Benzocyclobutene functional organic silicone resin and preparation method thereof

A benzocyclobutene functional, benzocyclobutene technology, applied in the field of silicone resin and its preparation, can solve problems such as low glass transition temperature

Active Publication Date: 2018-05-04
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Silicone polymers have good heat resistance but have a low glass transition temperature

Method used

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  • Benzocyclobutene functional organic silicone resin and preparation method thereof
  • Benzocyclobutene functional organic silicone resin and preparation method thereof
  • Benzocyclobutene functional organic silicone resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Preparation of tribenzocyclobutene-functionalized silicones by reaction of benzocyclobuten-4-yldimethylsilane and phenyltrimethoxysilane

[0066] .

[0067] Add benzocyclobuten-4-yldimethylsilane (0.70g), tris(pentafluorophenyl)borane (2.32mg), and 4ml of toluene into a 50ml three-necked flask equipped with a stirring bar and nitrogen protection, Ice bath. Slowly drop 0.285 g of phenyltrimethoxysilane into the three-necked flask. After the addition is complete, a large number of bubbles will be generated in the reaction system. After the bubbles disappeared, the temperature was raised to 60°C for 4 hours of reaction. After the reaction, cool to room temperature, add neutral alumina, filter, and spin the filtrate to dryness with a rotary evaporator. Using petroleum ether / ethyl acetate as the mobile phase, it was purified by silica gel column chromatography to obtain 0.61 g of a colorless transparent liquid (yield 66%).

Embodiment 2

[0069] Preparation of tribenzocyclobutene-functionalized silicones by reaction of benzocyclobuten-4-yldimethylsilane and phenyltrimethoxysilane

[0070] .

[0071] Add benzocyclobuten-4-yldimethoxysilane (0.70g), tris(pentafluorophenyl)borane (2.32mg), and 4ml of toluene into a 50ml three-necked flask equipped with a stirring bar and protected by nitrogen ,Ice bath. Slowly drop 0.22 g of tetraethyl orthosilicate into the three-necked flask. After the addition is complete, a large number of bubbles will be generated in the reaction system. After the bubbles disappeared, the temperature was raised to 60°C for 4 hours of reaction. After the reaction, cool to room temperature, add neutral alumina, filter, and spin the filtrate to dryness with a rotary evaporator. Using petroleum ether / ethyl acetate as the mobile phase, it was purified by silica gel column chromatography to obtain 0.52 g of a colorless transparent liquid (yield 65%).

Embodiment 3

[0073] Add 1,4-bis(dimethylsilyl)benzene (1.944g), tris(pentafluorophenyl)borane (8mg), and 10ml of toluene into a 50ml three-necked flask equipped with a stirring bar and protected by nitrogen. Add methyldimethoxy(benzocyclobuten-4-yl)silane (2.203g) and 10ml of toluene into a constant pressure dropping funnel and mix well. At room temperature, the mixture was dripped into a three-necked bottle, and the dripping was completed in one hour. After the addition was complete, the temperature was raised to 60°C for 4 hours of reaction. After the reaction, cool to room temperature, add neutral alumina, filter, and spin the filtrate to dryness with a rotary evaporator. 1 H NMR (500 MHz, CDCl3, δ): 7.514 (s, 4H), 7.403-7.351 (t, 1H), 7.215-7.185 (d, 1H), 6.988-6.973 (d, 1H), 6.146-5.978 (m , 2H), 5.887-5.784 (m, 1H), 3.203-3.129 (t, 4H), 0.399-0.241 (m, 12H)

[0074] .

[0075] Molecular weight is analyzed by GPC test MP=6811, polydispersity=1.015937.

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Abstract

The invention belongs to the technical field of high-performance resin, and particularly relates to a preparation method of benzocyclobutene functional organic silicone resin. Benzocyclobutene functional organic silicone raw materials-a compound containing silicon-hydrogen bonds and an organic silicone compound containing siloxy (at least one compound is functionalized by benzocyclobutene) are used to prepare an organic silicone polymer containing a BCB functional group by virtue of P-R condensation polymerization. By adopting different structures of silicon-hydrogen compounds and siloxane, the preparation of benzocyclobutene functional organic silicone resin of different topological structures can be realized. The organic silicone resin prepared by the invention can be cured to prepare alow-dielectric high-temperature-resistant film by spin coating and heating or to prepare a polymer composite material, and the organic silicone resin is widely applied to the fields of electron encapsulation, integrated circuits and the like.

Description

technical field [0001] The invention belongs to the technical field of high-performance resins, and in particular relates to organic silicon resins and a preparation method thereof. Background technique [0002] Benzocyclobutene is an excellent polymer material, and benzocyclobutene resin can undergo ring-opening polymerization after heating to produce a highly cross-linked, high-temperature-resistant low-dielectric polymer material. [0003] Silicone polymer has a unique organic / inorganic chemical structure, so it exhibits excellent heat resistance and low moisture absorption. Silicone polymer has low polarity and good insulation. At the same time, it is resistant to low polar solvents (such as petroleum ether, Toluene, etc.) good solubility, convenient post-processing and processing. Therefore, it is of great significance to prepare high-performance low-dielectric materials based on organosilicon polymers. But silicone glass transition temperature is low. [0004] The P...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/52
CPCC08G77/20C08G77/52C08G77/80
Inventor 程元荣肖斐田仕畅李君毅
Owner FUDAN UNIV
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