Process for the formation of polyhedral oligomeric silsesquioxanes

A polysilsesquioxane, silsesquioxane technology, applied in silicon-oxygen skeleton structure, various types of R groups. domain, able to address issues such as unproven effects

Inactive Publication Date: 2002-10-30
HYBRID PLASTICS INC
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  • Summary
  • Abstract
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Problems solved by technology

Thus POSS compositions and methods associated with the type of system desired for POSS monomer/polymer technology are unforeseen by the prior art
Additionally, the prior

Method used

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Embodiment Construction

[0074] In Omega-500 ( 1 H, 500MHz; 13 C, 125MHz; 29 NMR spectra were recorded on Si, 99 MHz). Tetrahydrofuran and methyl isobutyl ketone were distilled before use. All other solvents were purchased without purification.

[0075] Example of Method I. Conversion of Polysilsesquioxanes to POSS Fragments and Nanostructures

[0076] by [(C 6 h 5 ) SiO 1.5 ] ∞ Resin synthesis [((C 6 h 5 ) SiO 1.5 ) 8 ] ∑8 Toluene (100mL) in [(C 6 h 5 ) SiO 1.5 ] ∞ To the resin (13.0 g, 100.6 mmol) was added tetramethylammonium hydroxide (2.0 mL, 5.57 mmol). The reaction mixture was heated to 80 °C for up to 12 hours, then cooled to room temperature, acidified with 1N HCl, and filtered to give 12.065 g [((C 6 h 5 ) SiO 1.5 ) 8 ] ∑8 of white solid. The product was examined by EIMS, which showed a molecular ion of 1032.5 amu (atomic mass units) accompanied by product ions of 954.7, 877.4 and 800.6 amu corresponding to the loss of one, two and three phenyl groups, respectively. F...

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Abstract

Three methods for the preparation of polyhedral oligomeric silsesquioxanes (POSS) using the action of bases capable of attacking silicon atoms or any other compounds capable of reacting with protic solvents (such as ROH, H2O, etc.) and producing hydroxides[ OH]-, alkoxide [RO]- and other compounds. The first method utilizes these bases to effectively redistribute the silicon-oxygen framework in polymerized silsesquioxane [RSiO1.5]∞ into POSS nanostructures, that is, the formula [(RSiO1.5)n]∑ The homoleptic segment shown in #, the functionalized homoleptic segment shown in [(RXSiO1.5)n]∑#, the heterogeneous segment shown in [(RSiO1.5)m(R'SiO1.5)n]∑# Segment (heteroleptic) and {(RSiO1.5)m(RXSiO1.0)n}∑ #shown as a functionalized heterosegment nanostructure, where ∞=1-1,000,000 or higher. The second method uses a base to help form POSS nanostructures from silane RSiX3 and linear or cyclic silsesquioxanes of the formula RX2Si-(OSiRX)m-OSiRX2, that is, the formula [(RSiO1.5)n ]∑#, the homogeneous segment shown in [(RSiO1.5)m(R'SiO1.5)n]∑# and the miscellaneous segment shown in [(RSiO1.5)m(RXSiO1.0)n]∑# Functionalized heterosegment nanostructures, where m=0-10, X=OH, Cl, Br, I, alkoxide OR, acetate OOCR, peroxide OOR, amine NR2, isocyanate NCO and R. The third method utilizes bases to selectively open silicon-oxygen-silicon (Si-O-Si) bonds in the POSS structure to form POSS species with incompletely condensed nanostructures. These methods also provide control over the stereochemistry of X. The three methods can generate new POSS species, which can be finally transformed into POSS species suitable for polymerization, grafting or other desired chemical reactions after additional chemical control.

Description

Background of the invention [0001] The present invention describes methods that enable selective control of the silicon-oxygen backbone structure in polyhedral oligomeric silsesquioxane (POSS) cage molecules. It is desirable to be able to selectively control the framework structure of POSS as they serve as chemical species that can be further converted or incorporated into a wide variety of chemical feedstocks for the preparation of catalyst supports, monomers, polymers, And as a solubilized form of silica to replace fumed and precipitated silica or for biological applications and surface modification. POSS, when incorporated into polymeric materials, can provide new and improved thermal, mechanical and physical properties to common polymeric materials. [0002] A wide variety of POSS framework structures can be synthesized in useful quantities by hydrolytic condensation of alkyl- or aryl-trichlorosilanes. However, in most cases, hydrolytic condensation reactions of trifunct...

Claims

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Application Information

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IPC IPC(8): C07F7/08C07F7/12C07F7/21C08G77/38
CPCC07F7/0874C07F7/21C08G77/38C07F7/08C08G77/06B82B3/00
Inventor J·D·里奇滕汉J·J·施瓦博W·雷纳斯M·J·卡尔安以中F·J·菲尔R·特罗巴
Owner HYBRID PLASTICS INC
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