Skip to main content
Log in

Effect of microwave irradiation on the structural, chemical, and hydrophilicity characteristics of ordered mesoporous silica SBA-15

  • Original Paper: Sol-gel, hybrids and solution chemistries
  • Published:
Journal of Sol-Gel Science and Technology Aims and scope Submit manuscript

Abstract

Structural, chemical, morphological, and hydrophilic surface characteristics of SBA-15 silica synthesized by hydrothermal method in an autoclave and in a microwave-heated reactor were analyzed in this work. The influence of time and temperature on these characteristics was investigated. Materials were characterized by textural analysis (BET), FTIR, TGA, XRD, goniometer contact angle, SEM, and TEM. It was possible to obtain SBA-15 silicas assisted by microwave heating irradiation with short-time synthesis (0.5–8 h) compared with the hydrothermal classic method (24 h). Materials presented surface area between 650 and 850 m2 g−1. Through the XRD and TEM results, it was observed that mesostructured materials with two-dimensional, long-range, and hexagonal ordered channels are characteristic of SBA-15. This study showed that heating by microwave irradiation during silica synthesis generates materials with a greater amount of silanol groups. It is possible to control the surface properties of SBA-15 during the microwave-assisted synthesis through temperature tuning. Higher temperature provided SBA-15 with higher hydrophilicity.

Highlights

  • SBA-15 synthesis by MW reduces significant reaction time.

  • SBA-15 synthesized in MW at 80 °C showed 805 m2 g−1 of specific surface area.

  • Heating by MW in the silica synthesis generates materials with higher hydrophilicity.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9

Similar content being viewed by others

References

  1. Toufaily J, Soulard M, Guth JL, Patarin J, Delmote L, Hamieha T, Kodeih M, Naoufal D, Hamad H (2008) Synthesis and characterization of new catalysts formed by direct incorporation of heteropolyacids into organized mesoporous silica. Coll Surf A Physicochem Eng Asp 316:285–291

    Article  CAS  Google Scholar 

  2. Zhang X, Huang N, Wang G, Donf W, Yang M, Luan Y, Shi Z (2013) Synthesis of highly loaded and well dispersed CuO/SBA-15 via an ultrasonic post-grafting method and its application as a catalyst for the direct hydroxylation of benzene to phenol. Micro Mesopor Mater 177:47–53

    Article  CAS  Google Scholar 

  3. Park M, Park SS, Selvaraj M, Zhao D, Há CS (2009) Hydrophobic mesoporous materials for immobilization of enzymes. Micro Mesopor Mater 124:76–83

    Article  CAS  Google Scholar 

  4. Marczewska AD, Zienkiewicz-Strzalka M, Skrzypczynska K, Swiatkowski A, Kusmierek K (2016) Evaluation of the SBA-15 materials ability to accumulation of 4-chlorophenol on carbon paste electrode. Adsorption 22:801–812

    Article  CAS  Google Scholar 

  5. Zhao Y, Xu Y, Wu D, Wei W, Sun Y, Al-Arifi ASN, Aouak T, Al-Othman ZA (2010) Hydrophobic mesoporous silica applied in GC separation of hexene isomers J Sol-Gel Sci Technol 56:93–98

    Article  CAS  Google Scholar 

  6. Izquierdo-Barba I, Sousa E, Doadrio JC, Doadrio AL, Pariente JP, Martınez A, Babonneau F, Vallet-Regı M (2009) Influence of mesoporous structure type on the controlled delivery of drugs: release of ibuprofen from MCM-48, SBA-15 and functionalized SBA-15. J Sol-Gel Sci Technol 50:421–429

    Article  CAS  Google Scholar 

  7. Oliveira MR, Oliveira MM, Oliveira RJ, Dervanoski A, Franceschi E, Egues SM, De Conto JF (2019) Amine-modified silica surface applied as adsorbent in the phenol adsorption assisted by ultrasound. Chem Eng Commun 206:1565–1580

    CAS  Google Scholar 

  8. Beck JS, Vartuli JC, Roth WJ, Leonowicz ME, Kresge CT, Schmitt KD, Chu CTW, Olson DH, Sheppard EW, McCullen SB, Higgins JB, Schlenker JL (1992) A new family of mesoporous molecular sieves prepared with liquid crystal templates. J Am Chem Soc 114:10834–10843

    Article  CAS  Google Scholar 

  9. Chen CY, Li HX, Davis ME (1993) Studies on mesoporous materials. Microporous Mater 2:17–26

    Article  Google Scholar 

  10. Zhao DY, Feng JL, Huo QS, Melosh N, Fredrickson GH, Chmelka BF, Stucky GD (1998) Triblock copolymer syntheses of mesoporous silica with periodic 50 to 300 Angstrom pores. Science 279:548–552

    Article  CAS  Google Scholar 

  11. Huo Q, Leon R, Petroff PM, Stucky GD (1995) Mesostructure design with gemini surfactants: supercage formation in a three-dimensional hexagonal array. Science 268:1324–1327

    Article  CAS  Google Scholar 

  12. Tanev PT, Pinnavaia TJ (1995) A neutral templating route to mesoporous molecular sieves. Science 267:865–867

    Article  CAS  Google Scholar 

  13. Bagshaw SA, Prouzet E, Pinnavaia TJ (1995) Templating of mesoporous molecular sieves by nonionic polyethylene oxide surfactants. Science 269:1242–1244

    Article  Google Scholar 

  14. Galarneau A, Cambon H, Di Renzo F, Ryoo R, Choi M, Fajula F (2003) Microporosity and connections between pores in SBA-15 mesostructured silicas as a function of the temperature of synthesis. N. J Chem 27:73–79

    Article  CAS  Google Scholar 

  15. Szczodrowski K, Prélot B, Lantenois S, Douillard JM, Zajac J (2009) Effect of heteroatom doping on surface acidity and hydrophilicity of Al, Ti, Zr-doped mesoporous SBA-15. Micro Mesopor Mater 124:84–93

    Article  CAS  Google Scholar 

  16. Meléndez-Ortiz HI, Puente-Urbina B, Castruita-De LG, Mata-Padilla JM, García-Uriostegui L (2016) Synthesis of spherical SBA-15 mesoporous silica. Influence of reaction conditions on the structural order and stability. Ceram Int 42:7564–7570

    Article  CAS  Google Scholar 

  17. Zhang Z, Wang F, Nie H, Zhou T, Zhang G, Wang X, Cui M, Li Y (2017) A simple strategy for the synthesis of Zn-IL-SBA-15 by sol–gel and the application in desulfurization J Sol-Gel Sci Technol 82:827–833

    Article  CAS  Google Scholar 

  18. Dan H, Dong X, Lu X, Ding Y (2017) Facile route to synthesize mesoporous SBA-15 rods with different sizes for lysozyme immobilization. J Sol-Gel Sci Technol 81:782–790

    Article  CAS  Google Scholar 

  19. Parambadath S, Mathew A, Barnabas MJ, Kim SY, Ha CS (2016) Concentration-dependant selective removal of Cr(III), Pb(II) and Zn(II) from aqueous mixtures using 5-methyl-2-thiophenecarboxaldehyde Schiff base-immobilised SBA-15. J Sol-Gel Sci Technol 79:426–439

    Article  CAS  Google Scholar 

  20. Chaudhary V, Sharma S (2017) An overview of ordered mesoporous material SBA-15: synthesis, functionalization and application in oxidation reactions. J Porous Mater 24:741–749

    Article  CAS  Google Scholar 

  21. Zhao D, Huo Q, Feng J, Chmelka BF, Stucky GD (1998) Nonionic triblock and star diblock copolymer and oligomeric surfactant syntheses of highly ordered, hydrothermally stable, mesoporous silica structures. J Am Chem Soc 120:6024–6036

    Article  CAS  Google Scholar 

  22. Benamor T, Vidal L, Lebeau B, Marichal C (2012) Influence of synthesis parameters on the physico-chemical characteristics of SBA-15 type ordered mesoporous sílica. Micro Mesopor Mater 153:100–114

    Article  CAS  Google Scholar 

  23. Mily E, González A, Iruin JJ, Irusta L, Fernández-Berridi MJ (2010) Silica nanoparticles obtained by microwave assisted sol–gel process: multivariate analysis of the size and conversion dependence. J Sol-Gel Sci Technol 53:667–672

    Article  CAS  Google Scholar 

  24. De Conto JF, Oliveira MR, Oliveira MM, Brandão TG, Campos KV, Santana CC, Egues SM (2018) One-pot synthesis and modification of silica nanoparticles with 3-chloropropyltrimethoxysilane assisted by microwave irradiation. Chem Eng Commun 205:533–537

    Article  CAS  Google Scholar 

  25. Peres EC, Slaviero JC, Cunha AM, Hosseini–Bandegharaei A, Dotto GL (2018) Microwave synthesis of silica nanoparticles and its application for methylene blue adsorption. J Environ Chem Eng 6:649–659

    Article  CAS  Google Scholar 

  26. Oliveira RJ, De Conto JF, Oliveira MR, Egues SMS, Borges GR, Dariva C, Franceschi E(2019) CO2/CH4 adsorption at high-pressure using silica-APTES aerogel as adsorbent and near infrared as a monitoring technique J CO2 Util 32:232–240

    Article  CAS  Google Scholar 

  27. Bilecka I, Niederberger M (2010) Microwave chemistry for inorganic nanomaterials synthesis. Nanoscale 2:1269–1528

    Article  CAS  Google Scholar 

  28. Lakhi KS, Cha WS, Choy JH, Ejji MA, Abdullah AM, Enizi AMA, Vinu A (2016) Synthesis of mesoporous carbons with controlled morphology and pore diameters from SBA-15 prepared through the microwave assisted process and their CO2 adsorption capacity. Micro Mesopor Mater 233:44–52

    Article  CAS  Google Scholar 

  29. Celer EB, Jaroniec M (2006) Temperature-programmed microwave-assisted synthesis of SBA-15 ordered mesoporous silica. J Am Chem Soc 128:14408–14414

    Article  CAS  Google Scholar 

  30. Periyat P, Leyland N, McCormack DE, Colreavy J, Corr D, Pillai SCJ (2010) Rapid microwave synthesis of mesoporous TiO2 for electrochromic displays. Mater Chem 20:3650–3655

    Article  CAS  Google Scholar 

  31. Meng LY, Wang B, Ma MG, Lin KL (2016) The progress of microwave-assisted hydrothermal method in the synthesis of functional nanomaterials. Mater Today Chem 12:63–83

    Article  Google Scholar 

  32. Tompsett GA, Conner WC, Yngvesson KS (2006) Microwave synthesis of nanoporous materials. Chem Phys Chem 7:296–319

    Article  CAS  Google Scholar 

  33. Chaignon J, Bouizi Y, Davin L, Calin N, Albela B, Bonneviot L (2015) Minute-made and low carbon fingerprint microwave synthesis of high quality templated mesoporous silica. Green Chem 17:3130–3140

    Article  CAS  Google Scholar 

  34. De Conto JF, Oliveira MR, Oliveira RJ, Campos KV, De Menezes EW, Benvenutti EV, Franceschi E, Santana CC, Egues SM (2017) Synthesis of silica modified with 1-methylimidazolium chloride by sol-gel method: a comparison between microwave radiation-assisted and conventional methods. J Non Cryst Solids 471:209–214

    Article  CAS  Google Scholar 

  35. Pirez C, Morin JC, Manayil JC, Lee AF, Wilson K (2018) Sol–gel synthesis of SBA-15: impact of HCl on surface chemistry. Micro Mesopor Mater 271:196–202

    Article  CAS  Google Scholar 

  36. Lopez RO, Hermosillo IJP, Schulz JME, Uribe AC, Domınguez-Ortiz A (2015) SBA-15 materials: calcination temperature influence on textural properties and total silanol ratio. Adsorption 21:659–669

    Article  CAS  Google Scholar 

  37. Thommes M, Kaneko K, Neimark AV, Olivier JP, Rodriguez-Reinoso F, Rouquerol KSW (2015) Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC technical report). Pure Appl Chem 87:1051–1069

    Article  CAS  Google Scholar 

  38. Neves GM, Lenza RFS, Vasconcelos WL (2002) Evaluation of the influence of microwaves in the structure of silica gels. Mater Res 5:447–451

    Article  CAS  Google Scholar 

  39. Dudarko OA, Gunathilake C, Sliesarenko VV, Zuba YL, Jaroniec M (2014) Microwave-assisted and conventional hydrothermal synthesis of ordered mesoporous silicas with P-containing functionalities. Coll Surf A Physicochem Eng Asp 459:4–10

    Article  CAS  Google Scholar 

  40. Sujandi SE, Park DS, Han SC, Han MJ, Ohsuna TJ (2006) Amino-functionalized SBA-15 type mesoporous silica having nanostructured hexagonal platelet morphology. Chem Commun 39:4131–4133

    Article  CAS  Google Scholar 

  41. Lai TL, Shu YY, Lin YC, Chen WN, Wang CB (2009) Rapid removal of organic template from SBA-15 with microwave assisted extraction. Mater Lett 63:1693–1695

    Article  CAS  Google Scholar 

  42. Slosarczyk A, Barelkowski M, Niemier S, Jakubowska P (2015) Synthesis and characterization of silica aerogel/carbon microfibers nanocompositos dried in supercritical and ambient pressure. J Sol-Gel Sci Technol 76:227–232

    Article  CAS  Google Scholar 

  43. Sareen S, Mutreja V, Singh S, Pal B (2015) Fine CuO anisotropic nanoparticles supported on mesoporous SBA-15 for selective hydrogenation of nitroaromatics. J Colloid Interface Sci 461:203–210

    Article  CAS  Google Scholar 

  44. Liang Y, Lu S, Wu D, Sun B, Xu F, Fu R (2013) Polyethylene glycol-induced self-assembly to synthesize an ordered mesoporous polymer with a two-dimensional hexagonal structure. J Mater Chem A 1:3061–3067

    Article  CAS  Google Scholar 

  45. Pu Y, Xuan K, Wang F, Li A, Zhao N, Xiao F (2018) Synthesis of dimethyl carbonate from CO2 and methanol over a hydrophobic Ce/SBA-15 catalyst. RSC Adv 8:27216–27226

    Article  CAS  Google Scholar 

  46. Ye L, Zhang Y, Songa C, Lic Y, Jiang B (2017) A simple sol–gel method to prepare superhydrophilic silica coatings. Mater Lett 188:316–318

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The authors would like to thank the LPA laboratories that are part of the Institute of Technology and Research (ITP/UNIT) and COMCAP-UEM for the availability of equipment for characterization of materials. We also thank Iago Filipe Silva de Oliveira by graphical abstract edition.

Funding

The authors thank CAPES (Coordination for the Improvement of Higher Education Personnel)—Finance Code 001, CNPq (National Council for Scientific and Technological Development), FAPITEC/SE (Foundation for Research and Technological Innovation Support of the State of Sergipe), ANP (National Agency of Petroleum, Natural Gas, and Biofuels), and PETROBRAS S.A.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Juliana F. De Conto.

Ethics declarations

Conflict of interest

The authors declare that they have no conflict of interest.

Additional information

Publisher’s note Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Supplementary information

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Oliveira, M.R., Deon, M., Benvenutti, E.V. et al. Effect of microwave irradiation on the structural, chemical, and hydrophilicity characteristics of ordered mesoporous silica SBA-15. J Sol-Gel Sci Technol 94, 708–718 (2020). https://doi.org/10.1007/s10971-020-05219-w

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10971-020-05219-w

Keywords

Navigation