One Step Preparation of Spherical Silicon Resins from Immiscible Reaction Mixtures

Dayun Lee; Young-A Kim; Young Baek Kim; Jun-Kyu Kim; Yang-Kyoo Han

Macromolecular Research, Vol.16, No.4, 353-359, June, 2008

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One Step Preparation of Spherical Silicon Resins from Immiscible Reaction Mixtures

Dayun Lee, Young-A Kim, Young Baek Kim^†, Jun-Kyu Kim¹, and Yang-Kyoo Han²

Department of Nano-polymeric Materials, PaiChai University, Daejeon 302-735, Korea
¹Kolon Industry, Chemical Organization, Incheon 404-250, Korea
²Department of Chemistry, Hanyang University, Seoul 133-791, Korea

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Spheres of silicon resins with different compositions were prepared in one-step reaction from mixtures of water and water-insoluble precursors of polysiloxanes (PSO) and polysilsesquioxanes (PSQ) using different amines as catalysts. The presence of PSO and PSQ in the spheres was confirmed by their mechanical properties and FTIR spectroscopy. Spheres of pure PSO were obtained from only dimethoxymethylvinylsiloxane (DMMVS) and 3-mercaptopropylmethyldimethoxysilan (MPMDMS) when the reaction was induced with appropriate catalysts. DMMVS and MPMDMS always gave the most promising results regarding the formation of discrete solid spheres with the minimum tendency to form monolithic solids or fluid-like, premature products. The spheres were characterized by optical microscopy, scanning electron microscopy (SEM), and Fourier transform infrared (FTIR) spectroscopy. The mixtures containing larger amounts of PSO precursors commonly gave lower yields and softer spheres.

Keywords:polysiloxane;polysilsesquioxane;spheres;silicon resins;one-pot preparation

[References]

Baney RH, Itoh M, Sakakibara A, Suzuki T, Chem. Rev., 95(5), 1409 (1995)
Nalwa HS, Handbook of Organic-Inorganic Hybrid Materials and Nanocomposites, H. S. Nalwa, Ed., Americal Scientific Publishers, Stevenson Ranch, 2003, Vol. I & Vol. II
Zhang C, Liane RM, J. Organomet. Chem., 521, 199 (1996)
Arkhireeva A, Hay JN, J. Mater. Chem., 13, 3122 (2003)
Choi JY, Kim CH, Kim DK, J. Am. Ceram. Soc., 81, 1184 (1998)
Goller MI, Obey TM, Teare DOH, Vincent B, Colloids Surf. A: Physicochem. Eng. Asp., 123-124, 183 (1997)
Liu SM, Lang XM, Ye H, Zhang SJ, Zhao JQ, Eur. Polym. J., 41, 996 (2005)
OBEY TM, VINCENT B, J. Colloid Interface Sci., 163(2), 454 (1994)
Attard P, Gillies G, Aust. J. Chem., 54, 477 (2001)
Kim YB, Kim YA, Yoon KS, Macromol. Rapid Commun., 27(15), 1247 (2006)
Ottenbrite RM, Wall JS, Siddiqui JA, J. Am. Ceram. Soc., 83(12), 3214 (2000)
Dufaud O, Favre E, Sadtler V, J. Appl. Polym. Sci., 83(5), 967 (2002)
Embery CJ, Clarke SR, Matisons JG, in Handbook of Organic-Inorganic Hybrid Materials and Nanocomposites, H. S. Nalwa, Ed., Americal Scientific Publishers, Stevenson Ranch, 2003, Vol. I
Fina A, Tabuani D, Carniato F, Frache A, Boccaleri E, Camino G, Thermochim. Acta, 440(1), 36 (2006)

[Referenced By]

[1] Baney RH, Itoh M, Sakakibara A, Suzuki T, Chem. Rev., 95(5), 1409 (1995)

[2] Nalwa HS, Handbook of Organic-Inorganic Hybrid Materials and Nanocomposites, H. S. Nalwa, Ed., Americal Scientific Publishers, Stevenson Ranch, 2003, Vol. I & Vol. II

[3] Zhang C, Liane RM, J. Organomet. Chem., 521, 199 (1996)

[4] Arkhireeva A, Hay JN, J. Mater. Chem., 13, 3122 (2003)

[5] Choi JY, Kim CH, Kim DK, J. Am. Ceram. Soc., 81, 1184 (1998)

[6] Goller MI, Obey TM, Teare DOH, Vincent B, Colloids Surf. A: Physicochem. Eng. Asp., 123-124, 183 (1997)

[7] Liu SM, Lang XM, Ye H, Zhang SJ, Zhao JQ, Eur. Polym. J., 41, 996 (2005)

[8] OBEY TM, VINCENT B, J. Colloid Interface Sci., 163(2), 454 (1994)

[9] Attard P, Gillies G, Aust. J. Chem., 54, 477 (2001)

[10] Kim YB, Kim YA, Yoon KS, Macromol. Rapid Commun., 27(15), 1247 (2006)

[11] Ottenbrite RM, Wall JS, Siddiqui JA, J. Am. Ceram. Soc., 83(12), 3214 (2000)

[12] Dufaud O, Favre E, Sadtler V, J. Appl. Polym. Sci., 83(5), 967 (2002)

[13] Embery CJ, Clarke SR, Matisons JG, in Handbook of Organic-Inorganic Hybrid Materials and Nanocomposites, H. S. Nalwa, Ed., Americal Scientific Publishers, Stevenson Ranch, 2003, Vol. I

[14] Fina A, Tabuani D, Carniato F, Frache A, Boccaleri E, Camino G, Thermochim. Acta, 440(1), 36 (2006)