Skip to main content
SpringerLink
Log in

High-temperature hydrothermal synthesis of magnetically active, ordered mesoporous resin and carbon monoliths with reusable adsorption for organic dye

  • Published:
Adsorption Aims and scope Submit manuscript

Abstract

Magnetically active, thermally stable, and ordered mesoporous resin (MOMR-200) and carbon (MOMC-200) monoliths were prepared by one-pot hydrothermal synthesis from resol, copolymer surfactant, and iron cations at high-temperature (200 ∘C), followed by calcination at 360 ∘C and carbonization at 600 ∘C. X-ray diffraction results show that both MOMR-200 and MOMC-200 have ordered hexagonal mesoporous symmetry, and N2 isotherms indicate that these samples have uniform mesopores (3.71, 3.45 nm), high surface area (328, 621 m2/g) and large pore volume (0.31, 0.43 cm3/g). Transmission electron microscopy shows that iron nanoparticles, which are superparamagnetic in nature, are dispersed in the network. More importantly, the high temperature (200 ∘C) products exhibit much better stability than the samples synthesized at low temperature (100 ∘C). Interestingly, MOMC-200 has higher adsorption capacity for organic dyes when compared with commercial adsorbents (activated carbon and macroporous resin: XAD-4). Combining the advantages such as magnetically active, thermally stable networks, ordered and open mesopores, high surface area, large pore volume, adsorption of pollutants in water and desorption in ethanol solvent, MOMC-200 is potentially important for water treatments.

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

Access this article

Log in via an institution

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

Instant access to the full article PDF.

Institutional subscriptions

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

  • Bourlinos, A.B., Simopoulos, A., Boukos, N., Petridis, D.: Magnetic modification of the external surfaces in the MCM-41 porous silica: synthesis, characterization, and functionalization. J. Phys. Chem. B 105, 7432–7437 (2001)

    Article  CAS  Google Scholar 

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

    Article  CAS  Google Scholar 

  • Corma, A.: From microporous to mesoporous molecular sieve materials and their use in catalysis. Chem. Rev. 97, 2373–2419 (1997)

    Article  CAS  Google Scholar 

  • Fröba, M., Köhn, R., Bouffaud, G.: Fe2O3 nanoparticles within mesoporous MCM-48 silica: in situ formation and characterization. Chem. Mater. 11, 2858–2865 (1999)

    Article  Google Scholar 

  • Gross, A.F., Diehl, M.R., Beverly, K.C., Richman, E.K., Tolbert, S.H.: Controlling magnetic coupling between cobalt nanoparticles through nanoscale confinement in hexagonal mesoporous silica. J. Phys. Chem. B 107, 5475–5482 (2003)

    Article  CAS  Google Scholar 

  • Han, Y., Li, D.F., Zhao, L., Song, J.W., Yang, X.Y., Li, N., Di, Y., Li, C.J., Wu, S., Xu, X.Z., Meng, X.J., Lin, K.F., Xiao, F.S.: High-temperature generalized synthesis of stable ordered mesoporous silica-based materials by using fluorocarbon-hydrocarbon surfactant mixtures. Angew. Chem. Int. Ed. 42, 3633–3637 (2003)

    Article  CAS  Google Scholar 

  • Kresge, C.T., Leonowicz, M.E., Roth, W.J., Vartuli, J.C., Beck, J.S.: Ordered mesoporous molecular sieves synthesized by a liquid-template mechanism. Nature 359, 710–712 (1992)

    Article  CAS  Google Scholar 

  • Li, D., Han, Y., Song, J.W., Zhao, L., Xu, X.Z., Di, Y., Xiao, F.S.: High-temperature synthesis of stable ordered mesoporous silica materials by using fluorocarbon–hydrocarbon surfactant mixtures. Chem. Eur. J. 10, 5911–5922 (2004)

    Article  CAS  Google Scholar 

  • Liang, C.D., Li, Z.J., Dai, S.: Mesoporous carbon materials synthesis and modification. Angew. Chem. Int. Ed. 47, 3696–3717 (2008)

    Article  CAS  Google Scholar 

  • Liu, F.J., Li, C.J., Ren, L.M., Meng, X.J., Zhang, H., Xiao, F.-S.: High-temperature synthesis of stable and ordered mesoporous polymer monoliths with low dielectric constants. J. Mater. Chem. 19, 7921–7928 (2009)

    Article  CAS  Google Scholar 

  • Lu, A.H., Schmidt, W., Matoussevitch, N., Bǒnnemann, H., Spliethoff, B., Tesche, B., Bill, E., Kiefer, W., Schüth, F.: Nanoengineering of a magnetically separable hydrogenation catalyst. Angew. Chem. Int. Ed. 43, 4303–4306 (2004a)

    Article  CAS  Google Scholar 

  • Lu, A.H., Li, W.C., Kiefer, A., Schmidt, W., Bill, E., Fink, G., Schüth, F.: Fabrication of magnetically separable mesostructured silica with an open pore system. J. Am. Chem. Soc. 126, 8616–8617 (2004b)

    Article  CAS  Google Scholar 

  • Lu, A.H., Salabas, E.L., Schüth, F.: Magnetic nanoparticles: synthesis, protection, functionalization, and application. Angew. Chem. Int. Ed. 46, 1222–1224 (2007)

    Article  CAS  Google Scholar 

  • Meng, Y., Gu, D., Zhang, F.Q., Shi, Y.F., Yang, H.F., Li, Z., Yu, C.Z., Tu, B., Zhao, D.Y.: 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 

  • Su, F.B., Zeng, J.H., Bao, X.Y., Yu, Y.S., Lee, J.Y., Zhao, X.S.: Preparation and characterization of highly ordered graphitic mesoporous carbon as a Pt catalyst support for direct methanol fuel cells. Chem. Mater. 17, 3960–3967 (2005)

    Article  CAS  Google Scholar 

  • Sun, Z.H., Wang, L.F., Liu, P.P., Wang, S.C., Sun, B., Jiang, D.Z., Xiao, F.-S.: Magnetically motive porous sphere composite and its excellent properties for the removal of pollutants in water by adsorption and desorption cycles. Adv. Mater. 18, 1968–1971 (2006)

    Article  CAS  Google Scholar 

  • Teunissen, W., Grootde, F.M.F., Geus, J., Stephan, O., Tence, M., Colliex, C.: The structure of carbon encapsulated NiFe nanoparticles. J. Catal. 204, 169–174 (2001)

    Article  CAS  Google Scholar 

  • Vinu, A., Srinivasu, P., Takahashi, M., Mori, T., Balasubramanian, V.V.: Controlling the textural parameters of mesoporous carbon materials. Ariga K. Microporous Mesoporous Mater. 100, 20–26 (2007)

    Article  CAS  Google Scholar 

  • Wan, Y., Zhao, D.Y.: On the controllable soft-templating approach to mesoporous silicates. Chem. Rev. 107, 2821–2860 (2007)

    Article  CAS  Google Scholar 

  • Wang, X.Q., Dai, S.: A simple method to ordered mesoporous carbons containing nickel nanoparticles. Adsorption 15, 138–144 (2009)

    Article  CAS  Google Scholar 

  • Wang, L.F., Lin, K.F., Di, Y., Zhang, D.L., Li, C.J., Yang, Q., Yin, C.Y., Sun, Z.H., Jiang, D.Z., Xiao, F.-S.: High-temperature synthesis of stable ordered mesoporous silica materials using mesoporous carbon as a hard template. Microporous Mesoporous Mater. 86, 81 (2005)

    Article  CAS  Google Scholar 

  • Xiao, N., Wang, L., Zou, Y.C., Wang, C.Y., Ji, Y.Y., Song, J.W., Li, F., Meng, X.J., Xiao, F.S.: High-temperature synthesis of ordered mesoporous silicas from solo hydrocarbon surfactants and understanding of their synthetic mechanisms. J. Mater. Chem. 19, 661–665 (2009)

    Article  CAS  Google Scholar 

  • Yang, P.D., Zhao, D.Y., Margolese, D.I., Chmelka, B.F., Stucky, G.D.: Generalized syntheses of large-pore mesoporous metal oxides with semicrystalline frameworks. Nature 396, 152–155 (1998)

    Article  CAS  Google Scholar 

  • Yi, D.K., Lee, S.S., Papaefthymiou, G.C., Ying, J.Y.: Nanoparticle architectures templated by SiO2/Fe2O3 nanocomposites. Chem. Mater. 18, 614–619 (2006)

    Article  CAS  Google Scholar 

  • Zhai, Y.P., Dou, Y.Q., Liu, X.X., Tu, B., Zhao, D.Y.: One-pot synthesis of magnetically separable ordered mesoporous carbon. J. Mater. Chem. 19, 3292–3300 (2009)

    Article  CAS  Google Scholar 

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

    Article  CAS  Google Scholar 

  • Zhang, L., Qiao, S.Z., Jin, Y.G., Chen, Z.G., Gu, H.C., Lu, G.Q.: Magnetic hollow spheres of periodic mesoporous organosilica and Fe3O4 nanocrystals: fabrication and structure control. Adv. Mater. 20, 805–809 (2008)

    Article  Google Scholar 

  • Zhao, D.Y., Feng, J.L., Huo, Q.S., Melosh, N., Fredrickson, G.H., Chmelka, B.F., Stucky, G.D.: Triblock copolymer syntheses of mesoporous silica with periodic 50 to 300 angstrom pores. Science 279, 548–552 (1998a)

    Article  CAS  Google Scholar 

  • Zhao, D.Y., Huo, Q.S., Feng, J.L., Chmelka, B.F., Stucky, G.D.: 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 (1998b)

    Article  CAS  Google Scholar 

  • Zhao, W., Gu, J., Zhang, L., Chen, H., Shi, J.: Fabrication of uniform magnetic nanocomposite spheres with a magnetic core/mesoporous silica shell structure. J. Am. Chem. Soc. 127, 8916–8917 (2005)

    Article  CAS  Google Scholar 

Download references

Acknowledgements

This work is supported by the State Basic Research Project of China (2009CB623507) and National Natural Science Foundation of China (20973079).

Author information

Authors and Affiliations

  1. Institute of Applied Chemistry, Department of Chemistry, Shaoxing University, Huanchengxi Street 508, Shaoxing, 312000, China

    Fujian Liu

  2. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry and College of Chemistry, Jilin University, Qianjin Street 2699, Changchun, 130012, P.R. China

    Hao Zhang, Longfeng Zhu & Faisal Nawaz

  3. Key Lab of Applied Chemistry of Zhejiang Province, Department of Chemistry, Zhejiang University (XiXi Campus), Tianmushan Road 148, Hangzhou, 310028, China

    Yanmei Liao, Xiangju Meng & Feng-Shou Xiao

Authors
  1. Fujian Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Hao Zhang
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Longfeng Zhu
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Yanmei Liao
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Faisal Nawaz
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Xiangju Meng
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Feng-Shou Xiao
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Feng-Shou Xiao.

Electronic Supplementary Material

Below is the link to the electronic supplementary material.

(PDF 85 kB)

Rights and permissions

Reprints and permissions

About this article

Cite this article

Liu, F., Zhang, H., Zhu, L. et al. High-temperature hydrothermal synthesis of magnetically active, ordered mesoporous resin and carbon monoliths with reusable adsorption for organic dye. Adsorption 19, 39–47 (2013). https://doi.org/10.1007/s10450-012-9408-0

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10450-012-9408-0

Keywords

Search

Navigation