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Organic acid-assisted soft-templating synthesis of ordered mesoporous carbons

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Abstract

A series of soft-templated ordered mesoporous carbons (OMCs) was synthesized by using resorcinol and formaldehyde as carbon precursors, triblock copolymer Pluronic F127 as a soft-template, and an organic acid (acetic, benzoic, citric, oxalic, or succinic) as a polymerization reaction catalyst. The aforementioned organic acids were strong enough to facilitate the formation of ordered mesophases by the block copolymer template used and to catalyze the polymerization reaction of resorcinol and formaldehyde in this template. The use of weak organic acids instead of strong inorganic acids such as HCl eliminated inorganic anions from the reaction environment and resulted in high surface area OMCs. Basically, the resulting carbons showed the surface areas and pore volumes comparable to those reported for the carbons prepared under similar conditions but in the presence of strong inorganic acids. Electron microscopy analysis proved the presence of ordered mesopores, whereas thermogravimetric analysis showed a good thermal stability of these carbons.

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References

  • Brunauer, S., Emmett, P.H., Teller, E.: Adsorption of gases in multimolecular layers. J. Am. Chem. Soc. 60, 309–319 (1938)

    Article  CAS  Google Scholar 

  • Chai, G.S., Yoon, S.B., Kim, J.H., Yu, J.-S.: Spherical carbon capsules with hollow macroporous core and mesoporous shell structures as a highly efficient catalyst support in the direct methanol fuel cell. Chem. Commun. 23, 2766–2767 (2004)

    Article  Google Scholar 

  • Choma, J., Jaroniec, M., Kloske, M.: Improved pore-size analysis of carbonaceous adsorbents. Adsorption Sci. Technol. 20, 307–315 (2002)

    Article  CAS  Google Scholar 

  • Choma, J., Jedynak, K., Jamioła, D., Jaroniec, M.: Influence of carbonization temperature on the adsorption and structural properties of mesoporous carbons obtained by soft templating (in Polish). Ochrona Srodowiska (Poland) 34–2, 3–8 (2012)

    Google Scholar 

  • Choma, J., Zubrowska, A., Gorka, J., Jaroniec, M.: Adsorption properties of phenolic resin-based mesoporous carbons obtained by using mixed templates of Pluronic F127 and Brij 58 or Brij 78 polymers. Adsorption 16, 377–383 (2010)

    Article  CAS  Google Scholar 

  • Gorka, J. (Jaroniec, M—advisor): Polymer-based mesoporous carbons: soft-templating synthesis, adsorption and structural properties. Dissertation, Kent State University (2010)

  • Gorka, J., Fenning, C., Jaroniec, M.: Influence of temperature, carbon precursor/copolymer ratio and acid concentration on adsorption and structural properties of mesoporous carbons prepared by soft-templating. Coll. Surf. A 352, 113–117 (2009)

    Article  CAS  Google Scholar 

  • Grant, S.M., Jaroniec, M.: Effect of acid concentration on pore size in polymer-templated mesoporous alumina. J. Mater. Chem. 22, 86–92 (2012)

    Article  CAS  Google Scholar 

  • Gregg, S.J., Sing, K.S.W.: Adsorption, surface area and porosity, 2nd edn. Academic Press, London (1982)

    Google Scholar 

  • Han, S., Hyeon, T.: Simple silica particle template synthesis of mesoporous carbons. Chem. Commun. 19, 1955–1956 (1999)

    Article  Google Scholar 

  • Joo, S.H., Choi, S.J., Oh, I., Kwak, J., Liu, Z., Terasaki, O., Ryoo, R.: Ordered nanoporous arrays of carbon supporting high dispersions of platinum nanoparticles. Nature 412, 169–172 (2001)

    Article  CAS  Google Scholar 

  • Jaroniec, M., Choma, J., Gorka, J., Zawislak, A.: Colloidal silica templating synthesis of carbonaceous monoliths assuring formation of uniform spherical mesopores and incorporation of inorganic nanoparticles. Chem. Mater. 20, 1069–1075 (2008)

    Article  CAS  Google Scholar 

  • Jaroniec, M., Gorka, J., Choma, J., Zawislak, A.: Synthesis and properties of mesoporous carbons with high loadings of inorganic species. Carbon 47, 3034–3040 (2009)

    Article  CAS  Google Scholar 

  • Jaroniec, M., Madey, R., Choma, J., McEnaney, B., Mays, T.J.: Comparison of adsorption methods for characterizing the microporosity of activated carbons. Carbon 27, 77–83 (1989)

    Article  Google Scholar 

  • Jun, S., Joo, S.H., Ryoo, R., Kruk, M., Jaroniec, M., Liu, Z., Ohsuna, T., Terasaki, O.: Synthesis of new, nanoporous carbon with hexagonally ordered nanostructure. J. Am. Chem. Soc. 122, 10712–10713 (2000)

    Article  CAS  Google Scholar 

  • Kalbour, H., Baumann, T.F., Satcher, J.H., Saulnier, A., Ahn, C.C.: Toward new candidates for hydrogen storage: high-surface area carbon aerogels. Chem. Mater. 18, 6085–6087 (2006)

    Article  Google Scholar 

  • Kruk, M., Jaroniec, M., Gadkaree, K.P.: Nitrogen adsorption studies of novel synthetic active carbons. J. Coll. Interface Sci. 192, 250–256 (1997a)

    Article  CAS  Google Scholar 

  • Kruk, M., Jaroniec, M., Sayari, A.: Application of large pore MCM-41 molecular sieves to improve pore size analysis using nitrogen adsorption measurements. Langmuir 13, 6267–6273 (1997b)

    Article  CAS  Google Scholar 

  • Lee, J., Han, S., Hyeon, T.: Synthesis of new nanoporous materials using nanostructured silica materials as templates. J. Mater. Chem. 14, 478–486 (2004)

    Article  CAS  Google Scholar 

  • Li, Z., Jaroniec, M.: Colloidal imprinting: a novel approach to the synthesis of mesoporous carbons. J. Am. Chem. Soc. 123, 9208–9209 (2001)

    Article  CAS  Google Scholar 

  • Liang, C., Dai, S.: Synthesis of mesoporous carbon materials via enhanced hydrogen-bonding interaction. J. Am. Chem. Soc. 128, 5316–5317 (2006)

    Article  CAS  Google Scholar 

  • Liang, C., Dai, S., Guiochon, G.: A graphitized-carbon monolithe column. Anal. Chem. 75, 4904–4912 (2003)

    Article  CAS  Google Scholar 

  • Liu, L., Deng, Q.F., Ma, T.Y., Lin, X.Z., Hou, X.X., Liu, Y.P., Yuan, Z.Y.: Ordered mesoporous carbons: citric acid—catalyzed synthesis, nitrogen doping and CO2 capture. J. Mater. Chem. 21, 16001–16009 (2011)

    Article  CAS  Google Scholar 

  • Lu, A.H., Spliethoff, B., Schuth, F.: Aqueous synthesis of ordered mesoporous carbon via self-assembly catalyzed by amino acid. Chem. Mater. 20, 5314–5319 (2008)

    Article  CAS  Google Scholar 

  • Meng, Y., Gu, D., Zhang, F., Shi, Y., Cheng, L., Feng, D., Wu, Z., Chen, Z., Wan, Y., Stein, A., Zhao, D.: A family of highly ordered mesoporous polymer resin and carbon structures from organic–organic self-assembly. Chem. Mater. 18, 4447–4464 (2006)

    Article  CAS  Google Scholar 

  • Meng, Y., Gu, D., Zhang, F., Shi, Y., Yang, H., Li, Z., Yu, C., Tu, B., Zhao, D.: Ordered mesoporous polymers and homologous carbon frameworks: amphiphilic surfactant templating and direct transformation. Angew. Chem. Int. Ed. 44, 7053–7059 (2005)

    Article  CAS  Google Scholar 

  • Ryoo, R., Joo, S.H., Jun, S.: Synthesis of highly ordered carbon molecular sieves via template-mediated structural transformation. J. Phys. Chem. B 103, 7743–7746 (1999)

    Article  CAS  Google Scholar 

  • Ryoo, R., Joo, S.H., Kruk, M., Jaroniec, M.: Ordered mesoporous carbons. Adv. Mater. 13, 677–681 (2001)

    Article  CAS  Google Scholar 

  • Sing, K.S.W., Everett, D.H., Haul, R.A.W., Moscou, L., Pierotti, R.A., Rouquerol, J., Siemieniewska, T.: Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity. Pure Appl. Chem. 57, 603–619 (1985)

    Article  CAS  Google Scholar 

  • Wang, X., Liang, C., Dai, S.: Facile synthesis of ordered mesoporous carbons with high thermal stability by self-assembly of resorcinol–formaldehyde and block copolymers under highly acidic conditions. Langmuir 24, 7500–7505 (2008)

    Article  CAS  Google Scholar 

  • Yoon, S.B., Chai, G.S., Kang, S.K., Yu, J.S., Gierszal, K.P., Jaroniec, M.: Graphitized pitch-based carbons with ordered nanopores synthesized by using colloidal crystals as templates. J. Am. Chem. Soc. 127, 4188–4189 (2005)

    Article  CAS  Google Scholar 

  • Zakhidov, A.A., Baughaman, R.H., Iqbal, Z., Cui, C., Khayrullin, I., Dantas, S.O., Marti, J., Ralchenko, V.G.: Carbon structures with three-dimensional periodicity at optical wavelengths. Science 282, 897–901 (1998)

    Article  CAS  Google Scholar 

  • Zhang, F., Meng, Y., Gu, D., Yan, Y., Yu, C., Tu, B., Zhao, D.: A facile aqueous route to synthesize highly ordered mesoporous polymers and carbon frameworks with Ia3d bicontinuous cubic structure. J. Am. Chem. Soc. 127, 13508–13509 (2005)

    Article  CAS  Google Scholar 

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Acknowledgments

MJ acknowledges the National Science Foundation for support of this research under CHE-0848352 grant. JC acknowledges the National Science Centre for support of this research under Grant UMO 2011/03/N/ST5/04444. KJ acknowledges the Ministry of Science and Higher Education (Poland) for support of this research under Grant BS 038/2012. KJ—is a fellow under the program “Scholarships for Graduate Students of Majors Relevant to Regional Development” founded through Humane Capital Operational Program. The TEM data were recorded using the (cryo) TEM facility at the Liquid Crystal Institute, Kent State University, supported by the Ohio Research Scholars Program.

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Correspondence to Mietek Jaroniec.

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Choma, J., Jedynak, K., Marszewski, M. et al. Organic acid-assisted soft-templating synthesis of ordered mesoporous carbons. Adsorption 19, 563–569 (2013). https://doi.org/10.1007/s10450-013-9479-6

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