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Alkynyl-containing poly-siloxane and method for preparing same

A technology of alkynyl polysilazane and methyl, which is applied in the field of polysilazane and its preparation, and achieves the effect of good thermal stability

Inactive Publication Date: 2005-06-22
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the alkynyl-containing organosilicon conjugated polymers reported in the literature are silicon-carbon and silicon-oxygen polymers, and silicon-nitrogen polymers have not been reported yet. Therefore, we envisage introducing ethynyl groups into silazane to synthesize alkynyl-containing Polysilazane, the lone pair of electrons on the N atom and the π electrons of the silyne system form a large electron delocalization system, which may exhibit new optical properties and electrical conductivity

Method used

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Examples

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Effect test

Embodiment 1

[0019] In a 250ml three-necked flask, add 50ml tetrahydrofuran, 50ml diethyl ether and 50ml (n-BuLi, 2.5mol / L), under N 2 Under protection, a mixed solution of 36 ml of ether and 3.6 ml of trichlorethylene was slowly added dropwise to the mixed solution in the three-necked flask at -78°C. After the dropwise addition, the stirring was continued for 12 hours to obtain a white cloudy liquid of lithium acetylene.

[0020] Add 20ml ether and 0.1mol Me 2 SiCl 2 , N 2 Slowly drip the cloudy lithium acetylene solution under protection. After the dropwise addition was completed, stirring was continued at -30°C for 10 hours, and then left to settle. The system is layered, the upper layer is light yellow clear liquid, the lower layer is white precipitate, N 2 Protect the supernatant with a glass sand core under N 2 Press it into a clean and dry three-neck flask, and wash the precipitate three times with ether. Combine the filtrates. The solvent was removed from the filtrate under...

Embodiment 2

[0035] Add 50ml ether and 0.2mol MePhSiCl to a 500ml three-neck flask 2 , N 2 Slowly drip the cloudy lithium acetylene solution under protection. After the dropwise addition was completed, stirring was continued at 20° C. for 20 hours, and then left to settle. The system is layered, the upper layer is light yellow clear liquid, the lower layer is white precipitate, N 2Under protection, the supernatant was hydraulically poured into a clean and dry three-necked bottle with a glass sand core, and the precipitate was washed six times with ether. Combine the filtrates. The solvent was removed from the filtrate under reduced pressure to obtain the alkynyl-containing chlorosilane oligomer as a yellow viscous liquid with a yield of 93%.

[0036] Characterization of alkyne-containing chlorosilane oligomers:

[0037] 29 Si-NMR (ppm): -10.0 (Cl-SiMePh), -44.0 (C≡C-SiMePh-C≡C).

[0038] 2 g of alkynyl-containing chlorosilane oligomers were dissolved in 50 ml of xylene, stirred and ...

Embodiment 3

[0046] Add 100ml ether and 0.1molPh into a 500ml three-neck flask 2 SiCl 2 , N 2 Slowly drip the cloudy lithium acetylene solution under protection. After the dropwise addition was completed, stirring was continued at 0° C. for 12 hours, and the mixture was left to settle. The system is stratified, the upper layer is orange clear liquid, the lower layer is pink precipitate, N 2 Protect the supernatant with a glass sand core under N 2 Press it into a clean and dry three-neck flask, and wash the precipitate four times with ether. Combine the filtrates. The solvent was removed from the filtrate under reduced pressure to obtain the alkynyl-containing chlorosilane oligomer as a brown viscous liquid with a yield of 91%.

[0047] Characterization of alkyne-containing chlorosilane oligomers:

[0048] 29 Si-NMR (ppm): -20.0 (Cl-SiPh 2 ), -49.0 (C≡C-SiPh 2 -C≡C).

[0049] Dissolve 1 g of alkynyl-containing chlorosilane oligomer in 50 ml of benzene, and pass ammonia gas at 80°...

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Abstract

The invention discloses an alkynyl-containing polysiagzane with the structure of [SiR1R2(C=C-SiR1R2)*NH], wherein R1, R2 is C1-C6 alkane, alkene, phenyl or H, n=1-10, m=10-100. The alkynyl-containing polysiagzane is prepared through aminolysis method, thus has good thermally-stability and photoelectric function.

Description

technical field [0001] The invention relates to a polysilazane and a preparation method thereof. Background technique [0002] In recent years, studies on conjugated polymers have attracted attention. Due to their unique electronic structure, they have some special properties, such as optoelectronic properties, which can be made into large-area flat-panel displays and light-emitting diodes, conductive coatings, chemical and biological sensors, nonlinear optical materials, light-emitting materials and batteries, etc. (Burroughes, J.H.; Brown, A.R.; Marks, R.N.Nature 1990, 347, 539), the introduction of organosilicon groups into the conjugated backbone can improve the performance of conjugated polymers: for example, the introduction of silicon in styrene polymers , a blue shift can be observed, which changes its optical properties; the introduction of organosilicon groups into the conjugated backbone can also improve the solubility of the polymer and the processability of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20
Inventor 胡继东谢择民郑知敏罗永明张志杰
Owner INST OF CHEM CHINESE ACAD OF SCI
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