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Silicon-boron-azane ceramic precursor polymer containing borazine and preparation method and application of polymer

The technology of a ceramic precursor and borazane is applied in the field of preparation of the precursor polymer, which can solve the problems of low ceramization yield, poor process performance, affecting the performance of ceramic matrix composite materials, etc., and achieves excellent process performance, The effect of high ceramic yield

Active Publication Date: 2018-10-26
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Most of the borosilicate nitrogen carbon ceramic precursor polymers reported in the literature are in a solid state, and cannot be dissolved in most solvents, the process performance is poor, and the molding process is difficult; or the liquid silaborazane ceramic precursor is synthesized, but the ceramic production rate Low, affecting the performance of ceramic matrix composites

Method used

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  • Silicon-boron-azane ceramic precursor polymer containing borazine and preparation method and application of polymer
  • Silicon-boron-azane ceramic precursor polymer containing borazine and preparation method and application of polymer
  • Silicon-boron-azane ceramic precursor polymer containing borazine and preparation method and application of polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Precursor PBSZ-1

[0038] In a 500ml four-necked flask equipped with a nitrogen conduit, a stirrer, a thermometer and a condenser tube, after several cycles of dehumidification and deoxygenation by vacuuming and passing nitrogen, add NH 4 Cl powder 32g (0.30mol) and toluene 300ml, and vigorously stirred to form a suspension, heated to 110 ° C, slowly into the four-necked flask BCl 3 Gas, and insulation reaction 10h. Then cool down to room temperature, adopt shleck technique to suction filter under nitrogen protection, the filtrate is distilled off under reduced pressure to remove the solvent, and then sublimated to obtain colorless needle-shaped crystal trichloroborazine (TCB).

[0039] In the 2000ml four-neck flask equipped with nitrogen conduit, stirrer, thermometer and condensing tube, after vacuumizing, passing nitrogen several times to circulate dehumidification and deoxygenation, under the protection of nitrogen, add trichloroborazine 9g and Dichlorome...

Embodiment 2

[0043] Example 2 Precursor PBSZ-2

[0044] In a 500ml four-necked flask equipped with a nitrogen conduit, a stirrer, a thermometer, and a condenser tube, after several cycles of dehumidification and oxygen removal by vacuuming and nitrogen, add BCl 3 (0.09mol) of toluene solution, cooled to -10°C with salt ice, slowly dropwise added a mixture of 18.22g (0.18mol) of triethylamine and toluene (20mL) to it, and then added olefin Propylamine 5.14g (0.09mol) and toluene (10mL), then the system was slowly raised to 110°C for 6h, then cooled to room temperature. The shleck technique was used for suction filtration under the protection of nitrogen, the filtrate was transferred to a rotary evaporator, and the solvent was distilled off under reduced pressure to obtain a colorless and transparent liquid triallyltrichloroborazine (TV-TCB).

[0045] After checking the airtightness of the reaction system of the 2000ml four-necked flask equipped with a PTFE stirring rod, a thermometer, a sy...

Embodiment 3

[0047] Example 3 Precursor PBSZ-3

[0048] After checking the airtightness of the reaction system of the 2000ml four-necked flask equipped with a PTFE stirring rod, a thermometer, a syringe and a nitrogen gas guide tube, bake and vacuumize repeatedly, and then add the reaction system to it sequentially under the protection of nitrogen gas. Trichloroborazine 2.18g and dichloromethane 1400ml, start stirring, make trichloroborazine dissolve and disperse in dichloromethane, then, at normal temperature, slowly add 1mol / L of methylmagnesium bromide Grignard reagent 12ml, after the dropwise addition, the reaction system was reacted at room temperature for 3 hours to obtain a white solution of methyl-substituted borazine. Place the four-neck flask in a low-temperature bath at -10°C, then add 40 g of dichlorodihydrosilane to it, and finally feed ammonia gas into the reaction system to start the reaction until the reaction system is alkaline, stop the reaction, and then pump Filter, r...

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Abstract

The invention discloses a silicon-boron-azane ceramic precursor polymer containing borazine and a preparation method and application of the polymer. The silicon-boron-azane ceramic precursor polymer containing borazine has the structural characteristics that a molecular chain of the polymer has structures of borazine and silazane. The preparation method of the ceramic precursor polymer comprises the step that with ammonium chloride, organic primary amine, boron trihalide, dichlorosilane and ammonia gas as main raw materials, the silicon-boron-azane ceramic precursor polymer is synthesized through a three-step reaction under the protection of inert gas, wherein firstly, ammonium chloride or organic primary amine reacts with boron trihalide to synthesize b-trichloroborazine, secondly, b-trichloroborazine and a hydrocarbyl magnesium bromide Grignard reagent react with each other to obtain hydrocarbyl-substituted chloroborazine, and then hydrocarbyl-substituted chloroborazine and dichlorosilane are subjected to co-ammonolysis to synthesize the silicon-boron-azane ceramic precursor polymer. The silicon-boron-azane ceramic precursor polymer containing borazine is colorless or light yellow viscous liquid and is soluble in a common solvent and excellent in process performance. A precursor polymer solidified product can be pyrolyzed and transformed into ceramic, the yield of the ceramicis high, and the precursor polymer solidified product can be used for preparing silicon-boron-nitrogen ceramic-based composite materials.

Description

technical field [0001] The invention relates to a borazine-containing silaborazane ceramic precursor polymer, and also relates to a preparation method of the precursor polymer. Background technique [0002] The polymer precursor converted SiBCN ceramics and their ceramic matrix composites have excellent high temperature resistance, oxidation resistance, high temperature mechanical properties and wave transmission properties, making them have broad application prospects in the aerospace field. The outstanding feature of polymer precursor converted ceramics is that its microstructure and properties can be designed through changes in the molecular structure of the precursor. The chemical and physical properties of polymer precursor converted ceramics depend on the molecular structure and molding of the initial polymer precursor. process conditions. [0003] The preparation of SiBCN ceramic precursor was initially synthesized by boron-modified polysilazane. Jeon et al. used 2,4...

Claims

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Application Information

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IPC IPC(8): C08G79/08C08G77/62C04B35/589C04B35/583
CPCC04B35/583C04B35/589C08G77/62C08G79/08
Inventor 齐会民王帆朱亚平郭康康彭翔
Owner EAST CHINA UNIV OF SCI & TECH
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