Chemical crosslinking-curable phenyl MDQ-type silicone resin and preparation method thereof

A chemical cross-linking, silicone resin technology, applied in the field of organic polymer chemistry, can solve the problems of low refractive index of MDQ silicone resin, optical properties and mechanical properties, etc., and achieve the effects of good mechanical properties, increased refractive index, and narrowed differences.

Active Publication Date: 2013-01-30
XINYAQIANG SILICON CHEM JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to solve the problem that the MDQ silicone resin has a low refractive index and cannot be cured by chemical cross-linking while improving the optical and mechanical properties of the rubber-type packaging material reinforced by the silicone resin, the present invention propose

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In a 250 ml three-necked flask equipped with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, add 12.4 g (0.333 mol) of deionized water and 5.4 g (0.117 mol) of absolute ethanol and stir evenly, then Add 0.65 g hexamethyldisiloxane (0.004 mol), 3.6 g (0.0194 mol) 1,3-divinyltetramethyldisiloxane and 24.0 g (0.1143 mol) methylphenyldiethoxy A mixed solution composed of silane, then 1.2mL of 36% concentrated hydrochloric acid (0.0388 mol) was added dropwise, when the temperature was raised to 40°C, 24.0g (0.1154 mol) ethyl orthosilicate was added dropwise within 10min and then at 80 ℃ to maintain the reaction for 3h. When the temperature is lowered to 50°C, add 25ml of toluene for extraction, then cool to room temperature, wash with water until neutral, add anhydrous calcium chloride to dry until clear and transparent, filter to remove salt, and remove the toluene solvent by rotary evaporation to obtain chemically cross-linkable and solidified ...

Embodiment 2

[0036] In a 250 ml three-necked flask equipped with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, add 12.2 g (0.678 mol) of deionized water and 5.3 g (0.1152 mol) of absolute ethanol and stir evenly, and then Add 3.1 g (0.0191 mol) of hexamethyldisiloxane, 3.2 g (0.0172 mol) of 1,3-divinyltetramethyldisiloxane and 4.7 g (0.0224 mol) of methylphenyldiethoxy A mixed solution composed of silane, then dropwise added 3.4 Concentrated hydrochloric acid (0.1098 mol) with a concentration of 36% in mL, when the temperature was raised to 60°C, 21.0g (0.1010 mol) ethyl orthosilicate was added dropwise within 20min and then maintained at 90°C for 1h. When the temperature is lowered to 70°C, add 25ml of toluene for extraction, then cool to room temperature, wash with water until neutral, add anhydrous calcium chloride to dry until clear and transparent, filter to remove salt, and remove the toluene solvent by rotary evaporation to obtain chemically cross-link...

Embodiment 3

[0038] In a 250 ml three-neck flask equipped with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, add 12.1 g (0.672 mol) of deionized water and 5.3 g (0.1152 mol) of absolute ethanol and stir evenly, and then Add 1.2 g (0.0074 mol) hexamethyldisiloxane, 3.3 g (0.0177 mol) 1,3-divinyltetramethyldisiloxane and 8.5 g (0.0405 mol) methylphenyldiethoxy A mixed solution composed of silane, then 1.5mL of 36% concentrated hydrochloric acid (0.0484 mol) was added dropwise, when the temperature was raised to 50°C, 20.9g (0.1005 mol) ethyl orthosilicate was added dropwise within 30min and then at 60 The reaction was maintained at ℃ for 4h. When the temperature is lowered to 50°C, add 25ml of toluene for extraction, then cool to room temperature, wash with water until neutral, add anhydrous calcium chloride to dry until clear and transparent, filter to remove salt, and remove the toluene solvent by rotary evaporation to obtain chemically cross-linkable and sol...

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Abstract

The invention relates to the field of organic polymer chemistry and provides a chemical crosslinking-curable phenyl MDQ-type silicone resin and a preparation method thereof. The chemical crosslinking-curable phenyl MDQ-type silicone resin solves the problem that the existing MDQ-type silicone resin has a low refractive index and is not cured by a chemical crosslinking method, and improves optical and mechanical properties of a silicone resin-reinforced rubber-type packaging material. Hexamethyldisiloxane and 1,3-divinyltetramethyldisiloxane as blocking agents, methylphenyldiethoxysilane as a D chain unit source and tetraethoxysilane as a Q chain unit source undergo a co-hydrolytic condensation reaction in the presence of an ethanol aqueous solution as a reaction solvent, toluene as an extractant and hydrochloric acid as a catalyst to produce the chemical crosslinking-curable phenyl MDQ-type silicone resin. The chemical crosslinking-curable phenyl MDQ-type silicone resin improves mechanical properties of a MDQ-type silicone resin-reinforced rubber-type packaging material and improves optical properties of the rubber-type packaging material. The preparation method has mild reaction conditions, has simple processes and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of organic polymer chemistry, in particular to a chemically crosslinkable and curable phenyl MDQ type silicone resin and a synthesis method thereof. Background technique [0002] In addition to the advantages of ordinary silicone materials, silicone polymers cured by addition of hydrosilylation have the characteristics of no by-products during the vulcanization molding process, small shrinkage and deep vulcanization, etc., and are of great use in electronic and electrical packaging. . However, the cohesive energy density of silicone polymers is small, and the mechanical properties of silicone polymers without filler reinforcement are poor, and their performance indicators such as tensile strength, elongation at break, tear strength and hardness cannot meet the needs of packaging materials. Fumed or precipitated silica is the most common and the largest amount of reinforcing filler for silicone matrix materials, but i...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06C08L83/07
Inventor 伍川张宝华董红蒋剑雄程大海
Owner XINYAQIANG SILICON CHEM JIANGSU
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