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Preparation method for high-temperature-resistant silicon resin

A technology of high temperature resistance and resin, which is applied in the field of preparation of high temperature resistant silicone resin, can solve the problems of poor temperature resistance, complex reaction, and many raw materials, and achieve the effect of less environmental pollution

Active Publication Date: 2012-06-13
江苏明珠硅橡胶材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction does not produce hydrogen chloride, the reaction is stable, and the production efficiency is high. However, this method produces a large number of raw materials, complex reactions, and poor temperature resistance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 640g potassium acetate and 1700ml toluene were added to a four-neck flask, and the temperature was raised to reflux to remove water. Mix 424g of phenyltrichlorosilane and methyltrichlorosilane at a molar ratio of 3:1, and slowly add them dropwise into a four-neck flask. Control the reaction temperature at about 40°C. After the addition is complete, continue to stir for 2hr and add 209g methanol. In a four-necked flask, control the reaction temperature at 50°C. After the addition is complete, continue stirring for 1hr, heat up to 70°C and reflux for 2hr, recover the fraction below 78°C, distill out 484ml, add tap water to wash to pH=7, heat up and low pressure Distill toluene. 210 g of solid methyl phenyl silicone resin was obtained, the solid content was 99.5%, and the gel time was 28 minutes and 30 seconds.

Embodiment 2

[0021] 588g of sodium acetate and 1700ml of toluene were added to a four-necked flask, and the temperature was raised to reflux to remove water. Mix 426g of phenyltrichlorosilane, methyltrichlorosilane, and dimethyldichlorosilane with a molar ratio of 3:1:1, and slowly add them dropwise into a four-neck flask. Control the reaction temperature at about 42°C. Add dropwise After the completion, continue to stir for 2hr, add 215g of methanol to the four-necked flask, control the reaction temperature at 60℃, after the addition is complete, continue to stir for 1hr, heat up to 68℃, reflux for 2hr, recover the fraction below 80℃, distill out 496ml, add Wash with tap water to pH=7, and distill toluene at elevated temperature and low pressure. 200 g of solid methyl phenyl silicone resin was obtained, the solid content was 99.8%, and the gel time was 18 minutes and 47 seconds.

Embodiment 3

[0023] 671g of acetic anhydride and 1700ml of toluene were added to a four-necked flask and heated to reflux to remove water. Mix 575g of diphenyldichlorosilane and methyltrichlorosilane at a molar ratio of 3:2, and slowly add them dropwise into a four-neck flask. Control the reaction temperature at about 45°C. After the addition is complete, continue to stir for 2hr and add 215g Put methanol into a four-necked flask, control the reaction temperature at 60°C, after the addition, continue to stir for 1hr, heat up to 71°C and reflux for 2hr, recover the fraction below 80°C, distill 476ml, add tap water to wash to pH=7, warm up Toluene is distilled at low pressure. 215 g of solid methyl phenyl silicone resin was obtained, the solid content was 99.2%, and the gel time was 30 minutes and 15 seconds.

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PUM

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Abstract

The invention relates to a preparation method for high-temperature-resistant silicon resin, in particular to a preparation method for high-temperature methylphenyl silicon resin. The method is characterized by comprising the following steps of: dissolving an acetic acid derivative into methylbenzene; reflowing for removing water; mixing chlorosilane serving a raw material, and dropwise adding slowly; stirring; adding methanol; continually stirring and reflowing; recovering fractions which are in the temperature range of 67-80 DEG C; cooling, adding water and washing till the pH is equal to 6-7; removing a solvent under a negative pressure in vacuum; and cooling to obtain a solid finished product. The silicon solid methylphenyl silicon resin prepared by using the method has the characteristics of transparence, high-low temperature resistance, weather resistance, insulation and the like, and is environmentally-friendly.

Description

Technical field [0001] The invention relates to a method for preparing a high temperature resistant silicone resin, in particular to a method for preparing a high temperature resistant methyl phenyl silicone resin. Background technique [0002] Silicone resin is a polymer with a highly cross-linked network structure. The structure contains both organic groups and inorganic structures. This special composition and molecular structure is a combination of organic and inorganic properties and has unique physical properties. Chemical properties make it widely used as a base material for heat-resistant coatings, weather-resistant coatings and electrical insulating materials. Due to the introduction of phenyl silicon-oxygen bonds, methyl phenyl silicone resin has the weather resistance and electrical insulation properties of ordinary silicone resin. In addition to waterproof, breathable and physiological inertness, it also has super high and low temperature resistance, high refractive ...

Claims

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Application Information

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IPC IPC(8): C08G77/06C09D183/04C09D5/25
Inventor 朱德洪刘金明钱芬芬朱恩伟
Owner 江苏明珠硅橡胶材料有限公司