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1. 发明授权

US06972312B1 Process for the formation of polyhedral oligomeric silsesquioxanes 有权
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
IPC分类号： C08G77/04 , C08G77/06 , C08G77/08
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.

2. 发明授权

US06911518B2 Polyhedral oligomeric -silsesquioxanes, -silicates and -siloxanes bearing ring-strained olefinic functionalities 有权
公开(公告)号：US06911518B2
公开(公告)日：2005-06-28
申请号：US09747762
申请日：2000-12-21
申请人： Joseph D. Lichtenhan , Joseph J. Schwab , Yi-Zong An , William Reinerth , Frank J. Feher
发明人： Joseph D. Lichtenhan , Joseph J. Schwab , Yi-Zong An , William Reinerth , Frank J. Feher
IPC分类号： C07F7/08 , C07F7/18 , C07F7/21 , C07F11/00 , C08G77/20 , C08G77/08
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.

3. 发明授权

US5939576A Method of functionalizing polycyclic silicones and the compounds so formed 失效
标题翻译：使多环硅氧烷官能化的方法和如此形成的化合物
公开(公告)号：US5939576A
公开(公告)日：1999-08-17
申请号：US3084
申请日：1998-01-05
申请人： Joseph D. Lichtenhan , Joseph J. Schwab , Frank J. Feher , Daravong Soulivong
发明人： Joseph D. Lichtenhan , Joseph J. Schwab , Frank J. Feher , Daravong Soulivong
IPC分类号： C07F7/21 , C07F7/08 , C07F7/10
CPC分类号： C07F7/21
摘要： A synthetic process for the selective preparation of reactive polyhedral oligomeric silsesquioxanes (POSS) as well as polyhedral oligomeric silicate (POS) (spherosilicate) is provided. The inventive process employs the use of metal catalyzed hydrosilylation reactions for the selective reaction of silane containing polyhedral oligomeric silsesquioxanes or silicates with olefinic reagents bearing functionalities useful for grafting reactions, polymerization chemistry and sol-gel processes. The invention also discloses metal-catalyzed hydrosulfidation reactions and metal-catalyzed hydrophosphidation reacttions for functionalization of polycyclic silicones.
摘要翻译：提供了选择性制备反应性多面体低聚倍半硅氧烷（POSS）以及多面体低聚硅酸盐（POS）（硅藻土）的合成方法。本发明方法采用金属催化的氢化硅烷化反应来选择性反应含硅烷的多面体低聚倍半硅氧烷或硅酸盐与含有可用于接枝反应，聚合化学和溶胶 - 凝胶法的官能团的烯属试剂。本发明还公开了金属催化的加氢硫化反应和用于多环硅氧烷官能化的金属催化的氢磷化反应。

4. 发明授权

US06933345B1 Reactive grafting and compatibilization of polyhedral oligomeric silsesquioxanes 失效
标题翻译：多面体低聚倍半硅氧烷的反应性接枝和增容
公开(公告)号：US06933345B1
公开(公告)日：2005-08-23
申请号：US10351292
申请日：2003-01-23
申请人： Joseph D. Lichtenhan , Frank J. Feher , Joseph J. Schwab , Sixun Zheng
发明人： Joseph D. Lichtenhan , Frank J. Feher , Joseph J. Schwab , Sixun Zheng
IPC分类号： C08F8/00 , C08K5/5419 , C08K7/00 , C08L83/00
CPC分类号： B82Y30/00 , C08K5/5419 , C08K7/00 , C08K2201/011 , C08L2205/14 , C08L23/10
摘要： The nanoscopic dimensions of polyhedral oligomeric silsesquioxanes (POSS) and polyhedral oligomeric silicates (POS) materials ranges from 0.7 nm to 5.0 nm and enables the thermomechanical and physical properties of polymeric materials to be improved by providing nanoscopic reinforcement of polymer chains at a length scale that is not possible by physically smaller aromatic chemical systems or larger fillers and fibers. A simple and cost effective method for incorporating POSS/POS nanoreinforcements onto polymers via the reactive grafting of suitably functionalized POSS/POS entities with polymeric systems amenable to such processes is described. The method teaches that the resulting POSS-grafted-polymers are particularly well suited for alloying agents by nongrafted POSS entitles such as molecular silicas. The successful alloying of POSS-polymers is aided because their interfacial tensions are reduced relative to non-POSS containing systems.
摘要翻译：多面体低聚倍半硅氧烷（POSS）和多面体低聚硅酸盐（POS）材料的纳米尺寸范围为0.7nm至5.0nm，并且通过以长度尺度提供聚合物链的纳米级增强，可以改善聚合物材料的热机械和物理性能，通过物理上较小的芳族化学体系或较大的填料和纤维是不可能的。描述了通过适当功能化的POSS / POS实体与适合于这种方法的聚合物体系的反应性接枝将POSS / POS纳米增强剂结合到聚合物上的简单且成本有效的方法。该方法教导得到的POSS接枝聚合物特别适用于通过非接枝POSS权利如分子二氧化硅的合金化剂。有助于POSS聚合物的成功合金化，因为它们的界面张力相对于不含POSS的体系而降低。

5. 发明授权

US06927270B2 Process for the functionalization of polyhedral oligomeric silsesquioxanes 失效
公开(公告)号：US06927270B2
公开(公告)日：2005-08-09
申请号：US10186318
申请日：2002-06-27
申请人： Joseph D. Lichtenhan , Joseph J. Schwab , Yi-Zhong An , Qibo Liu , Timothy S. Haddad
发明人： Joseph D. Lichtenhan , Joseph J. Schwab , Yi-Zhong An , Qibo Liu , Timothy S. Haddad
IPC分类号： C07F7/07 , C08G20060101 , C08G77/00 , C08G77/06
CPC分类号： C08G77/04 , C08G77/24 , C08G77/38
摘要： Efficient processes have been developed for the cost effective functionalization of polyhedral oligomeric silsesquioxane-silanols (POSS-Silanols) and for the manufacture of polyfunctional polyhedral oligomeric silsesquioxanes. The processes utilize the action of bases or acids on silane coupling agents. The preferred process utilizes base to promote the silylation of POSS-Silanols of the formula [(RSiO1.5)n(R(HO)SiO1.0)m]Σ# with silane coupling agents to form POSS species with functionalized incompletely condensed nanostructures [(RSiO1.5)n(R(YSiR2O)SiO1.0)m]Σ# or functionalized completely condensed nanostructures [(RSiO1.5)n(YSiO1.5)1]Σ#. The process can alternately be conducted with acids. A second process utilizes base to alkylate POSS-Silanols with functionalized alkyl halides. A third related process utilizes base to react with silane coupling agents to form polyfunctional, fully condensed POSS species of formula [(YSiO1.5)n]Σ#. This process can also alternately be conducted under acidic conditions. Each of the processes result in new POSS compositions that can undergo additional desirable chemical reactions or which are directly suitable for polymerization or grafting into polymeric materials. POSS frameworks containing silanol and other reactive functionalities suitable for polymerizations have previously been described as valuable co-monomers in polymerizations and as feed-stocks for the preparation of a diverse number of chemical agents that are useful in polymeric materials in biological applications, and for the modification of surfaces.

6. 发明授权

US06767930B1 Polyhedral oligomeric silsesquioxane polyimide composites 有权
标题翻译：多面体低聚倍半硅氧烷聚酰亚胺复合材料
公开(公告)号：US06767930B1
公开(公告)日：2004-07-27
申请号：US10238923
申请日：2002-09-09
申请人： Steven A. Svejda , Shawn H. Phillips , Rene I. Gonzalez , Frank J. Feher , Joseph D. Lichtenhan , Joseph J. Schwab , William A. Reinerth
发明人： Steven A. Svejda , Shawn H. Phillips , Rene I. Gonzalez , Frank J. Feher , Joseph D. Lichtenhan , Joseph J. Schwab , William A. Reinerth
IPC分类号： C08J900
CPC分类号： C08J9/26 , C08G73/106 , C08G77/455 , C08J2379/08 , C08K5/49
摘要： Performance additives in high performance polymers using polyhedral oligomeric silsesquioxanes (POSS) and polyhedral oligomeric silicates (POS) as nanoscopic reinforcements, porosity control agents, thermal and oxidative stability aids to improve the properties of the polymers.
摘要翻译：使用多面体低聚倍半硅氧烷（POSS）和多面体低聚硅酸盐（POS）作为纳米增强剂的高性能聚合物的性能添加剂，孔隙度控制剂，热和氧化稳定性有助于改善聚合物的性能。

7. 发明授权

US07553904B2 High use temperature nanocomposite resins 有权
标题翻译：高使用温度的纳米复合树脂
公开(公告)号：US07553904B2
公开(公告)日：2009-06-30
申请号：US11225607
申请日：2005-09-12
申请人： Joseph D. Lichtenhan , Qibo Liu , Yan-Jyh Lee , Xuan Fu , Sukhendu Hait , Joseph J. Schwab , Rusty L. Blanski , Patrick N. Ruth
发明人： Joseph D. Lichtenhan , Qibo Liu , Yan-Jyh Lee , Xuan Fu , Sukhendu Hait , Joseph J. Schwab , Rusty L. Blanski , Patrick N. Ruth
IPC分类号： C08L83/00
CPC分类号： C08K5/549 , Y10T428/31663
摘要： A method of using olefin containing nanostructured chemicals and silanol containing nanostructured chemicals as high temperature resins is described. Vinyl containing nanostructured chemicals are particularity effective in thermosets as they control the motions of polymer chains, and segments, at the molecular level. Silanol containing nanostructured chemicals are particularity effective in thermosets containing polar groups as the silanol can enhance the reactivity of these groups. Because of their tailorable compatibility with fluorinated polymers, nanostructured chemicals can be readily and selectively incorporated into polymers by direct blending and polymerization processes. The incorporation of a nanostructured chemical into a polymer favorably impacts a multitude of polymer physical properties. Properties most favorably improved are heat distortion and flammability characteristics, permeability, optical properties, texture, feel and durability. Other properties improved include time dependent mechanical and thermal properties such as creep, compression set, shrinkage, modulus, and hardness. In addition to mechanical properties, other physical properties are favorably improved, including lower thermal conductivity, and gas oxygen permeability. These improved properties may be useful in a number of applications, including composite materials, foams, cosmetics, and durable coatings.
摘要翻译：描述了使用含烯烃的纳米结构化学品和含硅烷醇的纳米结构化学品作为高温树脂的方法。含乙烯基纳米结构化学品在热固性材料中特别有效，因为它们在分子水平上控制聚合物链和链段的运动。含硅烷醇的纳米结构化学品在含极性基团的热固性材料中是特别有效的，因为硅烷醇可增强这些基团的反应性。由于它们与氟化聚合物的可定制的相容性，纳米结构化学物质可以通过直接共混和聚合过程容易且选择性地引入到聚合物中。将纳米结构化学物质掺入聚合物有利地影响了许多聚合物的物理性质。性能最有利地提高了热变形和易燃特性，渗透性，光学性能，质地，手感和耐久性。改进的其它性能包括时间依赖性机械和热性能，如蠕变，压缩永久变形，收缩率，模量和硬度。除机械性能外，还有其他物理性能得到改善，包括较低的导热系数和气体透氧性。这些改进的性质可用于许多应用，包括复合材料，泡沫，化妆品和耐用涂层。

8. 发明授权

US07888435B2 Process for continuous production of olefin polyhedral oligomeric silsesquioxane cages 有权
标题翻译：连续生产烯烃多面体低聚倍半硅氧烷笼的方法
公开(公告)号：US07888435B2
公开(公告)日：2011-02-15
申请号：US11420449
申请日：2006-05-25
申请人： Joseph D. Lichtenhan , Sukhendu Bikash Hait , Joseph J. Schwab , Michael J. Carr
发明人： Joseph D. Lichtenhan , Sukhendu Bikash Hait , Joseph J. Schwab , Michael J. Carr
IPC分类号： C08G77/20
CPC分类号： A61K8/895 , A61Q19/00 , C07F7/0874 , C07F7/21
摘要： Methods for continuous bulk production of polyolefin polyhedral oligomeric silsesquioxanes and their amino, isocyanate, and alcohol derivatives using silane coupling agents as precursors.
摘要翻译：使用硅烷偶联剂作为前体的连续大量生产聚烯烃多面体低聚倍半硅氧烷及其氨基，异氰酸酯和醇衍生物的方法。

9. 发明申请

US20110201827A1 PROCESS FOR CONTINUOUS PRODUCTION OF OXIDIZED OLEFIN POLYHEDRAL OLIGOMERIC SILSESQUIOXANE CAGES 审中-公开
标题翻译：连续生产氧化烯烃聚氧乙烯低聚硅氧烷的方法
公开(公告)号：US20110201827A1
公开(公告)日：2011-08-18
申请号：US13026529
申请日：2011-02-14
申请人： Joseph D. Lichtenhan , Sukhendu Bikash Hait , Joseph J. Schwab , Michael J. Carr
发明人： Joseph D. Lichtenhan , Sukhendu Bikash Hait , Joseph J. Schwab , Michael J. Carr
IPC分类号： C07F7/18
CPC分类号： A61K8/895 , A61Q19/00 , C07F7/0874 , C07F7/21
摘要： Methods for continuous bulk production of polyolefin polyhedral oligomeric silsesquioxanes and their amino, isocyanate, and alcohol derivatives using silane coupling agents as precursors.
摘要翻译：使用硅烷偶联剂作为前体的连续大量生产聚烯烃多面体低聚倍半硅氧烷及其氨基，异氰酸酯和醇衍生物的方法。

10. 发明授权

US6100417A Functionalizing olefin bearing silsesquioxanes 失效
标题翻译：官能化烯烃轴承倍半硅氧烷
公开(公告)号：US6100417A
公开(公告)日：2000-08-08
申请号：US387682
申请日：1999-08-31
申请人： Joseph D. Lichtenhan , Frank J. Feher , Daravong Soulivong
发明人： Joseph D. Lichtenhan , Frank J. Feher , Daravong Soulivong
IPC分类号： C07F7/21 , C07F2/08
CPC分类号： C07F7/21
摘要： Method is provided for reacting silsesquioxane resins or polyhedral oligomeric silsesquioxanes (POSS) bearing one or more olefinic groups with strong acids to cleave one or more olefin bonds of the olefinic groups to form POSS species of monomers or polymers having one or more functionalities suitable for reaction with a wide range of polymeric systems, to thus form new POSS derived compounds. Also provided are the new compounds so formed.
摘要翻译：提供了将含有一个或多个烯属基团的倍半硅氧烷树脂或多面体低聚倍半硅氧烷（POSS）与强酸反应以切割烯烃基团的一个或多个烯烃键以形成具有一个或多个适合于反应的官能团的单体或聚合物的POSS种类的方法具有广泛的聚合体系，从而形成新的POSS衍生化合物。还提供了如此形成的新化合物。

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