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Cyclosiloxane polymeric monomers with silacyclobutane cross-linked structures and preparation methods of cyclosiloxane polymeric monomers

A technology of silacyclobutane and hexamethyltricyclotetrasilyl cyclohexasiloxane, which is applied in the field of cyclosiloxane polymerization monomer and its preparation

Active Publication Date: 2020-06-09
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide cyclosiloxane polymer monomers with silacyclobutane crosslinked structure and preparation method thereof, the present invention introduces optically active silacyclobutane into In the preparation of polycyclosiloxane monomers, it solves the shortcomings of difficult control and cumbersome preparation of traditional photosensitive silicone-based resins, and overcomes the difficulty of accurately controlling silacyclobutane by existing methods such as polysiloxane side group modification. Due to the shortcomings of the degree of functionalization and the chemical structure of the polymer, silacyclobutane is directly introduced from the monomer to realize the controllability and optimization of the resin structure and performance, thus providing a class of excellent performance, with silacyclobutane crosslinking Novel cyclosiloxane polymer monomer with structure, and preparation method of novel cyclosiloxane polymer monomer with silacyclobutane crosslinking structure

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  • Cyclosiloxane polymeric monomers with silacyclobutane cross-linked structures and preparation methods of cyclosiloxane polymeric monomers
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  • Cyclosiloxane polymeric monomers with silacyclobutane cross-linked structures and preparation methods of cyclosiloxane polymeric monomers

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Embodiment 1

[0045] The preparation method of pentacyclotetrasilyl cyclopentasiloxane polymerization monomer (I), concrete steps and condition are:

[0046]In a dry 250mL round bottom flask equipped with a magnetic stirrer, add 100mL of dry diethyl ether and 1,1-dichloro-1-silacyclobutane (11.9g, 84.35mmol) in sequence, and slowly add deionized Water (10mL, 556mmol, 2-3 seconds / drop); after reacting at room temperature for 1h, let stand to separate the layers, separate the organic ether layer, wash with deionized water three times, dry over anhydrous sodium sulfate, concentrate to remove the solvent, Residue (or be referred to as residue, the same hereinafter) carries out silica gel column chromatography (using sherwood oil as mobile phase), the colorless transparent oily thing that obtains is the pentacyclotetrasilyl cyclopentasiloxane polymerized monomer that obtains , yield 60%.

[0047] The pentacyclotetrasilyl cyclopentasiloxane polymerized monomer (I) basic feature that this embodim...

Embodiment 2

[0050] The preparation method of tetraphenyldicyclotetrasilyl cyclotetrasiloxane polymerization monomer (II), concrete steps and conditions are:

[0051] In a dry 100mL round bottom flask equipped with a magnetic stirrer, add dry tetrahydrofuran (30mL), dihydroxydiphenylsilane (3.67g, 16.86mmol), and dry pyridine (2.72mL, 33.72mmol) in sequence; After protection, a solution of 1,1-dichloro-1-silacyclobutane (3.38 g, 16.86 mmol) diluted in dry tetrahydrofuran (10 mL) was slowly added dropwise (2-3 sec / drop) at room temperature. After continuously stirring and reacting at room temperature for 24 hours, filter, concentrate the filtrate to remove the solvent, and the residue (or residue, the same hereinafter) is subjected to silica gel column chromatography (using petroleum ether as the mobile phase), and the obtained white solid is The obtained tetraphenylbicyclotetrasilylcyclotetrasiloxane polymerized monomer (II) had a yield of 48%.

[0052] Tetraphenylbicyclotetrasilyl cyclot...

Embodiment 3

[0055] The preparation method of hexamethyltricyclotetrasilyl cyclohexasiloxane polymerized monomer (Ⅲ), the specific steps and conditions are:

[0056] In a dry 100mL round bottom flask equipped with a magnetic stirrer, add 20mL of dry diethyl ether, 1,1-dichloro-1-silacyclobutane (3.38g, 16.86mmol), dimethyldichlorosilane (2.17 g, 16.86mmol), slowly drop deionized water (2mL, 111mmol, 2-3 seconds / drop) at 0°C; Washed 3 times, dried over anhydrous sodium sulfate, concentrated to remove the solvent, and the residue (or called residue, the same hereinafter) was subjected to silica gel column chromatography (using sherwood oil as mobile phase), and the colorless transparent oil obtained was The obtained hexamethyltricyclotetrasilylcyclohexasiloxane polymerized monomer (III) has a yield of 40%.

[0057] The hexamethyltricyclotetrasilylcyclohexasiloxane polymerized monomer (Ⅲ) basic characteristic that this embodiment makes: colorless transparent oil; Structural characterization ...

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Abstract

The invention discloses a pentacyclic butylsilyl cyclopentasiloxane polymeric monomer as shown in a formula (I) and a preparation method thereof. The preparation method comprises the following step: with 1,1-dichloro-1-silacyclobutane as an initial raw material, carrying out self-hydrolysis or co-hydrolysis on the 1,1-dichloro-1-silacyclobutane and substituted silanol or silicon chloride under theaction of a solvent and / or alkali to obtain the cyclosiloxane polymerization monomers with silacyclobutane cross-linked structures. Furthermore, the invention also discloses a tetraphenyl dicyclobutylsilyl-based cyclotetrasiloxane polymeric monomer, a hexamethyl tricyclobutylsilyl-based cyclohexasiloxane polymeric monomer, and preparation methods thereof. According to the invention, the preparation process of cyclosiloxane polymerization monomer products is simple and convenient, product yield is high, cost is low, and cured polycyclosiloxane resin has excellent thermal properties, mechanicalproperties, electrical properties and film-forming properties; and the cyclosiloxane polymerization monomer products are applicable as high-performance low-dielectric film materials or packaging materials in the fields of microelectronics industry, aerospace, national defense and the like.

Description

technical field [0001] The invention belongs to a silicon-containing organic compound and its preparation, and relates to a cyclosiloxane polymer monomer with a silacyclobutane crosslinking structure and a preparation method thereof. The cyclosiloxane polymerized monomer having a silacyclobutane crosslinked structure of the present invention, the polycyclosiloxane resin obtained after curing has excellent thermal properties, mechanical properties, electrical properties and film-forming properties; it is suitable for micro Electronic industry, aerospace and national defense and other fields as high-performance dielectric film materials or packaging materials. Background technique [0002] Organocyclosiloxanes are widely used as lubricants, adhesives, often in the form of oils, resins, and rubbers due to their excellent chemical and physical properties, such as low-temperature flexibility, high-temperature stability, radiation resistance, and good damping Compounds, insulatin...

Claims

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Application Information

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IPC IPC(8): C07F7/21
CPCC07F7/21
Inventor 袁文杨军校马佳俊胡欢黄亚文彭秋霞
Owner SOUTHWEAT UNIV OF SCI & TECH