Synthesis method of polysilsesquioxane coupling agent for RTV (Room Temperature Vulcanization) silicone rubber and ketoxime-removed silicone rubber

The technology of a siloxane coupling agent and an aminosilane coupling agent is applied to the synthesis method of a polysilsesquioxane coupling agent and the field of deketoxime type silicone rubber, which can solve the problem of large randomness of the viscosity of the target product and increase production. Time, difficult to obtain coupling agent and other problems, to achieve the effect of large market application and development potential, reduce solvent cost, and improve synthesis efficiency

Active Publication Date: 2021-11-12
广东高士高科实业有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with the use of strong acid and strong base is that the purification at the end of the reaction becomes complicated. The reaction system must be neutralized to acidity, and operations such as filtration and liquid separation are performed, which increases production time and costs.
In addition, tetramethylammonium hydroxide solution is used as a catalyst, but the price is expensive, and the compound is sensitive to air
The third is to add solvent (ethanol, isopropanol, etc.) to react at high temperature (above 80° C.). This synthesis method needs to use a large amount of solvent. After the reaction, it needs to be distilled for a long time, and the high temperature condition consumes high energy, which does not meet the requirements of green chemistry. Require
Fourth, the viscosity of the target product is random during the synthesis process, and it is difficult to obtain a coupling agent with the target viscosity to meet different user needs

Method used

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  • Synthesis method of polysilsesquioxane coupling agent for RTV (Room Temperature Vulcanization) silicone rubber and ketoxime-removed silicone rubber
  • Synthesis method of polysilsesquioxane coupling agent for RTV (Room Temperature Vulcanization) silicone rubber and ketoxime-removed silicone rubber
  • Synthesis method of polysilsesquioxane coupling agent for RTV (Room Temperature Vulcanization) silicone rubber and ketoxime-removed silicone rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 250mL three-necked flask, add 20g of aminopropyltriethoxysilane, 20g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 20g of ethyl orthosilicate, 0.2g of pure Water and 1 g of triethylamine were used as hydrolysis accelerators. After the addition was completed, the stirring was turned on at a rotation speed of 100 rpm, and the temperature of the oil bath was raised to 65° C., and the reaction was stirred for 1.5 hours. After the reaction is completed, carry out distillation. At a vacuum degree of 0.09-0.1MPa and a temperature of 80°C, after distillation for 1 hour, a colorless and transparent liquid product is obtained. The coupling agent does not have a viscosity peak in the production of the rubber material, and the rubber material is not yellow. Change, viscosity 62mPa·s.

[0027] Preparation steps of deketoxime type silicone rubber: at room temperature, mix 100 parts of 107 glue, 150 parts of nano-calcium, 11 parts of methyl silicone oil, 10 parts of methyl trib...

Embodiment 2

[0029] In a 250mL three-necked flask, add 20g of aminopropyltriethoxysilane, 20g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 20g of ethyl orthosilicate, 0.5g of pure Water and 1 g of triethylamine were used as hydrolysis accelerators. After the addition was completed, the stirring was turned on at a rotation speed of 100 rpm, and the temperature of the oil bath was raised to 65° C., and the reaction was stirred for 1.5 hours. After the reaction is completed, carry out distillation. At a vacuum degree of 0.09-0.1MPa and a temperature of 80°C, after distillation for 1 hour, a colorless and transparent liquid product is obtained. The coupling agent does not have a viscosity peak in the production of the rubber material, and the rubber material is not yellow. Change, viscosity 237mPa·s.

[0030] Preparation steps of deketoxime type silicone rubber: at room temperature, mix 100 parts of 107 glue, 150 parts of nano-calcium, 11 parts of methyl silicone oil, 10 parts of methyl tri...

Embodiment 3

[0032] In a 250mL three-necked flask, add 20g of aminopropyltriethoxysilane, 20g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 20g of ethyl orthosilicate, 0.8g of pure Water and 1 g of triethylamine were used as hydrolysis accelerators. After the addition was completed, the stirring was turned on at a rotation speed of 100 rpm, and the temperature of the oil bath was raised to 65° C., and the reaction was stirred for 1.5 hours. After the reaction is completed, carry out distillation. At a vacuum degree of 0.09-0.1MPa and a temperature of 80°C, after distillation for 1 hour, a colorless and transparent liquid product is obtained. The coupling agent does not have a viscosity peak in the production of the rubber material, and the rubber material is not yellow. Change, viscosity 259mPa·s.

[0033] Preparation steps of deketoxime type silicone rubber: at room temperature, mix 100 parts of 107 glue, 150 parts of nano-calcium, 11 parts of methyl silicone oil, 10 parts of methyl tri...

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Abstract

The invention discloses a synthesis method of a polysilsesquioxane coupling agent for RTV (Room Temperature Vulcanization) silicone rubber, which comprises the following steps: putting 20 parts by weight of amino silane coupling agent, 20 parts by weight of epoxy silane coupling agent, 10-20 parts by weight of other functional silane, 1.0-2.0 parts by weight of low-boiling-point hydrolysis accelerant and 0.2-1.0 part by weight of pure water into a reaction kettle with a stirring function, and conducting reacting for 1.5-2 hours while stirring at the kettle temperature of 65-80 DEG C at the stirring rotating speed of 60-100 rpm; and starting a vacuum pump, and carrying out vacuum distillation on the reaction kettle for 0.9-1.1 hours under the conditions that the vacuum degree is 0.09-0.1 MPa and the kettle temperature is 80-100 DEG C, so as to obtain a transparent liquid product, namely the polysilsesquioxane coupling agent. By using the method, the process equipment is simple, the raw materials are cheap and easy to obtain, the method is safe and environment-friendly, and the prepared product can be directly used as the tackifier of the RTV silicone rubber silicone adhesive, so that the production cost is reduced, the economic benefit is created, the production efficiency is improved, and the environmental pollution is reduced. The invention also discloses a ketoxime removal type silicone rubber prepared from the polysilsesquioxane coupling agent.

Description

technical field [0001] The invention relates to a method for synthesizing a polysilsesquioxane coupling agent used for RTV silicone rubber and a deketoxime type silicone rubber, belonging to the technical field of fine chemicals. Background technique [0002] Silane coupling agent is an important industrial additive, which can be used to couple organic and inorganic substances, as a tackifier, crosslinking agent and curing agent for silicone rubber and silicone resin, and as a textile finishing agent, paint additives and more. Since there are two functional groups in the middle of the silane coupling agent molecule, which are organic and inorganic, it can connect two materials with different chemical structure types and affinity at the interface, adding coatings and inorganic primers and pigments, fillers and polymers. combination between. [0003] Polysilsesquioxane (POSS), especially cage-shaped polysilsesquioxane, has been widely studied in the fields of reinforcement a...

Claims

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Application Information

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IPC IPC(8): C08G77/06C08G77/26C09J129/14C09J11/08
CPCC08G77/045C08G77/06C08G77/26C09J129/14C09J11/08C08L83/08
Inventor 陈君行程小莲翟晓旭胡新嵩李万华徐文杰王少辉钟志贤张杰龙
Owner 广东高士高科实业有限公司
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