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Method for preparing alcohol-solubility methyl silicone resin

A methyl silicone resin, alcohol-soluble technology, applied in the field of preparation of methyl silicone resin, can solve the problems of low degree of hydrolysis, low activity of activated clay, toxicity and the like, and achieves simple and easy synthesis process, low commercial price, The effect of low R/Si

Inactive Publication Date: 2016-05-18
衢州市璀璨化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activated clay used in this preparation method has low activity and low degree of hydrolysis, and it is difficult to obtain a methyl silicone resin with good adhesion, and it is easy to gel in the polycondensation process, which is not suitable for industrial production. In the toluene mixture used, toluene Has certain toxicity, not green enough

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 1000ml four-necked flask, add 272 grams of methyltrimethoxysilane, 12 grams of dimethyldimethoxysilane, 142 grams of methyl alcohol, 142 grams of n-butanol, 8.52 grams of Tween 80 and 0.142 grams of hydrochloric acid, and heat up To 50°C, add 119.2 grams of deionized water dropwise, the molar ratio of the amount of deionized water to the sum of methyltrimethoxysilane and dimethyldimethoxysilane alkoxy groups is 1.1:1, add dropwise The time is controlled at 3 hours, and the reaction is continued for 4 hours after the addition is completed. Use sodium bicarbonate to neutralize the hydrochloric acid until the solution is neutral, heat up to remove methanol, n-butanol and water in the solution, raise the temperature to 140°C and maintain the temperature for half an hour , After cooling, add methanol to prepare an alcohol solution with 50% solid content, and filter to obtain a methanol solution of methyl silicone resin with R / Si=1.05.

Embodiment 2

[0025] Add 356 grams of methyltriethoxysilane, 74 grams of dimethyldiethoxysilane, 215 grams of ethanol, 2.15 grams of Span 80 and 0.43 grams of acetic acid into a 1000ml four-necked flask, heat up to 70 ° C, drop 226.8 grams of deionized water, the molar ratio of the amount of deionized water to the sum of methyltriethoxysilane and dimethyldiethoxysilane alkoxy groups is 1.8:1, and the dropping time is controlled at 0.5 hours , continue to react for 3 hours after the dropwise addition, use sodium carbonate to neutralize acetic acid until the solution is neutral, heat up to remove ethanol and water in the solution, raise the temperature to 140°C and maintain the temperature for half an hour, add ethanol after cooling to prepare 50% Alcoholic solution with solid content, and filter to get methyl silicone resin ethanol solution with R / Si=1.2.

Embodiment 3

[0027] Add 272 grams of methyltrimethoxysilane, 29.6 grams of dimethyldiethoxysilane, 100 grams of methanol, 126.2 grams of isopropanol, 1.5 grams of Tween 20, and 1.5 grams of polyether modified Silicone oil and 0.23 gram of formic acid, heat up to 65 ℃, drop 172 grams of deionized water, the amount of deionized water is equal to the mole of the sum of methyltrimethoxysilane and dimethyldiethoxysilane alkoxy groups The ratio is 1.5:1, the dropping time is controlled at 3.5 hours, and the reaction is continued for 3.5 hours after the dropping is completed. Use potassium bicarbonate to neutralize the hydrochloric acid until the solution is neutral, and heat up to remove methanol, isopropanol and water in the solution. Raise the temperature to 140°C and maintain the temperature for half an hour. After cooling, add isopropanol to prepare an alcohol solution with 50% solid content, and filter to obtain a methyl silicone resin isopropanol solution with R / Si=1.09.

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PUM

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Abstract

The invention discloses a method for preparing alcohol-solubility methyl silicone resin. The method is simple, stable and environmentally friendly in technology. The method includes the steps that methyltrialkoxysilane, dimethyldialkoxysilane, an alcohol solvent and a molecule control assistant are mixed, an acid catalyst is added, deionized water is dropwise added at the temperature of 50-70 DEG C, the dropwise-adding time is controlled to range 0.5 hour to 3 hours, the reaction continues to be conducted for 3-4 hours after the dropwise-adding process is finished, carbonate is added to neutralize the acid catalyst till the solution is neutral, the solution is heated to remove the alcohol solvent and the water in the solution and heated to 140 DEG C, the temperature is maintained for 0.5 hour, the solution is cooled, an alcohol solvent is added, an alcohol solution in a certain proportion is prepared, and the alcohol-solubility methyl silicone resin is obtained through filtering. According to the preparing method, the cost of the adopted raw materials is low; in the production process, gel is not prone to occurrence, wastewater is avoided, and the produced methyl silicone resin has good solubility in the alcohol solvent.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a method for preparing alcohol-soluble methyl silicone resin. Background technique [0002] Silicone resin is a thermosetting polysiloxane system with a highly cross-linked structure. Its structure contains both organic groups and inorganic structures. This special composition and molecular structure make it have both organic properties and inorganic functions. It has good thermal stability, oxidation stability, excellent hydrophobicity, etc., and is used as an adhesive for high temperature resistant mica boards. [0003] The number of organic groups in the silicone resin will have a great impact on the performance of the silicone resin. With the increase of R / Si, the heat resistance and hardness of the silicone resin will decrease, and the bending and flexibility will increase. Therefore, in mica Products with low R / Si are required in board adhesive applications. At p...

Claims

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Application Information

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IPC IPC(8): C08G77/06C08G77/08
CPCC08G77/06C08G77/08
Inventor 毛国强李晓晨
Owner 衢州市璀璨化工有限公司