan dan aktiviti pemangkinan telah dijalankan terhadap dua parameter
iaitu masa (1 jam hingga 5 jam) dan suhu (160 hingga 240 ℃). Pemangkin
yang telah disediakan diperincikan menggunakan inframerah transformasi Fourier
(FTIR), pembelauan sinar-X (XRD), Brunauer-Emmet-Teller (BET) and mikroskopi
imbasan pancaran medan-spektrometri tenaga serakan sinar-X (FESEM-EDX)
manakala asid formik yang terhasil ditentukan menggunakan kromatografi cecair
berprestasi ultra tinggi (UHPLC). Bagi mengelakkan keputusan yang berat sebelah
dalam kajian, PTA tulen dan HT yang dikalsin telah dibandingkan dengan
perbezaan peratus PTA yang disokong. PTA-HT yang telah disediakan melalui
kaedah impregnasi dicirikan oleh XRD, FTIR, BET dan FESEM-EDX. Berdasarkan
keputusan, keadaan yang paling optimum bagi penukaran selulosa kepada asid formik
adalah apabila 25% PTA-HT digunakan pada 220 ℃ selama 4 jam dengan
menghasilkan 30% penukaran selulosa dan 18% penghasilan asid formik. Oleh
kerana ciri-ciri asid dan redoks yang dimiliki oleh PTA, keputusan kajian telah
menunjukkan bahawa PTA yang disokong oleh HT meningkatkan aktiviti pemangkin
sebanyak dua kali ganda berbanding HT yang telah dikalsin yang hanya
menghasilkan 8% asid formik. Kepentingan kajian ini akan membuka cadangan baru
terhadap penggunaan pemangkin dwifungsi dalam penukaran selulosa kepada asid
formik.
Kata kunci: pemangkin, selulosa, asid
formik, hidroterma, asid fosfotungstik
Graphical Abstract
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