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Preparation method for thermoset high temperature resistant methyl phenyl silicone resin

A technology of methyl phenyl silicon and high temperature resistance, which is applied in the field of preparation of thermosetting and high temperature resistant methyl phenyl silicone resin, can solve the problems of affecting popularization and application, small production scale and high cost, so as to overcome potential safety hazards and avoid gelling. The effect of less chemical impurities and low cost

Inactive Publication Date: 2012-07-18
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with foreign countries, there is still a long way to go due to the fact that foreign countries have adopted technical secrecy measures against my country, and the second is that the production scale is small and scattered, and the cost is too high, which affects popularization and application.

Method used

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  • Preparation method for thermoset high temperature resistant methyl phenyl silicone resin
  • Preparation method for thermoset high temperature resistant methyl phenyl silicone resin
  • Preparation method for thermoset high temperature resistant methyl phenyl silicone resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The fixed Ph / R value is 0.1 and the R / Si value is 1.2. Add 47.84 g of methyltrichlorosilane, 4.128 g of dimethyldichlorosilane, 9.168 g of methylphenyldichlorosilane and 91.704 g of xylene into a 1000 mL four-neck flask, keep stirring fully under an ice-water bath, drop Add a mixture of water and acetone, wherein the mass of water is 161.28 g, and the mass of acetone is 80.64 g. Keep for 3~5 h to complete the dropwise addition, and stir well to continue the reaction for 2 h. After the reaction, the upper oil layer was washed with water until neutral to obtain a white turbid prepolymer. Concentrate the prepolymer under reduced pressure at 120 °C to a solid content of 50-70 %, add 0.2445 g of stannous octoate condensation catalyst (the amount is 0.4 % of the total mass of monomers) at 150 °C, heat-preserve polycondensation, and remove the solvent , to obtain a translucent hard solid. Its infrared spectroscopic analysis see figure 1 , for thermogravimetric analysis see...

Embodiment 2

[0042] Same as Example 1, the Ph / R value is fixed at 0.1, and the R / Si value is changed to 1.3. Add 41.86 g of methyltrichlorosilane, 8.772 g of dimethyldichlorosilane, 9.932 g of methylphenyldichlorosilane and 90.846 g of xylene into a 1000 mL four-neck flask, keep stirring fully under an ice-water bath, drop Add a mixture of water and acetone, wherein the mass of water is 155.52 g, and the mass of acetone is 77.76 g. Keep for 3~5 h to complete the dropwise addition, and stir well to continue the reaction for 2 h. After the reaction, the upper oil layer was washed with water until neutral to obtain a white turbid prepolymer. Concentrate the prepolymer under reduced pressure at 120 °C to a solid content of 50-70 %, add 0.2422 g of stannous octoate condensation catalyst (the amount is 0.4 % of the total mass of the monomer) at 150 °C, heat-preserve polycondensation, and remove the solvent , to obtain a translucent hard solid. Thermogravimetric analysis see image 3 .

Embodiment 3

[0044] Same as Example 1, the Ph / R value is fixed at 0.1, and the R / Si value is changed to 1.4. Add 35.88 g of methyltrichlorosilane, 13.416 g of dimethyldichlorosilane, 10.696 g of methylphenyldichlorosilane and 89.988 g of xylene into a 1000 mL four-neck flask, keep stirring fully under an ice-water bath, drop Add a mixture of water and acetone, wherein the mass of water is 149.76 g, and the mass of acetone is 74.88 g. Keep for 3~5 h to complete the dropwise addition, and stir well to continue the reaction for 2 h. After the reaction, the upper oil layer was washed with water until neutral to obtain a white turbid prepolymer. Concentrate the prepolymer under reduced pressure at 120 °C to a solid content of 50-70 %, add 0.24 g of stannous octoate condensation catalyst (the amount is 0.4 % of the total mass of monomers) at 150 °C, heat-preserve polycondensation, and remove the solvent , to obtain a translucent hard solid. Thermogravimetric analysis see Figure 4 .

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Abstract

The invention discloses a preparation method for thermoset high temperature resistant methyl phenyl silicone resin, which relates to the technical field of resin preparation and comprises the steps of utilizing toluene or dimethylbenzene or mixed solution of the toluene and dimethylbenzene to serve as a solvent, utilizing methyl trichlorosilane, dichlorodimethylsilane and methylphenyldichloros as monomer raw materials, dropping mixed solution of acetone and water into the raw materials under the condition of ice-water bath, ensuring that the dropping is finished within 3-5 hours, obtaining a prepolymer of the methyl phenyl silicone resin, performing condensation and curing on the obtained prepolymer above 150 DEG C after pressure of the prepolymer is reduced and the prepolyme is concentrated, the adopted condensation catalyst is caprylate or naphthenate, particularly is stannous octoate, zinc isoocatanoate, cobalt naphthenate and dibutyltin dilaurate. The resin is semi-transparent hard or elastic solid, can not be dissolved or fused, and can be resistant to high temperature above 200 DEG C, and can be used as silicon rubber or a plastic filler.

Description

technical field [0001] The invention relates to a method for preparing high-temperature-resistant methylphenyl silicone resin by using the "reverse hydrolysis method", which belongs to the technical field of resin preparation, and specifically refers to: using toluene or xylene or a mixed solution of the two as a solvent, methyltrichlorosilane, Dimethyldichlorosilane and methylphenyldichlorosilane are used as monomer raw materials, and a mixed solution of acetone and water is added dropwise therein under an ice-water bath, and the dropwise addition is completed within 3 to 5 hours, and the hydrolysis reaction obtains methylbenzene Based silicone resin prepolymer, the obtained prepolymer is condensed under reduced pressure and then condensed and solidified above 150 °C. The condensation catalyst used is octoate or naphthenate, specifically stannous octoate, zinc isooctanoate, cyclohexanoate Cobalt alkanoate and dibutyltin dilaurate. The resin is translucent hard or elastic sol...

Claims

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Application Information

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IPC IPC(8): C08G77/04C08G77/08
Inventor 殷恒波姜逸倩柳艳君颜晓波葛超群沈玉堂马克超
Owner JIANGSU UNIV
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