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Method of preparing methyl phenyl polysiloxane

A technology of methylphenylsilicon and methylphenyldichlorosilane is applied in the field of preparation of methylphenylsilicone resin, and can solve the problems of reduced heat resistance, easy sticking of paint films, and inability to completely overcome sticking back. , to achieve the effect of low curing temperature

Active Publication Date: 2011-04-20
安徽比特海新材料股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, there are general-purpose methylphenyl silicone resins of existing brands at home and abroad, such as 1153, 1053 and other methylphenyl silicone resins. Their curing temperature needs to be ≥ 200°C, and the cured paint film has weak adhesion to the substrate and cannot be cured. Disadvantages such as the paint film is easy to stick back
Some brands of silicone resins with low-temperature curing characteristics mainly rely on external crosslinking agents, catalysts and other components to strengthen the curing reaction. As a result, the heat resistance of the cured silicone resin is reduced, especially the high-temperature flexibility deterioration and storage Stability, but still can not completely overcome the phenomenon of sticking back after curing

Method used

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  • Method of preparing methyl phenyl polysiloxane

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preparation example Construction

[0017] The preparation process of the present invention is as follows:

[0018] a. Add various monomers and toluene in proportion to the mixing kettle, mix evenly, add toluene and water into the reaction kettle, stir and heat up to 30-65°C, start adding the mixed monomer solution dropwise, and control the temperature at 30-65°C The dropwise addition is completed within 1.5 to 3 hours at 70°C, and then keep the temperature for half an hour to react;

[0019] b. Static layering, lower layer of acidic water;

[0020] c. Wash with hot water at 40-70°C until neutral;

[0021] d. Concentrate it to 40% to 60% (mass percentage) under high vacuum conditions and at a temperature not exceeding 60°C;

[0022] e. Adding an appropriate amount of catalyst, polycondensation reaction at a vacuum of -0.07 to -0.08MPa and a temperature of 50 to 60°C for 1 to 6 hours, and adding a corresponding amount of stabilizer to obtain a methylphenyl silicone resin.

Embodiment 1

[0024] Add 149.5g of methyltrichlorosilane, 37.5g of dimethyldichlorosilane, 38.1g of phenyltrichlorosilane and 286g of toluene into the mixing tank and mix well. Add 184g of toluene and 950g of water into the reaction kettle, stir and heat up to 65°C, start adding the mixed monomers dropwise, control the reaction temperature at 65-70°C within 3 hours, and finish the reaction for half an hour. After resting, remove the lower acidic water layer, then wash the silanol toluene solution with 65-70°C hot water until neutral, and concentrate under reduced pressure to a solid content of 60%. Take 100g of this silanol solution, add 0.03g of 10% triethylenetetraminebutanol solution as a catalyst, and then add 0.003g of acetic acid stabilizer at a vacuum degree of -0.08MPa and control the temperature at 50°C for 6 hours to obtain a viscosity of 15s (Apply 4 cups), methyl phenyl silicone resin (R / Si=1.2, Ph / R=0.1) that cures at 40°C for 1 hour and does not retack.

Embodiment 2

[0026] Add 195g of diphenyldichlorosilane, 105.8g of phenyltrichlorosilane, 81.3g of dimethyldichlorosilane, 15g of methyltrichlorosilane and 354g of toluene into the mixing tank and mix well. Add 189g of toluene and 1240g of water into the reaction kettle, stir and heat up to 30°C, start to add the mixed monomers dropwise, control the reaction temperature at 30-35°C for 1.5 hours, then stir the reaction for half an hour. After static separation, the lower acidic water layer was removed, and the silanol toluene solution was washed with warm water at 40-45°C until neutral, and then concentrated under reduced pressure to a solid content of 40%. Take 100 g of this silanol solution, add 0.12 g of 10% tetraethylammonium hydroxide butanol solution as a catalyst, and react at a vacuum degree of -0.07 MPa at 60° C. for 1 hour, then add 0.0012 g of acetic anhydride stabilizer, A methylphenyl silicone resin (R / Si=1.7, Ph / R=0.6) with a viscosity of 25 s (coating 4 cups), cured at 100° C....

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Abstract

The invention discloses a method for synthesizing organic silicon, in particular provides a method for preparing methyl phenyl silicone resin which has low curing temperature by self and is not sticky repeatedly. The invention uses the monomers of methyl trichlorosilane, dimethyldichlorosilance, phenyl trichlorosilane, dichloromethylphenylsilane, diphenyl dichlorosilane and the like to obtain a methyl phenyl silicone resin with low curing temperature and a paint film which is not sticky repeatedly after being cured by the processes of adjusting the proportion of raw materials, controlling proper reaction temperature and polymerization time, carrying out hydrolysis reaction and polycondensation reaction, etc. The invention has the advantages that the methyl phenyl silicone resin prepared by the method has the characteristics of low curing temperature, being not sticky repeatedly, being clear and transparent, high and low temperature resistance, weather resistance, being insulating and the like; the methyl phenyl silicone resin is in particular fit for dip varnish higher than grade H; and the methyl phenyl silicone resin is used for confecting insulated paint, weather-resistant paint and heat resistant paint higher than grade H, is used for heat resistant parting agent and also can be used in the fields with rigorous using requirements, such as heat resistant water blocking and sand prevention for oil drilling, etc.

Description

technical field [0001] The invention relates to a method for synthesizing organosilicon, in particular to a method for preparing methylphenyl silicone resin which itself has a low curing temperature and does not stick back. Background technique [0002] At present, there are general-purpose methylphenyl silicone resins of existing brands at home and abroad, such as 1153, 1053 and other methylphenyl silicone resins. Their curing temperature needs to be ≥ 200°C, and the cured paint film has weak adhesion to the substrate and cannot be cured. The paint film is easy to stick back and other shortcomings. Some brands of silicone resins with low-temperature curing characteristics mainly rely on external crosslinking agents, catalysts and other components to strengthen the curing reaction. As a result, the heat resistance of the cured silicone resin is reduced, especially the high-temperature flexibility deterioration and storage Stability, but still can not completely overcome the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/04C08G77/06C08G77/08
Inventor 吴连斌陈利民陈遒罗蒙贤来国桥蒋剑雄邱化玉
Owner 安徽比特海新材料股份有限公司
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