Method for preparing methyl phenyl vinyl silicone resin

A technology of methylphenylethylene and methylphenyldimethoxysilane, which is applied in the field of organic polymer materials, can solve the problems of unstable quality, poor storage, cumbersome synthesis process, etc., and achieve easy control of reaction and storage performance Better, easy separation and purification effect

Inactive Publication Date: 2010-06-02
SUZHOU UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0009] There are following deficiencies in the above preparation method: 1) adopt toxic toluene as solvent, it is difficult to recycle, pollute the environment, endanger human health; 2) the reaction monomer is organochlorosilane, the monomer source is limited, and a large amount of hydrogen chloride is generated in the reaction process Gas, together with the heat released by dissolving in water, promotes the spontaneous condensation reaction between silicon hydroxyl groups, resulting in difficult control of the degree of polymerization, the reaction system is prone to gel, and the hydrochloric acid generated by the reaction will cause corrosion to equipment; 3) The synthesis process is cumbersome , the types of reaction products are complex, need to be washed many times, and there

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  • Method for preparing methyl phenyl vinyl silicone resin
  • Method for preparing methyl phenyl vinyl silicone resin
  • Method for preparing methyl phenyl vinyl silicone resin

Examples

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Effect test

Embodiment 1

[0029] By weight, in a nitrogen atmosphere at a temperature of 35°C, dissolve 100 parts of methyltrimethoxysilane, 190 parts of vinyltrimethoxysilane, and 360 parts of diphenyldimethoxysilane in 460 parts of ethanol In, solution A is formed;

[0030] Add 105 parts of deionized water and a certain amount of concentrated hydrochloric acid dropwise to solution A to adjust the pH value of the system to 3.3, and react for 2 hours after the dropwise addition to form solution B;

[0031] Add 40 parts of methyltrimethoxysilane, 80 parts of vinyltrimethoxysilane, 150 parts of methylvinyldimethoxysilane, and 80 parts of deionized water into solution B, and react at a constant temperature of 50°C for 1 hours, then warming up to 78°C, and reacting at constant temperature for 8 hours to form solution C;

[0032] By weight, 350 parts of hexamethyldisiloxane and 40 parts of deionized water were added dropwise to solution C, and reacted at a constant temperature of 78°C for 6 hours to obtain...

Embodiment 2

[0035] By weight, under a nitrogen atmosphere at a temperature of 45°C, 130 parts of methyltrimethoxysilane, 285 parts of vinyltrimethoxysilane, 300 parts of diphenyldimethoxysilane and 90 parts of methyl Phenyldimethoxysilane was dissolved in 650 parts of ethanol to form solution A;

[0036] Add 105 parts of deionized water and a certain amount of concentrated hydrochloric acid dropwise to solution A to adjust the pH value of the system to 3.0, and react for 1 hour after the dropwise addition to form solution B;

[0037]Add 55 parts of methyltrimethoxysilane, 90 parts of vinyltrimethoxysilane, 170 parts of diphenyldimethoxysilane, and 120 parts of deionized water into solution B, and react at a constant temperature of 50°C for 1 hour , and then heated up to 74°C, and reacted at constant temperature for 10 hours to form solution C;

[0038] By weight, 480 parts of triphenylsilane and 55 parts of deionized water were added dropwise to solution C, and reacted at a constant temp...

Embodiment 3

[0041] By weight, in a nitrogen atmosphere at a temperature of 40°C, 140 parts of methyltrimethoxysilane, 260 parts of vinyltrimethoxysilane, 420 parts of diphenyldimethoxysilane and 100 parts of methyl Vinyldimethoxysilane was dissolved in 600 parts of ethanol to form solution A;

[0042] Add 150 parts of deionized water and a certain amount of nitric acid dropwise to solution A to adjust the pH value of the system to 3.3, and react for 1.5 hours after the dropwise addition to form solution B;

[0043] Add 55 parts of methyltrimethoxysilane, 110 parts of vinyltrimethoxysilane, 115 parts of diphenyldimethoxysilane, 90 parts of methylphenyldisiloxane and 105 parts of deionized water to the solution In B, react at a constant temperature at 60°C for 0.5 hours, then raise the temperature to 75°C, and react at a constant temperature for 8 hours to form solution C;

[0044] By weight, 250 parts of hexamethyldisiloxane, 220 parts of trivinylchlorosilane and 65 parts of deionized wat...

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Abstract

The invention discloses a method for preparing a methyl phenyl vinyl silicone resin, which comprises the following steps of: under a condition of a nitrogen atmosphere at the temperature of between 30 and 45 DEG C, dissolving a certain amount of methyl trimethoxy silane, vinyl trimethoxy silane and alkyl dimethoxy silane in ethanol; adjusting the pH of the system to between 2.8 and 3.5; after full reaction, adding the methyl trimethoxy silane, the vinyl trimethoxy silane, the alkyl dimethoxy silane and deionized water into the mixture to perform isothermal reaction for 0.5 to 1 hour at the temperature of between 50 and 60 DEG C; raising the temperature to between 72 and 78 DEG C, performing the isothermal reaction again for 8 to 10 hours, and then dropping an end capping agent and deionized water into the mixture; performing reaction at the temperature of between 72 and 78 DEG C for 6 to 10 hours to obtain a white emulsion; and standing the mixture until complete demixing, separating the mixture to obtain an oily matter at a lower layer, and performing vacuum drying on the oily matter to obtain a product of the methyl phenyl vinyl silicone resin. In the method, the process is simple, the product is easy to separate and purify, the reactions are mild and are easy to control, and the processability is greatly improved.

Description

technical field [0001] The invention relates to a method for synthesizing an organosilicon polymer, in particular to a method for preparing an organosilicon resin, and belongs to the technical field of organic polymer materials. Background technique [0002] Silicone resin has the characteristics of both organic resin and inorganic materials, such as excellent heat resistance, weather resistance, electrical insulation, water repellency and chemical resistance, etc. It is a promising electrical insulation material. The number of organic groups contained in the silicone resin, that is, the R / Si value (the average number of organic groups connected to a silicon atom) and the phenyl (Ph) content (the percentage of the number of organic groups occupied by the phenyl group) are the factors that control the silicone resin. important indicator of quality. R / Si value mainly affects the dryness of silicone resin, paint film hardness, softness, thermal weight loss and heat cracking re...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06
Inventor 顾嫒娟张北京梁国正卓东贤袁莉
Owner SUZHOU UNIV
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