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Heat-resisting poly (silazane-siloxane) polymer and preparation method thereof

A technology of high temperature resistance and silazane, applied in the field of high temperature resistance copolymer and its preparation, can solve the problems of harsh synthesis and purification conditions and low yield, achieve excellent thermal stability and thermal oxidation stability, and improve performance , easy to prepare and obtainable effects

Active Publication Date: 2012-08-15
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

However, the synthesis and purification conditions of the cyclodisilazane monomer of this structure are very harsh (diphenyldichlorosilane and N, N'-bis(dimethylchlorosilyl) tetramethylcyclodisilazane need The exchange reaction is carried out above 300°C, and the synthesized N,N'-bis(diphenylchlorosilyl)tetramethylcyclodisilazane needs to be purified by fractional distillation under reduced pressure above 200°C), resulting in extremely low yield (36%)

Method used

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  • Heat-resisting poly (silazane-siloxane) polymer and preparation method thereof
  • Heat-resisting poly (silazane-siloxane) polymer and preparation method thereof
  • Heat-resisting poly (silazane-siloxane) polymer and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0055] Raw materials used for synthesis: the molecular formula is as shown in the above-mentioned formulas II-IV, wherein, in the formula II, R 1 = R 2 =CH 3 ; In Formula IV, In Formula III, n=3.

[0056] Under a nitrogen atmosphere, 5.42g (0.01mol) of 1,3-bis(methylphenylhydroxysilyl)-2,4-dimethyl-2,4-diphenylcyclodisilazane (molecular formula shown in formula II) was dissolved in 20mL toluene, and 8.48g (0.02mol) α, ω-diethylaminosiloxane (molecular formula shown in formula III, n=3) (Aldrich Chemical Co.) and 2.93g (0.01mol) 1,3-bis(hydroxydimethylsilyl)-m-carborane (molecular formula as shown in formula IV), fully mixed evenly. Slowly raise the temperature to 110°C, keep mechanical stirring, blow out the generated diethylamine continuously with nitrogen until no more diethylamine is generated. The reaction was carried out for a total of 12 hours. After the reaction was completed, toluene was added to dissolve the polymer, and anhydrous methanol was used to precipitat...

Embodiment 2

[0061] Raw materials used for synthesis: the molecular formula is as shown in the above-mentioned formulas II-IV, wherein, in the formula II, R 1 = R 2 =C 6 h 5 ; In Formula IV, In Formula III, n=3.

[0062] Under a nitrogen atmosphere, 6.66g of 1,3-bis(diphenylhydroxysilyl)-2,4-dimethyl-2,4-diphenylcyclodisilazane (molecular formula shown in formula II) (0.01mol) dissolved in 20mL xylene, continue to add 8.48g (0.02mol) α, ω-diethylaminosiloxane (molecular formula shown in formula III, n=3) (Aldrich Chemical Co.) and 2.93g (0.01mol) 1,3-bis(hydroxydimethylsilyl)-m-carborane (molecular formula as shown in formula IV), fully mixed evenly. Slowly raise the temperature to 140°C, keep mechanical stirring, blow out the generated diethylamine continuously with nitrogen until no more diethylamine is generated. The reaction was carried out for a total of 12 hours. After the reaction was completed, n-hexane was added to dissolve the polymer, and precipitated with anhydrous metha...

Embodiment 3

[0067] Synthetic raw materials used: as shown in the above-mentioned formula II~IV, wherein, in formula II, R 1 = R 2 =CH 3 ; In Formula IV, In Formula III, n=3.

[0068] Under nitrogen atmosphere, 5.42g 1,3-bis(methylphenylhydroxysilyl)-2,4-dimethyl-2,4-diphenylcyclodisilazane (molecular formula shown in formula II ) (0.01mol) and 2.26g (0.01mol) 1,3-bis(hydroxydimethylsilyl)benzene (molecular formula shown in formula IV) (Shanghai Merrill Chemical Technology Co., Ltd.) was dissolved in 40mL petroleum ether (bp .90~120°C) and toluene (volume ratio=1:1), continue to add 8.48g α, ω-diethylaminosiloxane (molecular formula shown in formula III, n=3) (Aldrich Chemical Co.) (0.02mol), mix well. Slowly raise the temperature to 105°C, keep mechanical stirring, blow out the generated diethylamine continuously with nitrogen until no more diethylamine is generated. The reaction was carried out for a total of 12 hours. After the reaction was completed, xylene was added to dissolve...

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Abstract

The invention discloses a heat-resisting poly (silazane-siloxane) polymer, which has a molecular formula structure shown in a formula I, in the formula I, R1 is methyl or phenyl; R2 is methyl or phenyl; Z is carborane silicon alkyl, silicon arylene or alkyl phenyl silicone; and m is smaller than or equal to 100 and greater than or equal to 1, and n is smaller than or equal to 10 and greater than or equal to 3. The polymer has excellent thermal degradation stability and thermal-oxidative stability, can still keep certain strength under high-temperature condition, can be used as a matrix polymer of a heat-resisting sealing material, and has great application values in the fields such as an aerospace and the like. (FORMULA I).

Description

technical field [0001] The invention relates to a novel high temperature resistant polymer, in particular to a high temperature resistant copolymer containing a cyclodisilazane group, a carboryl group, a silicon arylene group or a phenylsilane group in a polysiloxane main chain and its Preparation. Background technique [0002] The most notable characteristic of silicone rubber is their high temperature stability, which can be used for a long time in an environment of about 200-300°C, so they are widely used in aerospace, electronics, construction and other industries. However, in a high-temperature environment, the linear polydimethylsiloxane will undergo a thermal cracking reaction into a cyclic siloxane, and the side group will undergo an oxidation reaction to generate crosslinking. For hydroxyl-terminated polysiloxanes, the main occurrence is the snapping rearrangement degradation, resulting in D 3 Isocyclic body, resulting in continuous reduction of polysiloxane molec...

Claims

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Application Information

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IPC IPC(8): C08G77/54C09D183/14C09J183/14C08L83/14
Inventor 郑艳谭永霞张志杰戴丽娜吕臻谢择民
Owner INST OF CHEM CHINESE ACAD OF SCI
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