Synthesis of polytitanosiloxanes by reaction of diphenylsilanediol with tetrabutoxytitanium

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Journal of Beijing University of Chemical Technology ›› 2010, Vol. 37 ›› Issue (5) : 51-56.

材料科学与工程

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Polytitanosiloxanes have been synthesized by reaction of diphenylsilanediol with tetrabutoxytitanium in a bulk polymerization system. The oligomers were characterized by gel permeation chromatography (GPC), energy dispersive X-ray spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), mass spectrometry (MS), X-ray diffraction (XRD) and thermogravimetric analysis (TGA) methods. The results show that the oligomers were composed of a series of compounds with molecular weights in the range 517-1248. Some of the oligomers were oligo-polytitanosiloxanes, and some were just oligomers of diphenylsilanediol. The TGA study showed that the residue after heating the oligomers to 1000 ℃ in a nitrogen atmosphere was about 48.9% and that they had good thermal resistance.

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Synthesis of polytitanosiloxanes by reaction of diphenylsilanediol with tetrabutoxytitanium[J]. Journal of Beijing University of Chemical Technology, 2010, 37(5): 51-56

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［1］Hoebbel D, Reinert T, Schmidt H. ²⁹Si NMR Investigation of Condensation Reactions of Diphenylsilanediol in Presence of Ti-, Zr-, Al-, Sn- and Si-Alkoxides［J］. Journal of Sol-Gel Science and Technology, 1996, 7(3): 217-224.
［2］Emili M, Incoccia L, Mobilio S. Structural Investigations of TiO2—SiO2 Glassy and Glass-Ceramic Materials Prepared by the Sol-Gel Method［J］. Journal of Non-Crystalline Solids, 1985, 74(1): 129-146.
［3］Hoebbel D, Reinert T, Schmidt H. ²⁹Si and ¹⁷O NMR Investigations on Si—O—Ti Bonds in Solutions of Diphenylsilanediol and Titanium-Tetra-Isopropoxide［J］. Journal of Sol-Gel Science and Technology, 1996, 6(2): 139-149.
［4］Dire S, Babonneau F, Carturan G, et al. Synthesis and Characterization of Siloxane-Titania Materials［J］. Journal of Non-Crystalline Solids, 1992, 147/148: 62-66.
［5］Davis P, Murugavel R. Recent developments in the chemistry of molecular titanosiloxanes and titanophosphonates［J］. Synth React Inorg, Met-Org, Nano-Met Chem, 2005, 35(8): 591-622.
［6］Murugavel R, Davis P, Shete V S. Reactivity Studies, Structural Characterization, and Thermolysis of Cubic Titanosiloxanes: Precursors to Titanosilicate Materials Which Catalyze Olefin Epoxidation［J］. Inorg Chem, 2003, 42(15): 4696-4706.
［7］Gunji T, Kasahara T, Abe Y, et al. Preparation of ceramics from cyclic metallosiloxane compounds as precursors［J］. Mater Technol(Tokyo), 2000, 18(3): 79-85.
［8］Zeitler V A , Brown C A. The Reactions of Triphenylsilanol and Diphenylsilanediol with Some Titanium Esters［J］. Journal of the American Chemical Society, 1957, 79(17): 4618-4621.
［9］Zeitler V A , Brown C A. The Infrared Spectra of Some Ti—O—Si, Ti—O—Ti and Si—O—Si Compounds［J］. Journal of Physical Chemistry, 1957, 61(9): 1174-1177.
［10］Lafond V, Mutin P H, Vioux A. Control of the Texture of Titania-Silica Mixed Oxides Prepared by Nonhydrolytic Sol-Gel［J］. Chemistry of Materials, 2004, 16(25): 5380-5386.
［11］Sun D H, Huang Y, Han B X. Ti—Si Mixed Oxides Prepared by Polymer in Situ Sol-Gel Chemistry with the Aid of CO₂［J］. Langmuir, 2006, 22 (10): 4793-4798.
［12］陈琦丽，唐超群，肖循. TiO₂纳米微粒的溶胶-凝胶法制备及XRD分析［J］. 材料科学与工程, 2002, 20 (2): 224-226.
Chen Q L, Tang C Q, Xiao X. Sol-Gel Preparation Method and XRD Study of TiO₂ Nanoparticles［J］. Materials Science & Engineering, 2002, 20(2): 224-226. （in Chinese）
［13］梅燕，梁慧峰，胡章记. 用电镜及XRD衍射仪表征不同晶型的纳米TiO₂粉末［J］. 现代仪器, 2002(4): 25-28.
Mei Y, Liang H F, Hu Z J. Characterization of nanometer TiO₂ in different crystal structure by TEM and XRD［J］. Modern Instruments, 2002(4): 25-28. （in Chinese）

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Received	Revised	Published
2010-03-01	1900-01-01	2010-09-20
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2010-09-20

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