Graphitization of Coconut Shell Charcoal for Sulfonated Mesoporous Carbon Catalyst Preparation and Its Catalytic Behavior in Esterification Reaction

Fahmi Fahmi  -  Department of Chemical Engineering, Institut Teknologi Sepuluh Nopember, Indonesia
Widiyastuti Widiyastuti orcid scopus  -  Department of Chemical Engineering, Institut Teknologi Sepuluh Nopember, Indonesia
*Heru Setyawan orcid scopus  -  Department of Chemical Engineering, Institut Teknologi Sepuluh Nopember, Indonesia
Received: 7 May 2020; Revised: 25 Jun 2020; Accepted: 26 Jun 2020; Published: 1 Aug 2020; Available online: 15 Jul 2020.
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Section: Original Research Articles
Language: EN
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Here, we reported the utilization of coconut shell charcoal used for solid acid catalysts and its performance in the esterification reaction of acetic acid and methanol. The graphitization of coconut shell charcoal was carried out by the calcination and KOH activation at the temperature of 400 °C for an hour and continued at the temperature of 800 °C for an hour under nitrogen flow resulted in graphitic carbon. The effect of the addition of KOH activation was observed by varied the weight ratio of coconut shell charcoal as raw material (RM) and KOH. The selected weight ratio of RM:KOH was 1:1, 1:2, and 1:4. The resulted graphitic carbon was sulfonated by heating with the sulfuric acid to obtain a solid acid catalyst. The sulfonic time was evaluated for 5 and 10 hours. The generated particles were characterized to examine the morphology, the crystallinity, the specific surface area, the chemical bonding, and the ionic capacity using Scanning Electron Microscopy (SEM), X-Ray diffraction (XRD), nitrogen gas absorption-desorption, Fourier Transform Infrared Spectroscopy (FTIR), and titration method, respectively. The best condition for graphitization of raw material is the use of RM:KOH = 1:4, resulting in the highest surface area reaching 1259.67 m2/g and the most dominant of the sulfonic group of −SO3 bond. Furthermore, increasing the sulfonating time from 5 to 10 hours led to the increase of the yield of esterification reaction from 85% to 96.57% for graphite synthesized using RM:KOH = 1:4. Copyright © 2020 BCREC Group. All rights reserved


Keywords: Solid Acid Catalyst; Sulfonating Time; Esterification; Graphitic Carbon; Ionic Capacity

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  1. Jagadeeshbabu, P.E., Sandesh, K., Saidutta, M.B. (2011). Kinetics of esterification of acetic acid with methanol in the presence of ion exchange resin catalysts. Industrial and Engineering Chemistry Research, 50(12), 7155–7160. DOI: 10.1021/ie101755r
  2. Yu, W., Hidajat, K., Ray, A.K. (2004). Determination of adsorption and kinetic parameters for methyl acetate esterification and hydrolysis reaction catalyzed by Amberlyst 15. Applied Catalysis A: General, 260(2), 191–205. DOI: 10.1016/j.apcata.2003.10.017
  3. Mekala, M., Goli, V.R. (2015). Kinetics of esterification of methanol and acetic acid with mineral homogeneous acid catalyst. Chinese Journal of Chemical Engineering, 23(1), 100–105. DOI: 10.1016/j.cjche.2013.08.002
  4. Tang, Z.E., Lim, S., Pang, Y.L., Ong, H.C., Lee, K.T. (2018). Synthesis of biomass as heterogeneous catalyst for application in biodiesel production: State of the art and fundamental review. Renewable and Sustainable Energy Reviews, 92, 235–253. DOI: 10.1016/j.rser.2018.04.056
  5. Borges, M.E., Díaz, L. (2012). Recent developments on heterogeneous catalysts for biodiesel production by oil esterification and transesterification reactions: A review. Renewable and Sustainable Energy Reviews, 16(5), 2839–2849. DOI: 10.1016/j.rser.2012.01.071
  6. Soltani, S., Rashid, U., Yunus, R., Taufiq-Yap, Y.H., Al-Resayes, S.I. (2016). Post-functionalization of polymeric mesoporous C@Zn core–shell spheres used for methyl ester production. Renewable Energy, 99, 1235–1243. DOI: 10.1016/j.renene.2016.08.025
  7. Liu, Y., Lotero, E., Goodwin, J.G. (2006). A comparison of the esterification of acetic acid with methanol using heterogeneous versus homogeneous acid catalysis. Journal of Catalysis, 242(2), 278–286. DOI: 10.1016/j.jcat.2006.05.026
  8. Peters, T.A., Benes, N.E., Holmen, A., Keurentjes, J.T.F. (2006). Comparison of commercial solid acid catalysts for the esterification of acetic acid with butanol. Applied Catalysis A: General, 297(2), 182–188. DOI: 10.1016/j.apcata.2005.09.006
  9. Tsai, Y.T., Lin, H.M., Lee, M.J. (2011). Kinetics behavior of esterification of acetic acid with methanol over Amberlyst 36. Chemical Engineering Journal, 171(3), 1367–1372. DOI: 10.1016/j.cej.2011.05.049
  10. Geng, L., Yu, G., Wang, Y., Zhu, Y. (2012). Ph-SO 3 H-modified mesoporous carbon as an efficient catalyst for the esterification of oleic acid. Applied Catalysis A: General, 427–428, 137–144. DOI: 10.1016/j.apcata.2012.03.044
  11. Geng, L., Wang, Y., Yu, G., Zhu, Y. (2011). Efficient carbon-based solid acid catalysts for the esterification of oleic acid. Catalysis Communications, 13(1), 26–30. DOI: 10.1016/j.catcom.2011.06.014
  12. Guliani, D., Kaur, K., Singh, N., Sobti, A., Toor, A.P. (2019). Catalytic performance of sulfate-grafted graphene oxide for esterification of acetic acid with methanol. Chemical Engineering Communications, 206(5), 592–604. DOI: 10.1080/00986445.2018.1514601
  13. Cheng, J., Qiu, Y., Huang, R., Yang, W., Zhou, J., Cen, K. (2016). Biodiesel production from wet microalgae by using graphene oxide as solid acid catalyst. Bioresource Technology, 221, 344–349. DOI: 10.1016/j.biortech.2016.09.064
  14. Allahresani, A., Nasseri, M.A., Akbari, A., Nasab, B.Z. (2015). Graphene oxide based solid acid as an efficient and reusable nano-catalyst for the green synthesis of diindolyl-oxindole derivatives in aqueous media. Reaction Kinetics, Mechanisms and Catalysis, 116(1), 249–259. DOI: 10.1007/s11144-015-0883-7
  15. Chen, C.L., Huang, C.C., Ho, K.C., Hsiao, P.X., Wu, M.S., Chang, J.S. (2015). Biodiesel production from wet microalgae feedstock using sequential wet extraction/transesterification and direct transesterification processes. Bioresource Technology, 194, 179–186. DOI: 10.1016/j.biortech.2015.07.021
  16. Na, S., Minhua, Z., Xiuqin, D., Lingtao, W. (2019). Preparation of sulfonated ordered mesoporous carbon catalyst and its catalytic performance for esterification of free fatty acids in waste cooking oils. RSC Advances, 9(28), 15941–15948. DOI: 10.1039/c9ra02546d
  17. Nata, I.F., Putra, M.D., Irawan, C., Lee, C.K. (2017). Catalytic performance of sulfonated carbon-based solid acid catalyst on esterification of waste cooking oil for biodiesel production. Journal of Environmental Chemical Engineering, 5(3), 2171–2175. DOI: 10.1016/j.jece.2017.04.029
  18. Yang, L., Yuan, H., Wang, S. (2019). Preparation and application of ordered mesoporous carbon-based solid acid catalysts for transesterification and epoxidation. Journal of Porous Materials, 26(5), 1435–1445. DOI: 10.1007/s10934-019-00742-w
  19. Chen, G., Fang, B. (2011). Preparation of solid acid catalyst from glucose-starch mixture for biodiesel production. Bioresource Technology, 102(3), 2635–2640. DOI: 10.1016/j.biortech.2010.10.099
  20. Fu, X.B., Chen, J., Song, X.L., Zhang, Y M., Zhu, Y., Yang, J., Zhang, C.W. (2015). Biodiesel production using a carbon solid acid catalyst derived from β-cyclodextrin. JAOCS, Journal of the American Oil Chemists’ Society, 92(4), 495–502. DOI: 10.1007/s11746-015-2621-8
  21. Janaun, J.A., Mey, T.J., Bono, A., Krishnaiah, D. (2017). Preparation and characterization of sugar based catalyst on various supports. Bulletin of Chemical Reaction Engineering & Catalysis, 12(1), 41–48. DOI: 10.9767/bcrec.12.1.478.41-48
  22. Zeng, D., Zhang, Q., Chen, S., Liu, S., Wang, G. (2016). Synthesis porous carbon-based solid acid from rice husk for esterification of fatty acids. Microporous and Mesoporous Materials, 219, 54–58. DOI: 10.1016/j.micromeso.2015.07.028
  23. Song, X.L., Fu, X.B., Zhang, C.W., Huang, W.Y., Zhu, Y., Yang, J., Zhang, Y.M. (2012). Preparation of a novel carbon based solid acid catalyst for biodiesel production via a sustainable route. Catalysis Letters, 142(7), 869–874. DOI: 10.1007/s10562-012-0840-2
  24. Yu, H., Niu, S., Lu, C., Li, J., Yang, Y. (2016). Preparation and esterification performance of sulfonated coal-based heterogeneous acid catalyst for methyl oleate production. Energy Conversion and Management, 126, 488–496. DOI: 10.1016/j.enconman.2016.08.036
  25. Fraga, A.C., Quitete, C.P.B., Ximenes, V.L., Sousa-Aguiar, E.F., Fonseca, I.M., Rego, A.M.B. (2016). Biomass derived solid acids as effective hydrolysis catalysts. Journal of Molecular Catalysis A: Chemical, 422, 248–257. DOI: 10.1016/j.molcata.2015.12.005

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