A kind of preparation method of room temperature curing high temperature resistant organic silica gel adhesive

A room temperature curing, silicone adhesive technology, applied in the preparation of silicone adhesives, high temperature and aging resistant room temperature curing silicone adhesives, can solve the problem of silicon oxygen bond breakage, colloid loss of elasticity and bonding ability, loss of sealing and bonding Use value etc.

Active Publication Date: 2021-05-14
武汉双键新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the silicon-oxygen chain segment is easily degraded at a high temperature of 250°C and above, it will cause the breakage and rearrangement of the silicon-oxygen bond, resulting in a decrease in the hardness, mechanical properties and adhesive properties of the sealant.
At a temperature of 300°C and above, the use value of sealing and bonding is basically lost
[0006] Ferrocene powder is directly introduced into the silicone adhesive system. After one day of continuous high-temperature aging at 300°C, compared with the silicone adhesive without ferrocene powder, the heat resistance has been significantly improved. The basic physical and mechanical properties before and after high temperature There is little change in performance, but after continuous high-temperature aging at 300°C and above for a week or even longer, the heat resistance will still decline significantly, and the colloid will completely lose its elasticity and bonding ability

Method used

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  • A kind of preparation method of room temperature curing high temperature resistant organic silica gel adhesive
  • A kind of preparation method of room temperature curing high temperature resistant organic silica gel adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation method provided in this example is as follows: pour 50 g of ferrocene lithium salt into a beaker, add 100 mL of toluene, stir to dissolve and set aside. Add 100 g of a mixture of methyltrichlorosilane and methyltrimethoxysilane, 100 mL of methanol into the flask, turn on nitrogen and stir. At room temperature, the toluene solution of the completely dissolved lithium ferrocene salt was dropped into the flask, and the dropping time was controlled to be 1 h. After the dropwise addition, react at room temperature for 3 h, and filter off the residue. Add 100mL of toluene and 35mL of pure water into the flask, mix the resulting product solution with 120g of a mixture of methyltrichlorosilane and methyltrimethoxysilane, and 50mL of methanol, and slowly drop it into the flask, controlling the dropping time for 3h. After the dropwise addition, the temperature was raised to 90°C, condensed and refluxed for 5 hours, cooled to room temperature, and the water layer ...

Embodiment 2

[0033] The preparation method provided in this example is as follows: pour 80 g of ferrocene chloride into a beaker, add 80 mL of toluene, stir to dissolve and set aside. Add 80 g of a mixture of dimethyldichlorosilane and trimethoxysilane, 80 mL of methanol to the flask, turn on nitrogen and stir. At room temperature, the toluene solution of the completely dissolved ferrocene chloride was dropped into the flask, and the dropping time was controlled to be 1 h. After the dropwise addition, react at room temperature for 5 h, and filter off the residue. Add 80mL of toluene and 30mL of pure water into the flask, mix the resulting product solution with 110g of a mixture of dimethyldichlorosilane and dimethyldimethoxysilane, and 50mL of methanol, and slowly drop them into the flask, controlling the dropping time for 3h . After the dropwise addition, raise the temperature to 90°C, condense and reflux for 6 hours, cool to room temperature, separate the water layer, neutralize the oi...

Embodiment 3

[0036] The preparation method provided in this example is as follows: pour 60 g of ferrocene ethanol into a beaker, add 100 mL of toluene, stir to dissolve and set aside. Add 100 g of tetrachlorosilane and methyl orthosilicate mixture, 100 mL of methanol into the flask, turn on nitrogen and stir. At room temperature, the completely dissolved ferrocene ethanol solution in toluene was dropped into the flask, and the dropping time was controlled to be 1 h. After the dropwise addition, react at room temperature for 8 h, and filter off the residue. Add 100mL of toluene and 35mL of pure water into the flask, mix the obtained product solution with 120g of tetrachlorosilane and methyl orthosilicate mixture, and 50mL of methanol, slowly drop into the flask, and control the dropping time for 3h. After the dropwise addition, raise the temperature to 90°C and reflux for 8 hours, cool to room temperature, separate the water layer, neutralize the oil layer with 10g of ammonium bicarbonate ...

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Abstract

The invention provides a method for preparing a room-temperature-curable high-temperature-resistant organic silica gel adhesive. Firstly, ferrocene polysiloxane is prepared, and then hydroxyl-terminated polydimethylsiloxane, filler, water remover, end-capping agent, poly Add siloxane ferrocene and end-capping catalyst into the reaction kettle in turn, start stirring and vacuum, heat up to the water removal reaction temperature and keep it warm for a period of time, heat up to the end-capping reaction temperature and keep it warm for a period of time; after cooling to room temperature, sequentially Add cross-linking agent and coupling agent into the kettle, mix well, then add organometallic catalyst, mix well, break the vacuum with nitrogen, discharge and pack. In this preparation method, the ferrocene group is introduced into the siloxane segment through the silane oxidation of ferrocene to improve the temperature resistance of the adhesive, and it can maintain good mechanical properties under the action of continuous high temperature of 300°C and above for a long time. strength and adhesive properties.

Description

technical field [0001] The invention provides a method for preparing a silicone adhesive, in particular to a method for preparing a high temperature and aging resistant room temperature curing silicone adhesive, which belongs to the technical field of silicone adhesive preparation. Background technique [0002] Room temperature curing silicone adhesive is a high molecular polymer formed by hydrolysis and condensation under humid conditions. It can be divided into a variety of types according to the different types of reactions. It is widely used in various industries such as construction, industry, and electronics. Applications. [0003] Room temperature curing silicone adhesive is a type of polysiloxane polymer with adhesiveness and sealing properties. The main structure is a linear, crosslinked or cyclic silicone polymer. The bond energy of the silicon-oxygen bond in the main chain is far Higher than polymers with carbon-carbon chains as the backbone, so siloxane polymers...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J183/04C09J183/08C09J11/04C09J11/06C08G77/22C08G77/16
CPCC08G77/16C08G77/22C08K2003/265C08K2201/011C08L2201/08C08L2205/025C08L2205/03C09J11/04C09J183/04C08L83/04C08L83/08C08K3/26
Inventor 孙雨声张喆朗珂洪建徐成华刘永刚雷木生游仁国
Owner 武汉双键新材料股份有限公司
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