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Modified hydrogen-containing cyclotetrasiloxane bonding accelerant as well as preparation method and application thereof

A technology of adhesion promoter and cyclotetrasiloxane, applied in adhesives, non-polymer adhesive additives, adhesive additives, etc., can solve the problems of decreased mechanical properties of silicone rubber, complex synthesis process, harsh vulcanization conditions, etc. , to achieve the effect of improving the bonding performance, the raw materials are cheap and easy to obtain, and the preparation process is simple.

Inactive Publication Date: 2013-10-23
广州纽楷美新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patent CN102408869A discloses a hydrolysis reaction of vinyl trimethyl (ethyl) oxysilane and γ-(2,3-glycidyloxy) propyl trimethyl (ethyl) oxysilane or the hydrolysis reaction product of the two and The adhesion promoter prepared by the reaction of γ‐aminopropyltrimethyl(ethyl)oxysilane, the study found that adding this adhesion promoter to the addition-type liquid silicone rubber can achieve adhesion to aluminum, but the presence of siloxane The hydrolysis reaction conditions are not easy to control, the reaction process is prone to gel, and the nitrogen-containing compounds are easy to poison the platinum catalyst.
But at the same time, due to the introduction of phenyl in the adhesion promoter molecule, the compatibility between the adhesion promoter and silicone rubber will be poor.
[0006] At present, although there have been some reports on adhesion promoters for improving the adhesion of addition-type liquid silicone rubber, most of these adhesion promoters have complex synthesis processes, harsh vulcanization conditions, poisoning of catalysts, and degradation of mechanical properties of silicone rubber. question
These problems have always limited the application of adhesion promoters for addition-type liquid silicone rubber in industrial production.

Method used

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  • Modified hydrogen-containing cyclotetrasiloxane bonding accelerant as well as preparation method and application thereof
  • Modified hydrogen-containing cyclotetrasiloxane bonding accelerant as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Synthesis of adhesion promoter

[0025] 22.6g of 1,6-hexanediol diacrylate and 0.02g of silica-supported chloroplatinic acid catalyst with a platinum concentration of 0.5% were mixed in a flask and heated at 60°C for 30min. The claims define that the platinum catalyst is chloroplatinic acid or platinum-vinylsiloxane complex dissolved in isopropanol or tetrahydrofuran solvent, loaded on silicon dioxide or activated carbon. Here is only the isopropanol solution of chloroplatinic acid. Does it still need to be supported on silica or activated carbon? (No support is required, this is a separate type of catalyst, chloroplatinic acid is directly supported on silica or activated carbon)

[0026] 24g1,3,5,7-Tetramethylcyclotetrasiloxane, 40g toluene and 0.1g p-hydroxyanisole were added to a four-necked flask with a thermometer and a condensing reflux tube, and the temperature was raised while stirring. When the temperature in the reactor reached 60°C, the mixture of prehe...

Embodiment 2

[0035] Mix 20.8g of 1,5-pentanediol diacrylate, 14.2g of hydroxypropyl methacrylate and 0.02g of tetrahydrofuran solution of chloroplatinic acid with a platinum concentration of 2000ppm in a flask, preheat at 50°C for 40min, and set aside . (no load required)

[0036] 24g1,3,5,7‐tetramethylcyclotetrasiloxane, 80g toluene and 0.1g p-hydroxyanisole were added to a four-necked flask with a thermometer and a condensing reflux tube, and the temperature was raised while stirring. When the temperature in the four-necked flask reached 60°C, the mixture of preheated 1,5-pentanediol diacrylate, hydroxypropyl methacrylate and tetrahydrofuran chloroplatinate solution was added dropwise to the four-necked flask, and the dropping time was for 2h. After the dropwise addition, the reaction temperature was controlled at 80° C. for 3 h. Then add 5g of activated carbon into the four-necked flask, and the adsorption time is 0.5h. Finally, the reacted solution was subjected to suction filtrati...

Embodiment 3

[0042] 19.8 g of 1,4-butanediol diacrylate, 24.8 g of γ-(methacryloxy)propyltrimethoxysilane and 0.03 g of platinum(0)-1,3-diethylene at a platinum concentration of 3200 ppm The base‐1,1,3,3‐tetramethyldisiloxane complex was mixed in a flask and preheated at 40°C for 50min, and then set aside.

[0043] Add 24g of 1,3,5,7‐tetramethylcyclotetrasiloxane (viscosity of 8mPa), 60g of toluene and 0.2g of p-hydroxyanisole into a four-necked flask with a thermometer and a reflux tube while stirring While raising the temperature, when the temperature in the four-necked flask reached 60°C, the preheated 1,4-butanediol diacrylate, γ-(methacryloyloxy)propyltrimethoxysilane and platinum (0) The mixture of ‐1,3‐divinyl‐1,1,3,3‐tetramethyldisiloxane complex was added dropwise into a four-neck flask, and the dropping time was 1.5h. After the dropwise addition, the reaction temperature was controlled at 90° C. for 2.5 h. Then add 5g of activated carbon into the four-necked flask, and the adso...

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Abstract

The invention discloses a modified hydrogen-containing cyclotetrasiloxane bonding accelerant as well as a preparation method and an application thereof. The preparation method comprises the following steps of: mixing an acrylic ester compound with a platinum catalyst solution, subsequently preheating at 30-60 DEG C, stirring and raising the temperature of 1,3,5,7-tetramethyl cyclotetrasiloxane, methylbenzene and para-hydroxybenzene methyl ether at the same time, when the temperature in a reactor is 30-80 DEG C, dropping a mixture which is preheated to be 30-60 DEG C, of the acrylic ester compound and the platinum catalyst solution, into the reactor, after the dropping, controlling the reaction temperature to be 50-90 DEG C, reacting for 0.5-4 hours, subsequently, adding activated carbon into the reactor to absorb for 0.5-3 hours, and after the absorption, sucking, filtering and evaporating the solution so as to obtain the bonding accelerant. By utilizing the bonding accelerant prepared by using the preparation method, the bonding property of addition-type liquid silica rubber is remarkably improved. The preparation process is simple, raw materials are cheap and easily obtained, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to the technical field of silicone material bonding, in particular to a modified hydrogen-containing cyclotetrasiloxane adhesion promoter and its preparation method and application; the adhesion promoter can improve the adhesion performance of addition-type liquid silicone rubber. Background technique [0002] In today's world, material science and technology are developing rapidly. Among them, addition-type liquid silicone rubber is widely used in many fields due to its excellent moisture resistance, water resistance, cold resistance, heat resistance, ultraviolet light resistance, insulation, radiation resistance and ozone resistance. Its main applications include: potting glue for electronic appliances, liquid injection molding glue and mold glue, etc. However, after the addition type liquid silicone rubber is vulcanized, most of the molecular surface is a non-polar organic group, so the adhesion to other materials is very poor....

Claims

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Application Information

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IPC IPC(8): C07F7/21C08K5/549C08L83/07C08K13/02C08K3/36C08K5/5445C09J11/06C09J183/07C09J11/04
Inventor 曾幸荣周为李红强赖学军汪昱辰王全苏俊柳肖贵斌汤胜山
Owner 广州纽楷美新材料科技有限公司
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