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Hydrothermal Saline Promoted Grafting of Periodic Mesoporous Organic Sulfonic Acid Silicas for Sustainable FAME Production


Hydrothermal saline promoted grafting of sulfonic acid groups onto SBA-15 and periodic mesoporous organic silica analogues affords solid acid catalysts with high acid site loadings (>2.5 mmol g−1 H+), ordered mesoporosity and tunable hydrophobicity. The resulting catalysts show excellent activity for fatty acid esterification and tripalmitin transesterification to methyl palmitate, with framework phenyl groups promoting fatty acid methyl esters production.

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  1. Asefa T, MacLachlan MJ, Coombs N, Ozin GA (1999) Nature 402: 867. doi:

  2. Su F, Guo Y (2014) Green Chem 16:2934. doi:10.1039/c3gc42333f

    Article  CAS  Google Scholar 

  3. Melero JA, Iglesias J, Morales G (2009) Green Chem 11:1285. doi:10.1039/b902086a

    Article  CAS  Google Scholar 

  4. Dacquin JP, Lee AF, Pirez C, Wilson K (2012) Chem Commun 48:212. doi:10.1039/c1cc14563k

    Article  CAS  Google Scholar 

  5. Pirez C, Caderon J-M, Dacquin J-P, Lee AF, Wilson K (2012) ACS Catalysis 2:1607. doi:10.1021/cs300161a

    Article  CAS  Google Scholar 

  6. Dhainaut J, Dacquin J-P, Lee AF, Wilson K (2010) Green Chem 12:296. doi:10.1039/b919341c

    Article  CAS  Google Scholar 

  7. Mbaraka IK, Shanks BH (2005) J Catal 229:365. doi:

  8. Melero JA, Bautista LF, Morales G, Iglesias J, Sánchez-Vázquez R (2010) Chem Eng J 161:323. doi:

  9. Dacquin J-P, Cross HE, Brown DR, Duren T, Williams JJ, Lee AF, Wilson K (2010) Green Chem 12:1383. doi:10.1039/C0GC00045K

    Article  CAS  Google Scholar 

  10. Inagaki S, Guan S, Ohsuna T, Terasaki O (2002) Nature 416: 304. doi:

  11. Inagaki S, Guan S, Fukushima Y, Ohsuna T, Terasaki O (1999) J Am Chem Soc 121:9611. doi:10.1021/ja9916658

    Article  CAS  Google Scholar 

  12. Melde BJ, Holland BT, Blanford CF, Stein A (1999) Chem Mater 11:3302. doi:10.1021/cm9903935

    Article  CAS  Google Scholar 

  13. Hunks WJ, Ozin GA (2005) J Mater Chem 15:3716. doi:10.1039/b504511h

    Article  CAS  Google Scholar 

  14. Van Der Voort P, Esquivel D, De Canck E, Goethals F, Van Driessche I, Romero-Salguero FJ (2013) Chem Soc Rev 42:3913. doi:10.1039/c2cs35222b

    Article  Google Scholar 

  15. Park SS, Moorthy MS, Ha C-S (2014) NPG Asia Mater 6:e96. doi:10.1038/am.2014.13

  16. Mizoshita N, Tani T, Inagaki S (2011) Chem Soc Rev 40:789. doi:10.1039/C0CS00010H

  17. Yang Q, Liu J, Yang J, Kapoor MP, Inagaki S, Li C (2004) J Catal 228:265. doi:10.1016/j.jcat.2004.09.007

    Article  CAS  Google Scholar 

  18. Morales G, Athens G, Chmelka BF, van Grieken R, Melero JA (2008) J Catal 254:205. doi:10.1016/j.jcat.2007.12.011

    Article  CAS  Google Scholar 

  19. Pirez C, Lee AF, Jones C, Wilson K (2014) Catal Today 234:167. doi:10.1016/j.cattod.2014.01.042

    Article  CAS  Google Scholar 

  20. Pirez C, Lee AF, Manayil JC, Parlett CMA, Wilson K (2014) Green Chem 16:4506. doi:10.1039/c4gc01139b

    Article  CAS  Google Scholar 

  21. Esquivel D, Jiménez-Sanchidrián C, Romero-Salguero FJ (2011) Mater Lett 65:1460. doi:10.1016/j.matlet.2011.02.037

    Article  CAS  Google Scholar 

  22. Smeulders G, Meynen V, Silvestre-Albero A, Houthoofd K, Mertens M, Silvestre-Albero J, Martens JA, Cool P (2012) Mater Chem Phys 132:1077. doi:10.1016/j.matchemphys.2011.12.072

    Article  CAS  Google Scholar 

  23. Sánchez-Vázquez R, Pirez C, Iglesias J, Wilson K, Lee AF, Melero JA (2013) ChemCatChem 5:994. doi:10.1002/cctc.201200527

    Article  Google Scholar 

  24. Esquivel D, Jimenez-Sanchidrian C, Romero-Salguero FJ (2011) J Mater Chem 21:724. doi:10.1039/c0jm02980g

    Article  CAS  Google Scholar 

  25. Hao N, Wang H, Webley PA, Zhao D (2010) Microporous Mesoporous Mater 132:543. doi:10.1016/j.micromeso.2010.04.008

    Article  CAS  Google Scholar 

  26. Ide M, El-Roz M, De Canck E, Vicente A, Planckaert T, Bogaerts T, Van Driessche I, Lynen F, Van Speybroeck V, Thybault-Starzyk F, Van Der Voort P (2013) Phys Chem Chem Phys 15:642. doi:10.1039/C2CP42811C

    Article  CAS  Google Scholar 

  27. Duan X, Liu Y, Zhao Q, Wang X, Li S (2013) RSC Adv 3:13748. doi:10.1039/C3RA40219C

    Article  CAS  Google Scholar 

  28. López DE, Goodwin JG Jr, Bruce DA (2007) J Catal 245:381. doi:10.1016/j.jcat.2006.10.027

    Article  Google Scholar 

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We thank the EPSRC (EP/K000616/1, EP/F063423/1 and EP/G007594/3) for financial support and a Leadership Fellowship (AFL), and the Royal Society for the award of an Industry Fellowship (KW). We also acknowledge the kind assistance of D.C. Apperley at the EPSRC UK National Solid-state NMR Service at Durham. VCS acknowledges CNPq (Conselho Nacional de Desenvolvimento Cientifico e Tecnológico) for the award of a postdoctoral scholarship.

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Correspondence to K. Wilson.

Electronic supplementary material

Below is the link to the electronic supplementary material. Electronic Supplementary Information (ESI) available: [porosimetry data, XRD, XPS, MAS-NMR, TGA, DRIFT spectra and FFA esterification reaction profiles]. See DOI: 10.1039/c000000x/

Supplementary material 1 (DOCX 1505 kb)

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Pirez, C., Reche, M.T., Lee, A.F. et al. Hydrothermal Saline Promoted Grafting of Periodic Mesoporous Organic Sulfonic Acid Silicas for Sustainable FAME Production. Catal Lett 145, 1483–1490 (2015).

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  • Heterogeneous catalysis
  • Biodiesel
  • Sulfonic acid
  • Solid acid
  • Esterification
  • Transesterification
  • Mesoporous materials