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Benzocyclobutene polycarbosilane polymerized monomer or resin and preparation method thereof
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A technology of benzocyclobutene polycarbosilane and benzocyclobutenyl disilacyclobutane, which is applied in the field of polymer compounds
Inactive Publication Date: 2020-05-15
SOUTHWEAT UNIV OF SCI & TECH
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However, the heat resistance and stability of silicone resin materials in the prior art need to be further improved, the dielectric constant needs to be further reduced, and the preparation process steps need to be further simplified to meet different needs.
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Embodiment 1
[0054] 1,3-dimethyl-1,3-dibenzocyclobutenyl disilacyclobutane, the benzocyclobutene polycarbosilane polymerization monomer has the chemical structural formula shown in formula (I):
[0055]
Embodiment 2
[0057] The preparation method of 1,3-dimethyl-1,3-dibenzocyclobutenyl disilacyclobutane, the steps are:
[0058] a. Synthesis of chloromethylmethylisopropoxychlorosilane:
[0059] In an ice-water bath, add 22.89 g of chloromethylmethyldichlorosilane to the reactor under the protection of nitrogen; take 7.8 g of isopropanol and add it to a constant pressure dropping funnel, and drop it into the reactor for 2 hours (slowly); After the addition is complete, continue the reaction at room temperature for 1 hour; throughout the reaction process, nitrogen gas has been passed to take away the hydrogen chloride gas generated in the reaction process; It is the distillate under the condition of 0.4~0.5 Torr, and the colorless transparent liquid is obtained, which is the obtained chloromethylmethylisopropoxychlorosilane;
[0060] b. Synthesis of 1,3-diisopropoxy-1,3-dimethyl-1,3-disilacyclobutane:
[0061] Add 1.64g of magnesium and 0.011g of iodine into the reactor, vacuumize and fill ...
Embodiment 3
[0066] The preparation method of 1,3-dimethyl-1,3-dibenzocyclobutenyl disilacyclobutane, the steps are:
[0067] a. Synthesis of chloromethylmethylisopropoxychlorosilane:
[0068] In an ice-water bath, add 22.89 g of chloromethylmethyldichlorosilane to the reactor under the protection of nitrogen; take 7.8 g of isopropanol and add it to a constant pressure dropping funnel, and drop it into the reactor over 4 hours (slowly); After the addition is complete, continue the reaction at room temperature for 1 hour; throughout the reaction process, nitrogen gas has been passed to take away the hydrogen chloride gas generated in the reaction process; It is the distillate under the condition of 0.4~0.5 Torr, and the colorless transparent liquid is obtained, which is the obtained chloromethylmethylisopropoxychlorosilane;
[0069] b. Synthesis of 1,3-diisopropoxy-1,3-dimethyl-1,3-disilacyclobutane:
[0070] Add 2.78g of magnesium and 0.013g of iodine into the reactor, vacuumize and fill...
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Abstract
The invention discloses 1,3-dimethyl-1,3-dibenzocyclobutenyl disilacyclobutane as shown by a formula (I) and a preparation method thereof. The preparation method is characterized in that a preparation method of a benzocyclobutene polycarbosilane polymeric monomer comprises the following steps of dropwise adding isopropanol into chloromethylmethyldichlorosilane under nitrogen protection, carrying out a reaction, and then carrying out reduced pressure distillation, so as to obtain chloromethylmethylisopropoxychlorosilane; subsequently, preparing 1,3-diisopropoxy-1,3-dimethyl-1,3-disilacyclobutane; subsequently, carrying out an agitation reaction on the 1,3-diisopropoxy-1,3-dimethyl-1,3-disilacyclobutane and a grignard reagent of 4-bromobenzocyclobutene, and then carrying out separation and purification, so that the benzocyclobutene polycarbosilane polymeric monomer is made; further, being capable of preparing a polycarbosilane homopolymer and a polycarbosilane linear copolymer. Benzocyclobutene polycarbosilane resin prepared by adopting the preparation method provided by the invention has favorable thermal stability, chemical stability, mechanical performance and electrical performance, and is applicable to the fields of microelectronics industry, aerospace, national defense and the like.
Description
technical field [0001] The invention belongs to polymer compounds obtained by reactions other than carbon-carbon unsaturated bonds, and relates to a benzocyclobutene polycarbosilane polymer monomer or resin and a preparation method thereof. The benzocyclobutene polycarbosilane resin prepared by the invention has good thermal stability, chemical stability, mechanical properties and electrical properties, and is suitable for the fields of microelectronics industry, aerospace, national defense and the like. Background technique [0002] Benzocyclobutene (BCB for short) materials have been widely used abroad because of their excellent high and low temperature resistance, weather resistance, good air tightness, radiation resistance, especially excellent film-forming properties and moisture resistance. Applied to military and civilian fields. Common silicone polymers have excellent properties such as high and low temperature resistance, weather resistance, electrical insulation, ...
Claims
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