Synthesis of sulfonated rice husk silica for PFAD esterification: Effect of calcination temperature
DOI:
https://doi.org/10.18686/cest832Keywords:
rice husk silica; biodiesel; sulfonic acid; esterification; palm fatty acid distillateAbstract
This study investigates the possibility of silica produced from rice husks as a precursor for the development of solid acid catalysts, indicating mostly heterogeneous behavior under the conditions examined to produce biodiesel. Rice husk silica (RHS) was prepared via controlled thermal treatment and subsequently functionalized with sulfonic acid groups via a post-grafting-oxidation method using 3-mercaptopropyltrimethoxysilane as a precursor. The influence of calcination temperature (700–900 °C) on the structural, textural, and acidic properties of the resulting catalysts was systematically examined. It was found that lower calcination temperatures favor the preservation of surface silanol groups, which are essential for effective grafting and high acid site density. Among the synthesized materials, RHS-700-SO3H exhibited the highest acidity (0.55 mmol H+ g−1) and demonstrated the highest catalytic activity among the synthesized catalysts. Under investigated conditions, a maximum free fatty acid conversion of 92.7% was achieved in the esterification of palm fatty acid distillate (PFAD). The observed catalytic activity is correlated with the physicochemical properties of the synthesized catalysts, including surface acidity and pore structure, although further characterization is required to fully elucidate the nature of the active sites. The RHS-700-SO3H catalyst showed reasonable reusability. However, a gradual decline in activity was observed due to partial leaching of sulfonic acid groups. These findings demonstrate that rice husk-derived silica is a promising platform for the development of biomass-derived solid acid catalysts, although further evaluation of economic feasibility and process efficiency is required.
References
1. Pranta MH, Cho HM. A comprehensive review of the evolution of biodiesel production technologies. Energy Conversion and Management. 2025; 328: 119623. doi: 10.1016/j.enconman.2025.119623
2. Guo M, Jiang W, Chen C, et al. Process optimization of biodiesel production from waste cooking oil by esterification of free fatty acids using La3+/ZnO-TiO2 photocatalyst. Energy Conversion and Management. 2021; 229: 113745. doi: 10.1016/j.enconman.2020.113745
3. Borges ME, Díaz L. Recent developments on heterogeneous catalysts for biodiesel production by oil esterification and transesterification reactions: A review. Renewable and Sustainable Energy Reviews. 2012; 16(5): 2839–2849. doi: 10.1016/j.rser.2012.01.071
4. Kumar S, Salam P, Shrestha P, et al. An Assessment of Thailand’s Biofuel Development. Sustainability. 2013; 5(4): 1577–1597. doi: 10.3390/su5041577
5. Cho HJ, Kim SH, Hong SW, et al. A single step non-catalytic esterification of palm fatty acid distillate (PFAD) for biodiesel production. Fuel. 2012; 93: 373–380. doi: 10.1016/j.fuel.2011.08.063
6. Sani YM, Daud WMAW, Aziz ARA. Activity of solid acid catalysts for biodiesel production: A critical review. Applied Catalysis A: General. 2014; 470: 140–161. doi: 10.1016/j.apcata.2013.10.052
7. Melero JA, Van Grieken R, Morales G. Advances in the Synthesis and Catalytic Applications of Organosulfonic-Functionalized Mesostructured Materials. Chemical Reviews. 2006; 106(9): 3790–3812. doi: 10.1021/cr050994h
8. Gupta P, Paul S. Solid acids: Green alternatives for acid catalysis. Catalysis Today. 2014; 236: 153–170. doi: 10.1016/j.cattod.2014.04.010
9. Saha L, Bauddh K. Phytomanagement of iron mine soil by Ricinus communis L. and garden soil. Chemosphere. 2023; 313: 137534. doi: 10.1016/j.chemosphere.2022.137534
10. Adam F, Appaturi JN, Iqbal A. The utilization of rice husk silica as a catalyst: Review and recent progress. Catalysis Today. 2012; 190(1): 2–14. doi: 10.1016/j.cattod.2012.04.056
11. Hassan Q, Algburi S, Sameen AZ, et al. A review of hybrid renewable energy systems: Solar and wind-powered solutions: Challenges, opportunities, and policy implications. Results in Engineering. 2023; 20: 101621. doi: 10.1016/j.rineng.2023.101621
12. Quevedo-Amador RA, Escalera-Velasco BP, Arias AMR, et al. Application of waste biomass for the production of biofuels and catalysts: a review. Clean Technologies and Environmental Policy. 2024; 26(4): 943–997. doi: 10.1007/s10098-023-02728-4
13. Maroa S, Inambao F. A review of sustainable biodiesel production using biomass derived heterogeneous catalysts. Engineering in Life Sciences. 2021; 21(12): 790–824. doi: 10.1002/elsc.202100025
14. Tedesco AD, Ambrosi E, Borsacchi S, et al. Functionalization of Mesoporous Silica Nanoparticles with Organosilanes: Experimental Evidence of the Interaction Between Organic Groups and Silica Surface. Current Organic Chemistry. 2017; 21(24). doi: 10.2174/1385272821666161230120108
15. Sharghi H, Shiri P, Aberi M. An overview on recent advances in the synthesis of sulfonated organic materials, sulfonated silica materials, and sulfonated carbon materials and their catalytic applications in chemical processes. Beilstein Journal of Organic Chemistry. 2018; 14: 2745–2770. doi: 10.3762/bjoc.14.253
16. Aneu A, Wijaya K, Syoufian A. Silica-Based Solid Acid Catalyst with Different Concentration of H2SO4 and Calcination Temperature: Preparation and Characterization. Silicon. 2021; 13(7): 2265–2270. doi: 10.1007/s12633-020-00741-6
17. Na Lumphoon K, Ngampradit S, Yousatit S, et al. Tunable organosulfonic acid-functionalized natural rubber/wormhole-like mesostructured silica nanocomposites for enhancing the esterification of carboxylic acids with methanol. ScienceAsia. 2024; 50S(1): 1. doi: 10.2306/scienceasia1513-1874.2024.s002
18. Nuntang S, et al. Development of highly effective sulfonic acid–functionalized NR/MS nanocomposites for biodiesel production. Applied Environmental Research. 2025, 47(2). Available online: https://digital.car.chula.ac.th/aer/vol47/iss2/10/
19. Chaowamalee S, Yan N, Ngamcharussrivichai C. Propylsulfonic Acid-Functionalized Mesostructured Natural Rubber/Silica Nanocomposites as Promising Hydrophobic Solid Catalysts for Alkyl Levulinate Synthesis. Nanomaterials. 2022; 12(4): 604. doi: 10.3390/nano12040604
20. Thommes M. Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report). Chemistry International. 2016; 38(1): 25–25. doi: 10.1515/ci-2016-0119
21. Dong Z, Chen W, Xu K, et al. Understanding the Structure–Activity Relationships in Catalytic Conversion of Polyolefin Plastics by Zeolite-Based Catalysts: A Critical Review. ACS Catalysis. 2022; 12(24): 14882–14901. doi: 10.1021/acscatal.2c04915
22. Rouquerol F, et al. Adsorption by Powders and Porous Solids. Academic Press; 2021. Available online: http://www.cailiaoniu.com/wp-content/uploads/2016/12/Adsorption-by-Powders-and-Porous-Solids.pdf
23. Tan X, Sudarsanam P, Tan J, et al. Sulfonic acid-functionalized heterogeneous catalytic materials for efficient biodiesel production: A review. Journal of Environmental Chemical Engineering. 2021; 9(1): 104719. doi: 10.1016/j.jece.2020.104719
24. Lokman IM, Rashid U, Taufiq-Yap YH, et al. Methyl ester production from palm fatty acid distillate using sulfonated glucose-derived acid catalyst. Renewable Energy. 2015; 81: 347–354. doi: 10.1016/j.renene.2015.03.045
25. Peixoto AF, Soliman MMA, Pinto TV, et al. Highly active organosulfonic aryl-silica nanoparticles as efficient catalysts for biomass derived biodiesel and fuel additives. Biomass and Bioenergy. 2021; 145: 105936. doi: 10.1016/j.biombioe.2020.105936
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