Synthesis, characterization and catalytic application of H3PW12O40/MCM-48 in the esterification of methacrylic acid with n-butyl alcohol

Yijun Zhang , Shuijin Yang

Journal of Wuhan University of Technology Materials Science Edition ›› 2008, Vol. 23 ›› Issue (3) : 346 -349.

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Journal of Wuhan University of Technology Materials Science Edition ›› 2008, Vol. 23 ›› Issue (3) : 346 -349. DOI: 10.1007/s11595-007-3346-9
Article

Synthesis, characterization and catalytic application of H3PW12O40/MCM-48 in the esterification of methacrylic acid with n-butyl alcohol

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Abstract

A novel environmental friendly catalyst, H3PW12O40/MCM-48, was prepared by impregnation method. The catalysts were characterized by means of XRD and FT-IR. The synthesis of n-butyl methacrylate catalyzed by H3PW12O40/MCM-48 was studied with methacrylic acid and n-butyl alcohol as reactants. H3PW12O40/MCM-48 is an excellent catalyst for synthesizing n-butyl methacrylate and Keggin structure of H3PW12O40 kept unchanged after being impregnated on surface of the molecular sieve support. Effects of n(methacrylic acid):n(n-butyl alcohol), catalyst dosage, cyclohexane(water-stripped reagent) and reaction time on yields of the product were investigated. The optimum conditions have been found, that is, molar ratio of acid to alcohol is 1:1.6, mass ratio of catalyst used to the reactants is 0.5% and reaction time is 2.0 h. Under these conditions, the yield of n-butyl methacrylate can reach 93.7%.

Keywords

MCM-48 molecular sieve / phosphotungstic acid / n-butyl methacrylate / catalysis

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Yijun Zhang, Shuijin Yang. Synthesis, characterization and catalytic application of H3PW12O40/MCM-48 in the esterification of methacrylic acid with n-butyl alcohol. Journal of Wuhan University of Technology Materials Science Edition, 2008, 23(3): 346-349 DOI:10.1007/s11595-007-3346-9

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References

[1]

Xu K. X. The Handbook of Materials and Intermediates for Fine Chemicals[M], 1998. Beijing: Chemical Industry Press.

[2]

Zhou D. F., Zhu Z. P., Liu J. F. Heteropolyacids Catalysis in Synthesizing Butyl Methacrylate[J]. Journal of Northeast Normal University(Natural Science Edition), 2000, 32(4): 33-36.

[3]

Li X. G., Liu L., Qian J. H. Cerous(III) Nitrate Synthesized from Catalytic Reaction of n-Butyl Methacrylate Esterification[J]. Journal of Bohai University (Natural Science Edition), 2006, 27(1): 10-13.

[4]

Wang C. G., Jiang C. J., Hu C. G. Synthesis of Propylene Carbonate Catalyzed by Dawson-type Polyoxometalate[J]. Chemical Journal of Chinese Universities, 2004, 15(7): 1 325-1 327.

[5]

Yang S. J. Recent Advance of TiSiW12O40/TiO2 in Synthesis of Esters and Acetal (Ketal)[J]. Chinese Journal of Rare Metals, 2003, 27(1): 183-185.

[6]

Han H. J., Chen T., Wang G. Y. Recent Advances in Ester Reactions Catalyzed by Supported Heteropoly Compounds[J]. Industrial Catalysis, 2006, 14(1): 1-6.

[7]

Jiang X. P., Yuan X. Y., Zhang M. Catalytic Synthesis of Acetals and Ketals from Pentaerythritol with Carbonyl Compounds over HPW/C[J]. Chemical Research and Application, 2003, 15(4): 506-512.

[8]

Yang S. J., Li Z., Tong W. L. Catalytic Synthesis of Acetals and Ketals with H3PW12O40/TiO2[J]. Fine Chemicals, 2005, 22(11): 841-852.

[9]

David K. L., Warren K. M., Thomas N., . Highly Oxidation Resistant Inorganic-porphyrin Analogue Polyoxometalate Oxidation Catalysts. 1. The Synthesis and Characterization of Aqueous-Soluble Potassium Salts of α 2-P2W17O61(Mnn+·OH2)(n−10) and Organic Solvent Soluble tetra-n-Butylammonium Salts of α 2-P2W17O61(Mnn+·Br)(n−11)(M=Mn3+, Fe3+, Co2+, Ni2+ Cu2+)[J]. J. Am. Chem. Soc., 1991, 113(19): 7 209-7 221.

[10]

Guo Y. H., Hu C. W., Jiang S. C. Heterogeneous Photodegradation of Aqueous Hydroxyl Butanedioic Acid by Microporous Polyoxometalates[J]. Applied Catalysis B:Environmental, 2002, 36(1): 9-17.

[11]

Wang C. L., Shen E. H., Wang E. B. Controllable Synthesis of ZnO Nanocrystals via a Surfactant-Assisted Alcohol Thermal Process at a Low Temperature[J]. Materials Letters, 2005, 59(23): 2 867-2 871.

[12]

Kang Z. H., Wang E. B., Mao B. D. Heterogeneous Hydroxylation Catalyzed by Multi-walled Carbon Nanotubes at Low Temperature[J]. Applied Catalysis A: General, 2006, 299: 212-217.

[13]

Yusuke I., Katsunori H., Tomoko H. Acid Catalysis of Silicaincluded Heteropolyacid in Polar Reaction Media[J]. Applied Catalysis A: General, 1999, 181(2): 277-282.

[14]

Wang E. B., Hu C. W., Xu L. Polyhydric Chemist Introduction[M], 1998. Beijing: Chemical Industry Press.

[15]

Saeid F., Mozhgan A., Mansoureh M. Photocatalytic Oxidation of Primary and Secondary Benzylic Alcohols to Carbonyl Compounds Catalyzed by H3PW12O40/SiO2 under an O2 Atmosphere[J]. Tetrahedron Letters, 2005, 46(49): 8 483-8 486.

[16]

Lei P. X., Chen C. C., Yang J. Degradation of Dye Pollutants by Immobilized Polyoxometalate with H2O2 under Visible-light Iirradiation[J]. Environ. Sci. Technol., 2005, 39(21): 8 466-8 474.

[17]

Gallis K. W., Landry C. C. Synthesis of MCM-48 by a Phase Transformation Process[J]. Chem. Mater., 1997, 9(10): 2 035-2 038.

[18]

Xu J., Luan Z. H., He H. Y. A Reliable Synthesis of Cubic Mesoporous MCM-48 Molecular Sieve[J]. Chem. Mater., 1998, 10(11): 3 690-3 698.

[19]

Cai Q., Wei C. P., Xu Y. Y. Synthesis, Characterization and Catalysis Acitivity of the MCM-48 Framework Containing Ti, Co, Cr, Mn, Cu, Mo[J]. Chemical Journal of Chinese Universities, 1999, 20(3): 344-349.

[20]

weakley T. J. R., Malik S. A. Heteropolyanions Containing Two Different Heteroatoms-I[J]. J.Inorg.Nucl.Chem., 1967, 29(3): 2 935-2 944.

[21]

Zhang Y. J., Zhao S. L., Sun G. D. Synthesis and Characterization of Mesoporous Molecular Sieve W-MCM-48 by Microwave Radiation[J]. Chinese Journal of Catalysis, 2000, 21(4): 345-349.

[22]

Claude R. D., Michel F., Raymonde F. Vibrational Investigation of Polyoxometalates. 2. Evidence for Anion-anion Interaction in Molybdenum(VI) and Tungstun(VI) Compounds Related to the Keggin Structure[J]. Inorg. Chem., 1983, 22(2): 107-216.

[23]

Chen C. C., Wang Q., Lei P. X. Photodegradation of Dye Pollutants Catalyzed by Porous K3PW12O40 under Visible Irradiation[J]. Environ. Sci. Technol., 2006, 40(12): 3 965-3 970.

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