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Low-temperature-resistant neutral silicone sealant and preparation method thereof

A silicone sealant, low temperature resistant technology, applied in the field of silicone adhesive, can solve the problems of carcinogenic risk and inapplicability, and achieve the effect of ensuring bonding strength, improving environmental protection, and improving deep curing speed

Active Publication Date: 2022-03-08
HANGZHOU ZHIJIANG SILICONE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, butanone oxime type silicone rubber vulcanization by-product is butanone oxime, butanone oxime has a carcinogenic risk, and it is not suitable for environments with high environmental protection requirements such as cold storage.

Method used

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  • Low-temperature-resistant neutral silicone sealant and preparation method thereof
  • Low-temperature-resistant neutral silicone sealant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0043] Preparation Example 1, an aminosilane oligomer, was prepared according to the following steps:

[0044] S101: In a 3000ml three-necked flask, add 1500g aminopropyltrimethoxysilane and ammonia 250g methanol, then install a reflux condenser, a thermometer and a constant pressure dropping funnel on the three-necked flask, and make the three-necked flask under stirring conditions The temperature of the mixture is raised to 50°C, and then a mixed solution of 50g of water and 150g of methanol is dropped through a constant pressure dropping funnel to promote the full hydrolysis of the aminosilane coupling agent to obtain a hydrolyzate;

[0045] S102: Heat the hydrolyzate to 100°C, polymerize for 1.5 hours, and collect methanol by distillation under reduced pressure to obtain a prepolymer, then continue to heat the prepolymer to 130°C, polymerize for 2 hours, and cool down to room temperature to obtain an average degree of polymerization of 6 aminosilane oligomers.

preparation example 2

[0046] Preparation 2, an aminosilane oligomer, was prepared according to the following steps:

[0047] S101: In a 3000ml three-necked flask, add 1500g of aminopropyltriethoxysilane and ammonia 250g methanol, then install a reflux condenser, a thermometer and a constant pressure dropping funnel on the three-necked flask, and make the three-necked flask The temperature of the mixture was raised to 50°C, and then a mixed solution of 30g of water and 170g of methanol was dropped through a constant pressure dropping funnel to promote the full hydrolysis of the aminosilane coupling agent to obtain a hydrolyzed product;

[0048] S102: Heat the hydrolyzate to 100°C, polymerize for 1 hour, and collect methanol by vacuum distillation to obtain a prepolymer, then continue to heat the prepolymer to 120°C, polymerize for 2 hours, and cool it down to room temperature to obtain a compound with an average degree of polymerization of 3. Aminosilane oligomers.

preparation example 3

[0049] Preparation Example 3, an aminosilane oligomer, was prepared according to the following steps:

[0050] S101: In a 3000ml three-necked flask, add 1500g N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and 300g methanol of ammonia, then install a reflux condenser, a thermometer and a constant pressure dropping funnel on the three-necked flask , under stirring conditions, the temperature of the mixture in the three-necked flask was raised to 50 ° C, and then the mixed solution of 50 g of water and 150 g of methanol was dropped through a constant pressure dropping funnel to promote the sufficient hydrolysis of the aminosilane coupling agent to obtain a hydrolyzed product;

[0051] S102: Heat the hydrolyzate to 100°C, polymerize for 2 hours, and collect methanol by vacuum distillation to obtain a prepolymer, then continue to heat the prepolymer to 130°C, polymerize for 2.5 hours, and cool it down to room temperature to obtain an average degree of polymerization of 9 aminosila...

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Abstract

The invention discloses a low-temperature-resistant neutral silicone sealant, which is prepared from the following raw materials in parts by mass: 90 to 110 parts of 107 base glue; 80 to 130 parts of nano calcium carbonate; 0.1 to 2 parts of fumed silica; 10 to 30 parts of methyl silicone oil; 6 to 15 parts of a cross-linking agent; 0.6 to 2 parts of a coupling agent; the cross-linking agent is an acetoxime silane cross-linking agent. The silicone sealant prepared by the invention generates a cancerogen diacetylmonoxime in the use process, has relatively high environmental protection performance, and can meet the bonding performance required in low-temperature and high-humidity environments and the like.

Description

technical field [0001] The invention relates to the field of silicone glue, in particular to a low-temperature-resistant neutral silicone sealant and a preparation method thereof. Background technique [0002] The deketoxime type silicone sealant releases small neutral molecules during the curing process, so it is a neutral glue. At present, the most widely used ketoxime silicone glue on the market is the butyroxime silicone glue. Tributyroxime silane, dimethyl dibutyroxime silane, tetrabutyl ketoxime silane, etc., have good adhesion to various substrates. [0003] However, the by-product of the vulcanization of butanone oxime type silicone rubber is butanone oxime, which has a carcinogenic risk and is not suitable for environments with high environmental requirements such as cold storage. Contents of the invention [0004] In order to improve the environmental protection performance of the deketoxime type silicone adhesive, the application provides a low-temperature res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J183/04C09J11/04C09J11/06C09J11/08
CPCC09J183/04C09J11/04C09J11/06C09J11/08C08K2201/011C08K2003/265C08L83/04C08L83/08C08K5/544C08K3/26C08K5/5465C08K7/26Y02E10/50
Inventor 倪建华沈翔倪皇伟凌建峰沈永飞徐俊刘明何永富
Owner HANGZHOU ZHIJIANG SILICONE CHEM
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