Sains Malaysiana 51(2)(2022): 519-532

http://doi.org/10.17576/jsm-2022-5102-16

Synthesis and Characterization of Metal Sulfates Loaded Palm Empty Fruit Bunch (PEFB) for Biodiesel Production

(Sintesis dan Pencirian Sulfat Logam Dimuatkan Tandan Kosong Kelapa Sawit (PEFB) untuk Pengeluaran Biodiesel)

RAHILA ISHFAQ¹*, NURUN NAJWA RUSLAN¹, NURSYAFREENA ATTAN², SUZI SALWAH JIKAN¹ & AMIRA SARYATI AMERUDDIN¹

¹Faculty of Applied Sciences and Technology, Universiti Tun Hussein Onn Malaysia, 86400 Parit Raja, Johor Darul Takzim, Malaysia

²Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM, Johor Darul Takzim, Malaysia

Received: 6 February 2021/Accepted: 28 May 2021

ABSTRACT

Biodiesel has been globally accepted as a green substitute for diesel fuel. However, the insecurity of food raised with the application of edible sources in biodiesel production has caused much debate. The feasible alternative technique is the use of inedible and low-grade sources such as palm fatty acid distillate (PFAD). In this work, the production of biodiesel (FAME) from PFAD using solid acid catalysts (SACs) derived from palm empty fruit bunch (PEFB) is investigated. The SACs were synthesized through impregnation of different metal sulfate precursors, i.e. ferrous sulfate heptahydrate (FeSO₄.7H₂O), copper sulfate pentahydrate (CuSO₄.5H₂O), and magnesium sulfate heptahydrate (MgSO₄.7H₂O) over PEFB. SEM-EDX observations found that impregnation and then calcination resulted in attachment of sulfur (S) and improved surface porosity. FT-IR analysis showed that there were distinct interactions between metal sulfates and PEFB. XRD characterization showed that the prepared catalysts have a crystalline structure. Besides, the catalytic activity of the SACs was closely associated with their acid densities measured by the titration method. Fe-PEFB catalyst showed the highest acid density (2.44 mmol/g) among the catalysts studied. To study the effect of process parameters on FFA conversion (%), optimization of methanol: PFAD molar ratio, catalyst dosage, reaction temperature, and reaction time was conducted. Maximum FFA conversion of 89.1% was obtained over Fe-PEFB while Cu-PEFB and Mg-PEFB achieved an FFA conversion of 63 and 56.5%, respectively, under the optimum reaction conditions. Thus, the present study offers a sustainable and environmentally benign method for biodiesel production.

Keywords: Biodiesel; biomass waste; esterification; impregnation; palm fatty acid distillate; solid acid catalysts

ABSTRAK

Biodiesel telah diterima secara global sebagai pengganti hijau untuk bahan api diesel. Walau bagaimanapun, ketidakamanan makanan yang dibangkitkan dengan penggunaan sumber yang boleh dimakan dalam pengeluaran biodiesel telah menyebabkan banyak perdebatan. Teknik alternatif yang boleh dilaksanakan ialah penggunaan sumber yang tidak boleh dimakan dan bermutu rendah seperti sulingan asid lemak kelapa sawit (PFAD). Dalam kerja ini, pengeluaran biodiesel (FAME) daripada PFAD menggunakan mangkin asid pepejal (SAC) yang diperoleh daripada tandan kosong kelapa sawit (PEFB) telah dikaji. SAC telah disintesis melalui penjejalan pelopor sulfat logam yang berbeza, iaitu, ferus sulfat heptahidrat (FeSO₄.7H₂O), kuprum sulfat pentahidrat (CuSO₄.5H₂O) dan magnesium sulfat heptahidrat (MgSO₄.7H₂O) berbanding PEFB. Pemerhatian SEM-EDX mendapati bahawa penjejalan dan kemudian pengkalsinan menghasilkan perlekatan sulfur (S) dan liang permukaan bertambah baik. Analisis FT-IR menunjukkan bahawa terdapat interaksi yang berbeza antara sulfat logam dan PEFB. Pencirian XRD menunjukkan bahawa pemangkin yang disediakan mempunyai struktur hablur. Selain itu, aktiviti pemangkin SAC berkaitan dengan ketumpatan asid mereka yang diukur dengan kaedah pentitratan. Mangkin Fe-PEFB menunjukkan ketumpatan asid tertinggi (2.44 mmol/g) antara mangkin yang telah dikaji. Untuk mengkaji kesan parameter proses terhadap penukaran FFA (%), pengoptimuman metanol:nisbah molar PFAD, dos mangkin, suhu tindak balas dan masa tindak balas telah dijalankan. Penukaran FFA maksimum sebanyak 89.1% diperoleh berbanding Fe-PEFB manakala Cu-PEFB dan Mg-PEFB mencapai penukaran FFA sebanyak 63 dan 56.5%, dalam keadaan tindak balas yang optimum. Oleh itu, kajian ini menawarkan kaedah yang mampan dan jinak alam sekitar untuk pengeluaran biodiesel.

Kata kunci: Biodiesel; mangkin asid pepejal; pengesteran; penjejalan; penyulingan asid lemak sawit; sisa biojisim

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*Corresponding author; email: rahilanaz.ishfaq@gmail.com