Benzocyclobutene silicone oil resin and preparation method thereof

A technology of benzocyclobutene silicon-based ethylene and hydrogen silicone oil, which is applied in chemical instruments and methods, other chemical processes, etc., can solve problems such as difficult mass production, limited application of materials, and cumbersome preparation of silicone resins.

Inactive Publication Date: 2012-06-27
BEICHUAN RUIHUI SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese invention patent (ZL200710111698.4, 2009.7) synthesized a class of benzocyclobutene silicone resin, showing excellent thermal and mechani

Method used

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  • Benzocyclobutene silicone oil resin and preparation method thereof
  • Benzocyclobutene silicone oil resin and preparation method thereof
  • Benzocyclobutene silicone oil resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0054] Example 1:

[0055] The preparation method of dimethyl-4-benzocyclobutene silylethylene graft modified hydrogen-containing silicone oil includes the following steps:

[0056] a. Ingredients: take raw material hydrogen-containing silicone oil, graft monomer II, platinum-containing catalyst;

[0057] The hydrogen-containing silicone oil is a hydrogen-containing silicone oil with a mass percentage of hydrogen content of 1.3%, and the grafting monomer II is 4-(1,1-dimethyl-1-vinyl)silicon benzocyclobutene ( Namely: 4-DMVSBCB), the platinum-containing catalyst is a Pt / C catalyst;

[0058] According to the number of moles of Si-H bonds in the hydrogen-containing silicone oil: graft monomer II: platinum (Pt) (ie the number of moles of platinum in the Pt / C catalyst) is 1:2: 1.56×10 -2 The molar ratio of each raw material component;

[0059] b. Mixing reaction: In a dry test tube equipped with a magnetic stirrer, blow nitrogen for 5 minutes to remove oxygen in the system, and then add 1....

Example Embodiment

[0062] Example 2:

[0063] The preparation method of dimethyl-4-benzocyclobutene silylethylene graft modified hydrogen-containing silicone oil includes the following steps:

[0064] a. Ingredients: take raw material hydrogen-containing silicone oil, graft monomer II, platinum-containing catalyst;

[0065] The hydrogen-containing silicone oil is a hydrogen-containing silicone oil with a mass percentage of hydrogen content of 1.3%, and the grafting monomer II is 4-(1,1-dimethyl-1-vinyl)silicon benzocyclobutene ( Namely: 4-DMVSBCB), the platinum-containing catalyst is chloroplatinic acid;

[0066] According to the number of moles of Si-H bonds in the hydrogen-containing silicone oil: graft monomer II: platinum (Pt) (ie the number of moles of platinum in the platinum-containing catalyst chloroplatinic acid) is 1:2: 1.56×10 -2 The molar ratio of each raw material component;

[0067] Preparation of chloroplatinic acid: 1g H 2 PtCl 6 ·6H 2 O was dissolved in 100 ml of anhydrous toluene and s...

Example Embodiment

[0071] Example 3:

[0072] The preparation method of dimethyl-1-benzocyclobutene silyl ethylene graft modified hydrogen-containing silicone oil includes the following steps:

[0073] a. Ingredients: take raw material hydrogen-containing silicone oil, graft monomer III, platinum-containing catalyst;

[0074] The hydrogen-containing silicone oil is a hydrogen-containing silicone oil with a mass percentage of hydrogen content of 1.3%, and the grafting monomer III is 1-(1,1-dimethyl-1-vinyl)silicon benzocyclobutene ( Namely: 1-DMVSBCB), the platinum-containing catalyst is a Pt / C catalyst;

[0075] According to the number of moles of Si-H bonds in hydrogen-containing silicone oil: graft monomer III: platinum (Pt) (ie the number of moles of platinum in the platinum-containing catalyst Pt / C) is 1:5: 1.56×10 -2 The molar ratio of each raw material component;

[0076] b. Mixing reaction: In a dry test tube equipped with a magnetic stirrer, blow nitrogen for 5 minutes to remove oxygen in the sys...

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Abstract

The invention discloses dimethyl-4-benzocyclobutene silicon-based vinyl-grafted modified hydrogen-containing silicone oil shown as a formula (IV) and a preparation method thereof. The preparation method of benzocyclobutene silicone oil resin comprises the following steps of: putting solvent-toluene-diluted hydrogen-containing silicone oil and 4-(1,1-dimethyl-1-vinyl) silicon benzocyclobutene intoa reactor, adding a platinum catalyst after being protected by N2, and stirring and carrying out reaction for 20-40 hours at the reaction temperature of 60-90 DEG C; and adding triphenylphosphine, heating to reflux for 3 hours, cooling, filtering, adding methanol and mixing after a filtrate is concentrated, carrying out precipitation, filtering, carrying out repeated precipitation on solids for 1-2 times by using methanol, and then, drying to obtain a product. The product, i.e. benzocyclobutene silicone oil resin, has excellent thermal properties, mechanical properties, electrical properties and film forming properties and has wide development and application prospects in fields, such as microelectronics industry, aerospace and national defense and the like.

Description

technical field [0001] The invention belongs to a silicone resin and a preparation method thereof, and relates to a benzocyclobutene silicone oil resin and a preparation method thereof. The prepared benzocyclobutene silicone oil resin has excellent properties and is suitable for use as a high-performance dielectric film material or packaging material in the fields of microelectronics industry, aerospace and national defense. Background technique [0002] Benzocyclobutene (BCB) materials have been widely used abroad due to their excellent high and low temperature resistance, weather resistance, good air tightness, radiation resistance, especially excellent film-forming properties and moisture resistance. It has been used in military and civilian fields; common silicone polymers have excellent properties such as high and low temperature resistance, weather resistance, electrical insulation, radiation resistance, flame retardancy, good air tightness, and corrosion resistance, a...

Claims

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Application Information

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IPC IPC(8): C08G77/38C09K3/10
Inventor 杨军校李慧玲黄亚文曹克
Owner BEICHUAN RUIHUI SCI & TECH CO LTD
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