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Method for preparing methyl phenyl trifluoro propyl silicone resin

A technology of trifluoropropyl silicon and methyl phenyl, applied in the direction of chemical instruments and methods, applications, organic fertilizers, etc., can solve the problems of unfavorable long-term use and poor aging resistance, and achieve improved UV resistance and good weather resistance , The process is easy to control the effect

Inactive Publication Date: 2013-04-24
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the resin treatment, the strength and waterproof performance of the soil ruins have been improved to a certain extent, but the aging resistance is poor, which is not conducive to long-term use

Method used

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  • Method for preparing methyl phenyl trifluoro propyl silicone resin
  • Method for preparing methyl phenyl trifluoro propyl silicone resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 100g methylphenyldiethoxysilane, 800g phenyltriethoxysilane, 200g trifluoropropyltriethoxysilane, 100g dimethyltrifluoropropylethoxysilane to a 5000mL reactor Base silane and 120 grams of ferric chloride solution (mass concentration 1%) were stirred, the temperature was controlled at 70°C, and 800 grams of water was added. Hydrolyze and polymerize for 4-6 hours, wash with deionized water until neutral, raise the temperature to 180°C, control the vacuum degree above 0.095MPa to remove low molecular weight, and obtain clear and transparent methylphenyl trifluoropropyl silicone resin, the conversion rate per pass is 88.51%, its refractive index (n 25 D ) was 1.5364, the R / Si (molar ratio) was 1.29, the trifluoropropyl content was 19.36 mol%, and the phenyl content was 58.11 mol%.

Embodiment 2

[0016] Add 600g methylphenyldimethoxysilane, 600g dimethyldimethoxysilane, 1000g phenyltrimethoxysilane, 200g dimethyltrifluoropropylethoxysilane to a 5000mL reactor Stir with 80 grams of ferric chloride solution, the temperature is controlled at 70 ° C, and 700 grams of water are added. Hydrolyze and polymerize for 4-6 hours, wash with deionized water until neutral, raise the temperature to 180°C, control the vacuum degree above 0.095MPa to remove low molecular weight, and obtain clear and transparent methylphenyl trifluoropropyl silicone resin, the conversion rate per pass is 90.12%, its refractive index (n 25 D ) is 1.5286, the R / Si (molar ratio) is 1.71, the trifluoropropyl content is 4.42 mol%, and the phenyl content is 33.88 mol%.

Embodiment 3

[0018] Add 700g methylphenyldiethoxysilane, 1200g phenyltriethoxysilane, 200g trifluoropropyltrimethoxysilane, 300g dimethyltrifluoropropylmethoxysilane to a 5000mL reactor Silane and 60 grams of ferric chloride solution were stirred, the temperature was controlled at 70°C, and 800 grams of water was added. Hydrolyze and polymerize for 4-6 hours, wash with deionized water until neutral, raise the temperature to 180°C, control the vacuum degree above 0.095MPa to remove low molecular weight, and obtain clear and transparent methylphenyl trifluoropropyl silicone resin, the conversion rate per pass is 86%, its refractive index (n 25 D ) was 1.5315, the R / Si (molar ratio) was 1.60, the trifluoropropyl content was 14.52 mol%, and the phenyl content was 47.83 mol%.

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Abstract

The invention relates to a method for preparing methyl phenyl trifluoro propyl silicone resin. The present invention overcomes the defects existed in the prior art and provides a novel silicone resin preparation method with the characteristics of consolidation, water resistance, ultraviolet resistance and the like. The method comprises the following step: taking feeding amount of two functional groups siloxane, three functional groups siloxane, one or more simple functional group siloxane, regulating the mol ratio of organic group to silicon atom at 1.2-1.6:1 and the mol ratio of phenyl to organic group at 0.2-0.5:1; adding in a reaction kettle, controlling the temperature of 40-100 DEG C, under the effect of a catalyst ferric chloride, stirring by adding water, carrying out a hydrolysis-condensation reaction, wherein the polymerization time is 2-8 hours, washing by deionized water to neutrality, reducing the pressure and removing a low boiling substrate to obtain the transparent phenyl trifluoro propyl silicone resin; wherein the usage amount of ferric trichloride is 1-5% of silicone feed amount.

Description

technical field [0001] The invention relates to a reinforcing material for earthen ruins, in particular to a preparation method of methylphenyl trifluoropropyl silicone resin. The material is used together with a curing agent for the protection of earthen sites in arid areas. Background technique [0002] Due to the erosion and damage of weathering, rain erosion and other natural factors, a large number of ancient earth building sites collapsed and suffered devastating damage. Many countries in the world have carried out the protection of ancient earthen building sites. At present, chemical materials are mainly used for weatherproofing and rainproof reinforcement of earthen buildings. Chemical materials commonly used include inorganic materials, organic polymer materials, and organic-inorganic composite materials. Wait. Inorganic materials are mainly some silicates, such as high-modulus potassium silicate solutions prepared by Li Zuixiong and Wang Xudong of the Dunhuang Re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/24C09K17/38
Inventor 张飞豹倪勇来国桥许文东
Owner HANGZHOU NORMAL UNIVERSITY