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Diene silicoxyane linking disbenzocyclobutylene monomer and process for preparing prepolymer

A technology of dienyl siloxane bridge and benzocyclobutene, applied in the field of preparation of dienyl siloxane bridged bisbenzocyclobutene monomer and prepolymer, can solve the molecular weight of prepolymer Wide distribution, non-recyclable solvent, long polymerization time and other problems, to achieve the effect of shortening the production cycle, shortening the polymerization time, and reducing energy consumption

Inactive Publication Date: 2006-06-28
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvent used in this method cannot be recovered, and the polymerization time is long, the energy consumption is high, and the molecular weight distribution of the obtained prepolymer is wide

Method used

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  • Diene silicoxyane linking disbenzocyclobutylene monomer and process for preparing prepolymer
  • Diene silicoxyane linking disbenzocyclobutylene monomer and process for preparing prepolymer
  • Diene silicoxyane linking disbenzocyclobutylene monomer and process for preparing prepolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] In a 50ml two-neck flask equipped with a magnetic stirring bar, first add 32mmol NaOAc 2.624g, distilled water 5.8ml and stir to dissolve, then add [C 2 Py]PF 6 2.9g, Pd(OAc) 2 4mg, 8mmol DVS 1.488g, 16mmol4-BrBCB 2.912g, then pass nitrogen gas to remove the air in the reaction flask, and react at 90°C for 22 hours under nitrogen atmosphere; extract the reaction solution with petroleum ether (3×20ml), and combine Organic phase, anhydrous Na 2 SO 4 After drying, the organic phase was filtered on silica gel, rinsed with petroleum ether, and the eluent was concentrated to dryness under reduced pressure to obtain 2.5 g of a colorless or light yellow oily liquid, with a yield of 80%. 1 HNMR (400MHz, CDCl 3 ), 6.89-7.25 (br, 6H), 6.31-6.37 (d, 4H), 3.16 (s, 8H), 0.23 (s, 12H). The ionic liquid was washed and dried to obtain a white solid [C 2 Py]PF 6 2.8g.

Embodiment 2

[0047] In the 50ml two-neck flask equipped with a magnetic stirrer, first add 32mmol NaOAc 2.624g, distilled water 5.8ml and stir to dissolve, then add the recovered [C 2 Py]PF 6 2.9g, Pd(OAc) 2 4mg, 8mmol DVS1.488g, 16mmol 4-BrBCB 2.912g, then pass nitrogen gas to remove the air in the reaction flask, and react at 90°C for 22 hours under nitrogen atmosphere; the reaction solution was extracted with petroleum ether (3×20ml), Combined organic phases, anhydrous Na 2 SO 4 After drying, the organic phase was filtered through silica gel, rinsed with petroleum ether, and the eluent was concentrated to dryness under reduced pressure to obtain 2.47 g of a colorless or light yellow oily liquid with a yield of 79%. The ionic liquid was washed and dried to obtain a white solid [C 2 Py]PF 6 2.78g.

Embodiment 3

[0049] In the 50ml two-neck flask equipped with a magnetic stirrer, first add 32mmol NaOAc 2.624g, distilled water 5.8ml and stir to dissolve, then add the recovered [C 2 Py]PF 6 2.9g, Pd(OAc) 2 4mg, 8mmol DVS1.488g, 16mmol 4-BrBCB 2.912g, then pass nitrogen gas to remove the air in the reaction flask, and react at 90°C for 22 hours under nitrogen atmosphere; the reaction solution was extracted with petroleum ether (3×20ml), Combined organic phases, anhydrous Na 2 SO 4 After drying, the organic phase was filtered through silica gel, rinsed with petroleum ether, and the eluent was concentrated to dryness under reduced pressure to obtain 2.55 g of a colorless or light yellow oily liquid, with a yield of 81.7%. The ionic liquid was washed and dried to obtain a white solid [C 2 Py]PF 6 2.8g.

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Abstract

The invention discloses a method to make diene siloxane crosslink bibenzo cyclobutene monomer that includes the following steps: whisking alkali and water to dissolve, adding solvent, catalyst, reacting material, reacting for 18-30 hours at 90-150 degree centigrade in nitrogen air, extracting and post processing to gain the monomer. The feature is that it solvent is iron liquid or recycled iron liquid. The invention also discloses the manufacture method for performed polymer. It has no pollution to the environment, low cost, short production cycle, and no influence to yield, lower power consumption.

Description

1. Technical field [0001] The invention belongs to the technical field of preparation of dienyl siloxane bridged dibenzocyclobutene monomers and prepolymers, and specifically relates to the preparation of dienyl siloxane bridged dibenzocyclobutene in ionic liquid or recovered ionic liquid A new method of cyclobutene monomer and prepolymer. 2. Background technology [0002] Among monomers containing benzocyclobutene (BCB) structure, due to its special molecular structure, ring opening usually occurs at about 200°C to form a polymer with a linear or network structure. Such polymers are widely used because of their excellent electrical properties, low moisture absorption, high flatness, high thermal and chemical stability, easy uniform film formation, and high flatness. For example, the dienyl siloxane bridged bisbenzocyclobutene (DVS-BCB) resin with the following structure: [0003] [0004] This type of resin is formed by thermal curing of monomers at 200-250°C, and has ...

Claims

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Application Information

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IPC IPC(8): C07F7/08C07D213/18C07D233/58C08F112/34
Inventor 朱方华谢如刚杨军校顾忠伟
Owner SICHUAN UNIV
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