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Poly(carborane-siloxane/silazane) polymer and preparation method thereof

A carborane and polymer technology, applied in the field of high-temperature-resistant polymers and their preparation, can solve the problems of difficult growth of molecular weight, excessive silicon-nitrogen bonds, and difficult regulation of molecular structure, etc., and achieve the effect of great application value

Active Publication Date: 2011-08-31
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] The disadvantage of this method is that its molecular weight is difficult to increase, and the silicon-nitrogen bond is greatly excessive, and the molecular structure is not easy to control

Method used

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  • Poly(carborane-siloxane/silazane) polymer and preparation method thereof
  • Poly(carborane-siloxane/silazane) polymer and preparation method thereof
  • Poly(carborane-siloxane/silazane) polymer and preparation method thereof

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Effect test

Embodiment 1

[0044] Embodiment 1, the preparation of poly(carborane-siloxane / silazane) polymer

[0045] Under an inert atmosphere, put 2.44g of bis(hydroxydimethylsilyl)-m-carborane and 0.61g of hexamethylcyclotrisilazane in a reaction flask, and add 5mL of toluene and 0.5g of anhydrous acetic acid (where , the amount of acetic acid is two (hydroxydimethylsilyl)-m-carborane and hexamethylcyclotrisilazane (structure shown in formula (III), wherein, a is 0, b is 3, R 3 and R 4 16.4% of the total mass of methyl group), stirred and reacted at 90° C. for 24 hours. After the reaction, the solution obtained was washed with methanol to remove small molecules to obtain a white waxy solid polymer. Its number average molecular weight is 2.8×10 4 , with a weight average molecular weight of 4.2×10 4 , Elemental analysis: C 28.04%, H 8.23%, N 0.62%. by 29 Si NMR analysis shows that its structure is shown in formula (IV), wherein the degree of polymerization x is 118.

[0046]

Embodiment 2

[0047] Embodiment 2, the preparation of poly(carborane-siloxane / silazane) polymer

[0048] Under an inert atmosphere, 7.25g of bis(hydroxydiphenylsilyl)-m-carborane and 0.98g of hexamethylcyclotrisilazane were added to the reaction flask, and 0.5g of acetic anhydride was added (wherein, acetic anhydride The consumption is bis(hydroxyl diphenylsilyl)-m-carborane and hexamethylcyclotrisilazane (structure shown in formula (III), wherein, a is 0, b is 3, R 3 and R 4 6.1% of the total mass of the methyl group), reacted at 110° C. for 24 hours under solvent-free conditions, raised the temperature to 150° C. and continued to stir and reacted for 12 hours. After the reaction, a viscous polymer was obtained. Wash away the small molecules with methanol, and measure the number average molecular weight to be 4.6×10 4 , with a weight average molecular weight of 7.0×10 4 ,by 29 Si NMR analysis shows that its structure is shown in formula (V), wherein the degree of polymerization x is 10...

Embodiment 3

[0050] Embodiment 3, the preparation of poly(carborane-siloxane / silazane) polymer

[0051] Under an inert atmosphere, mix 2.00 g of bis(hydroxydimethylsilyl)-m-carborane with 0.58 g of 1,3,5-trimethyl-1,3,5-trivinyl-cyclotrisilazide Add 0.05g of ammonium chloride into the reaction flask, and add 0.05g of ammonium chloride as a catalyst (wherein, the amount of ammonium chloride is two (hydroxyl diphenylsilyl)-m-carborane and 1,3,5-trimethyl- 1,3,5-trivinyl-cyclotrisilazane (structure shown in formula (III), wherein, a is 0, b is 3, R 3 Methyl, R 4 1.9% of the total mass of vinyl), add 10mL xylene as a solvent, and stir and react at 110° C. for 24 hours. After the reaction is finished, wash off small molecular substances with methanol to obtain a white waxy polymer. The number average molecular weight was determined to be 1.4×10 5 , with a weight average molecular weight of 1.6×10 5 ,by 29 Si NMR analysis shows that its structure is shown in formula (VI), wherein the degree...

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Abstract

The invention provides a poly(carborane-siloxane / silazane) polymer and a preparation method thereof. The structure of the polymer is shown in the formula (I), wherein the formula represents carborane group; p and q are natural numbers between 3 and 16; R1, R2, R3 and R4 are selected from hydrogen, substituted or unsubstituted C1-20 alkyl, cycloalkyl, alkenyl, alkynyl or aryl; m is a number between 0 and 100, except for 0; n is a number between 0 and 100; and x represents the polymerization degree of the polymer and is a number between 0 and 1000. In the invention, a simple method is adopted to synthesize the carborane-containing polysiloxane-silazane polymer with the new structure, wherein the polymer contains repetitive units such as carborane, siloxane and silazane in the structure; unsaturated groups such as vinyl and ethynyl can be conveniently introduced to the side group to ensure that polymer performs crosslinking under the thermal effect to form resin materials, and the resin materials are further heated to form ceramic materials. The polymer can be used as high-temperature resistant binders, atomic oxygen resistant coatings, ceramic precursors and the like and have great application value in the fields such as national defense, aviation and aerospace.

Description

technical field [0001] The invention relates to a poly(carborane-siloxane / silazane) polymer and a preparation method thereof, belonging to the field of high temperature resistant polymers and the preparation thereof. Background technique [0002] In the 1960s, American researchers synthesized icosahedral carborane, which is a "super-aromatic" icosahedral structure composed of boron, carbon, and hydrogen. The ions of the nucleus, and then react with the halosilane, can introduce the carborane structure into the organic compound or organosilicon monomer, so as to obtain high temperature resistant, oxidation resistant monomer and its polymer material. American Olin Company and Union Carbide Company have successively carried out a lot of poly(carborane-siloxane) synthesis research work. Among them, the Dexsil series silicon-boron rubber synthesized by Olin Company is based on the reaction of bis(dimethylchlorosilyl)-m-carborane and dimethoxydimethylsilane under the catalysis of...

Claims

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Application Information

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IPC IPC(8): C08G77/54C09J183/14C09D183/14
Inventor 张学超孔令虹张学忠戴丽娜汪倩谭永霞张志杰谢择民
Owner INST OF CHEM CHINESE ACAD OF SCI
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