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Photo/thermal double crosslinkable hyperbranched polycarbosilane benzocyclobutene resin and preparation method thereof

A technology of benzocyclobutene and bromobenzocyclobutene is applied in the field of hyperbranched polycarbosilane benzocyclobutene resin and its preparation, which can solve the problems of cumbersome preparation process, limited wide application, and influence of material performance preparation process bigger problems

Active Publication Date: 2020-05-19
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Benzocyclobutene resin has excellent properties such as heat resistance, dielectric, moisture absorption resistance, and film flatness. Various benzocyclobutene silicone polymers and their preparation methods have been reported in the literature, such as: US5882836, US5138081, ZL201110367893.X, ZL201110367900.6, etc. reported several polysiloxane-type benzocyclobutene silicone resins; literature [Journal of Polymer Science, Part A: Polymer Chemistry, 2011,49,381-391], [Polymer,2014,55,5680-5688], [Polymer,2015,66,58-66] reported a class of polycarbosilane benzocyclobutene resins, all of which showed excellent thermal, electrical and film-forming properties. However, the preparation process of the above materials is cumbersome, the yield is not high, and the material properties are greatly affected by the preparation process, which greatly limits their further wide application.

Method used

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  • Photo/thermal double crosslinkable hyperbranched polycarbosilane benzocyclobutene resin and preparation method thereof
  • Photo/thermal double crosslinkable hyperbranched polycarbosilane benzocyclobutene resin and preparation method thereof
  • Photo/thermal double crosslinkable hyperbranched polycarbosilane benzocyclobutene resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A kind of preparation method of hyperbranched polycarbosilane benzocyclobutene resin capable of photo / thermal double crosslinking, the steps are:

[0043] Using magnesium (Mg) as a catalyst and tetrahydrofuran (THF) as a solvent, chloromethyltrichlorosilane (Cl 3 SiCH 2 Cl), 4-bromobenzocyclobutene (4-BrBCB), p-bromostyrene (C 8 h 7 Br), bromooctane (C 8 h 17 Br) preparation, according to chloromethyltrichlorosilane: monomer I: monomer II: monomer III: magnesium (Mg) molar ratio 1:3:3:2:1.5 feeding intake;

[0044] Add magnesium chips (Mg) (0.36g, 15mmol) and a catalytic amount of iodine into a dry flask equipped with a magnetic stirrer, a constant pressure dropping funnel, and a reflux condenser, seal it, vacuumize it, and fill it with nitrogen to remove oxygen in the system , repeated three times. Under nitrogen protection, add chloromethyltrichlorosilane (Cl 3 SiCH 2 Cl) (1.84g, 10mmol) in tetrahydrofuran (THF) (37.5mL) solution, drop a little in the flask an...

Embodiment 2

[0047] A kind of preparation method of hyperbranched polycarbosilane benzocyclobutene resin capable of photo / thermal double cross-linking, the steps are: take magnesium (Mg) as catalyst, tetrahydrofuran (THF) as solvent, by chloromethyltrichlorosilane (Cl 3 SiCH 2 Cl), 4-bromobenzocyclobutene (4-BrBCB), p-bromostyrene (C 8 h 7 Br), bromooctane (C 8 h 17 Br) is prepared by feeding in the molar ratio of chloromethyltrichlorosilane:monomer I:monomer II:monomer III:magnesium (Mg) 1:4:3:2:1.5.

[0048] The preparation method is the same as in Example 1.

[0049] Basic features: white or light yellow viscous jelly; the structural characterization results are the same as in Example 1.

[0050] Example: 3:

[0051] A kind of preparation method of hyperbranched polycarbosilane benzocyclobutene resin capable of photo / thermal double cross-linking, the steps are: take magnesium (Mg) as catalyst, tetrahydrofuran (THF) as solvent, by chloromethyltrichlorosilane (Cl 3 SiCH 2 Cl), 4-b...

Embodiment 4

[0055] A kind of preparation method of hyperbranched polycarbosilane benzocyclobutene resin capable of photo / thermal double cross-linking, the steps are: take magnesium (Mg) as catalyst, tetrahydrofuran (THF) as solvent, by chloromethyltrichlorosilane (Cl 3 SiCH 2 Cl), 4-bromobenzocyclobutene (4-BrBCB), p-bromostyrene (C 8 h 7 Br), bromooctane (C 8 h 17 Br) is prepared by feeding in according to the molar ratio of chloromethyltrichlorosilane:monomer I:monomer II:monomer III:magnesium (Mg) 1:3:3:3:1.5.

[0056] The preparation method is the same as in Example 1.

[0057] Basic features: white or light yellow viscous jelly; the structural characterization results are the same as in Example 1.

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Abstract

The invention discloses light / heat double crosslinked hyperbranched polycarbosilane benzocyclobutene resin as shown in a formula (IV) and a preparation method thereof. The preparation method of the hyperbranched polycarbosilane benzocyclobutene resin comprises the following steps: generating a Grignard reagent from chloromethyltrichlorosilane under the action of magnesium; then performing a coupling reaction with Si-Cl to further form a hyperbranched Si-Cl bond-containing hyperbranched polycarbosilane polymer; adding 4-bromobenzocyclobutene to react; adding p-bromostyrene to react; then adding alkyl (alkenyl) halide to react; performing cooling; adding distilled water (deionized water) into the system for a quenching reaction; and performing solvent extraction, concentration, and purification steps such as distillation or column chromatography on silica gel to obtain the light / heat double crosslinked hyperbranched polycarbosilane benzocyclobutene resin. The light / heat double crosslinked hyperbranched polycarbosilane benzocyclobutene resin prepared by the method is excellent in thermal, electrical and photosensitive properties and is suitable for being used as a high performance dielectric film material or a packaging material in the field of microelectronics industry, space flight and aviation and national defense and the like. The formula (IV) is as shown in the specification.

Description

technical field [0001] The invention belongs to organic polymer compounds and their preparation, and relates to a hyperbranched polycarbosilane benzocyclobutene resin capable of photo / thermal double crosslinking and a preparation method thereof; the photo / thermal double crosslinkable resin prepared by the present invention Hyperbranched polycarbosilane benzocyclobutene resin has excellent thermal, electrical, and photosensitive properties, and is suitable for use as high-performance dielectric film materials or packaging materials in the fields of microelectronics industry, aerospace, and national defense. Background technique [0002] In the prior art, polycarbosilane (Polycarbosilane, referred to as PCS) is an organosilicon polymer formed by Si, C, H and other elements. Low dielectric (dielectric constant can be as low as 2.5), excellent properties such as moisture absorption resistance, is an important class of silicon carbide ceramic precursors (Preceramicpolymers), and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60C08L83/16
CPCC08G77/60C08L83/16C08L2201/08C08L2203/16
Inventor 李娴杨军校钟楠范立胡欢黄亚文
Owner SOUTHWEAT UNIV OF SCI & TECH
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