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公开(公告)号：US06972312B1
公开(公告)日：2005-12-06
申请号：US09631892
申请日：2000-08-04
申请人： Joseph D. Lichtenhan , Joseph J. Schwab , Yi-Zong An , William Reinerth , Michael J. Carr , Frank J. Feher , Raquel Terroba , Qibo Liu
发明人： Joseph D. Lichtenhan , Joseph J. Schwab , Yi-Zong An , William Reinerth , Michael J. Carr , Frank J. Feher , Raquel Terroba , Qibo Liu
CPC分类号： C08G77/04 , C08G77/045 , C08G77/06 , C08G77/08
摘要： Three processes for the manufacture of polyhedral oligomeric silsesquioxanes (POSS) which utilize the action of bases that are capable of either attacking silicon or any compound that can react with a protic solvent (e.g. ROH, H2O etc.) and generate hydroxide [OH]−, alkoxide [RO]−′, etc. The first process utilizes such bases to effectively redistribute the silicon-oxygen frameworks in polymeric silsesquioxanes [RSiO1.5]28 where ∞=1-1,000,000 or higher into POSS nanostructures of formulas [(RSiO1.5)nΣ#, homoleptic, [(RXSiO1.5)n]Σ#, functionalized homoleptic, [(RSiO1.5)m(R′SiO1.5)n]Σ#, heteroleptic, and {(RSiO1.5)m(RXSiO1.0)n}Σ#, functionalized heteroleptic nanostructures. The second process utilizes base to aid in the formation of POSS nanostructures of formulas [(RSiO1.5)n]Σ# homoleptic and [(RSiO1.5)m(R′SiO1.5)n]Σ# heteroleptic and [(RSiO1.5)m(RXSiO1.0)n]Σ# functionalized heteroleptic nanostructures from silanes RSiX3 and linear or cyclic silsesquioxanes of the formula RX2Si—(OSiRX)m—OSiRX2 where m=0-10, X=OH, Cl, Br, I, alkoxide OR, acetate OOCR, peroxide OOR, amine NR2, isocyanate NCO, and R. The third process utilizes base to selectively ring-open the silicon-oxygen-silicon (Si—O—Si) bonds in POSS structures to form POSS species with incompletely condensed nanostructures. These processes also afford stereochemical control over X. The three processes result in new POSS species that can undergo additional chemical manipulations to ultimately be converted into POSS-species suitable for polymerization, grafting, or other desirable chemical reactions.
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公开(公告)号：US20050239985A1
公开(公告)日：2005-10-27
申请号：US11166008
申请日：2005-06-24
申请人： Joseph Lichtenhan , Joseph Schwab , Yi-Zong An , William Reinerth , Michael Carr , Frank Feher , Raquel Terroba
发明人： Joseph Lichtenhan , Joseph Schwab , Yi-Zong An , William Reinerth , Michael Carr , Frank Feher , Raquel Terroba
CPC分类号： C08G77/04 , C08G77/045 , C08G77/06 , C08G77/08
摘要： Three processes for the manufacture of polyhedral oligomeric silsesquioxanes (POSS) which utilize the action of bases that are capable of either attacking silicon or any compound that can react with a protic solvent (e.g. ROH, H2O etc.) and generate hydroxide [OH]−, alkoxide [RO]−, etc. The first process utilizes such bases to effectively redistribute the silicon-oxygen frameworks in polymeric silsesquioxanes [RSiO1.5]∞ where ∞=1−1,000,000 or higher into POSS nanostructures of formulas [(RSiO1.5)n]Σ#, homoleptic, [(RXSiO1.5)n]Σ#, functionalized homoleptic, [(RSiO1.5)m(R′SiO1.5)n]Σ#, heteroleptic, and {(RSiO1.5)m(RXSiO1.0)n}Σ#, functionalized heteroleptic nanostructures. The second process utilizes base to aid in the formation of POSS nanostructures of formulas [(RSiO1.5)n]Σ# homoleptic and [(RSiO1.5)m(R′SiO1.5)n]Σ# heteroleptic and [(RSiO1.5)m(RXSiO1.0)n]Σ# functionalized heteroleptic nanostructures from silanes RSiX3 and linear or cyclic silsesquioxanes of the formula RX2Si—(OSiRX)m—OSiRX2 where m=0-10, X═OH, Cl, Br, I, alkoxide OR, acetate OOCR, peroxide OOR, amine NR2, isocyanate NCO, and R. The third process utilizes base to selectively ring-open the silicon-oxygen-silicon (Si—O—Si) bonds in POSS structures to form POSS species with incompletely condensed nanostructures. These processes also afford stereochemical control over X. The three processes result in new POSS species that can undergo additional chemical manipulations to ultimately be converted into POSS-species suitable for polymerization, grafting, or other desirable chemical reactions.
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公开(公告)号：US06911518B2
公开(公告)日：2005-06-28
申请号：US09747762
申请日：2000-12-21
CPC分类号： C08G77/20 , C07F7/0829 , C07F7/0874 , C07F7/0879 , C07F7/1876 , C07F7/188 , C07F7/21 , C07F11/005
摘要： Processes have been developed for the manufacture of polyhedral oligomeric silsesquioxanes (POSS), polysilsesquioxanes, polyhedral oligomeric silicates (POS), and siloxane molecules bearing reactive ring-strained cyclic olefins (e.g. norbornenyl, cyclopentenyl, etc. functionalities). The preferred manufacturing processes employ the silation of siloxides (Si—OA, where A=H, alkaline or alkaline earth metals) with silane reagents that contain at least one reactive ring-strained cyclic olefin functionality [e.g., X3-ySi(CH3)y(CH2)2 where y=1-2 and X=OH, Cl, Br, I, alkoxide OR, acetate OOCR, peroxide OOR, amine NR2, isocyanate NCO, and R]. Alternatively, similar products can be prepared through hydrosilation reactions between silanes containing at least one silicon-hydrogen bond (Si—H) with ring-strained cyclic olefin reagents [e.g., 5-vinyl, 2 norbornene CH2═CH, cyclopentadiene]. The two processes can be effectively practiced using polymeric silsesquioxanes [RSiO1.5]∞ where ∞=1-1,000,000 or higher and which contain unreacted silanol or silane groups at chain terminus or branch points, on POSS nanostructures of formulas [(RSiO1.5)n]Σ#, homoleptic, [(RSiO1.5)m(R′SiO1.5)n]Σ#, heteroleptic, and {(RSiO1.5)m(RXSiO1.0)n}Σ#, functionalized heteroleptic nanostructures, on silanes RSiX3, linear, cyclic, oligomeric and polymeric siloxanes (polymeric formula RX2Si—(OSiRX)m—OSiRX2 where m=0-1000, X=OH, Cl, Br, I, alkoxide OR, acetate OOCR, peroxide OOR, amine NR2, isocyanate NCO, and R). Each of the processes result in new chemical species bearing one or more ring strained olefins that can undergo polymerization, grafting, or other desirable chemical reactions to form polymeric products. These polymeric systems are most desirably utilized in polymerizations for the modification of properties of thermoplastic or thermoset resin systems or for the preparation of polymers with utility in electronics, medical devices, sporting goods, and aerospace as coatings and structural components.
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