Novel high temperature-resisting phenylboronic acid-silane-ethynyl polymer and preparation method thereof
A technology based on phenylboronic acid and ethynyl, which is applied in the field of organoborosilicate-alkyne hybrid polymers, can solve problems such as inability to meet high temperature requirements, and achieve the effects of abundant raw material sources, simple preparation process, and convenient operation
Inactive Publication Date: 2013-01-23
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology
However, with the development of science and technology, especially national defense and aerospace technology, people have put forward higher and more urgent requirements for the heat resistance of products, and the existing silicone materials have been decomposed due to thermal oxidation at high temperatures. Unable to meet special high temperature requirements
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Embodiment approach
[0024] Embodiment: the first step, in the inert gas N 2 10mmol of phenylboronic acid and 40ml of butyl acetate were added to a 250ml three-necked flask, and then 18mmol of first-grade hydrodichlorosilane was added dropwise to the three-necked flask. The dropwise addition process took 10 to 20 minutes, and the temperature was slowly raised to 130°C for 20 Hour. In the second step, in the inert gas N 2 Under protection, 16mmol of phenylacetylene and 40ml of tetrahydrofuran were added to another 250ml three-necked flask, the temperature of the system dropped to -78°C, and then 16mmol of butyllithium was slowly added dropwise, and the reaction was completed for 4 hours. After the first step reaction was completed, the temperature was lowered to -20°C, and then the product of the second step reaction was added to the first step reaction system, and reacted at 15°C for 24 hours. After the reaction is complete, add saturated NH 4 Cl solution, fully stirred, liquid separation, take...
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The invention discloses a novel phenylboronic acid-silane-ethynyl polymer and a preparation method thereof. The polymer is prepared by three steps by taking silane dihalide, phenylboronic acid, monoethynyl compound and organic lithium as raw materials to carry out reaction under the protection of inert gases, wherein during the first step of reaction, the phenylboronic acid reacts with the silanedihalide to generate polymer which has silicon-oxygen-boron-oxygen repeating units and two halogen-terminated ends; during the second step of reaction, the monoethynyl compound reacts with the organic lithium to generate monoethynyl lithium compound; and during the third step of reaction, the monoethynyl lithium compound and the polymer generated in the first step of reaction undergo coupled reaction to carry out end termination, thereby obtaining the final product. The raw materials adopted by the preparation method have extensive sources and simple preparation process flow; the polymer prepared by the method undergoes coupled reaction to form a three-dimensional network structure under the action of light, heat or chemical initiation; and the condensate of the polymer has excellent hightemperature resistance and thermal oxidation resistance and can be further pyrolyzed in air or inert gases to form a complex phase ceramic structure. Moreover, the polymer can be used as matrix resin, high temperature-resisting coat and ceramic precursor of advanced composite materials.
Description
technical field [0001] The invention relates to a high temperature resistant polymer, in particular to an organoborosilicate hybrid polymer containing phenylboronic acid, silane and ethynyl groups in the main chain, the repeating unit of which is composed of silicon-oxygen-boron-oxygen, monofunctional ethynyl group The compound caps the polymer. The ethynyl group undergoes a curing crosslinking reaction under light, heat or chemical action to form a three-dimensional network structure, and further pyrolysis can prepare composite ceramics. Background technique [0002] Among the many known silicone polymers, polysiloxanes, polysilanes and polysilazanes have been widely used in the past nearly 30 years. Due to their excellent thermal oxidation resistance, mechanical properties, dielectric properties and good solvent resistance, many polymers have been prepared as applied materials or materials with potential application value, including silicone rubber, silicone resin, silico...
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IPC IPC(8): C08G79/08
Inventor 周权倪礼忠程睿
Owner EAST CHINA UNIV OF SCI & TECH