A kind of secondary aminosilane modified polyether polymer and preparation method thereof

A technology of secondary aminosilane and polyether polymer, which is applied in the field of secondary aminosilane modified polyether polymer and its preparation, can solve the problems of high price, complicated preparation, gel, etc., and achieve low environmental pollution, convenient construction, Produce reproducible results

Active Publication Date: 2021-05-07
SHANGHAI DONGDA CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the preparation methods of existing silane-modified polyether polymers, some use terminal isocyanate group silane coupling agents to carry out capping modification to polyether polyols, but the price of current isocyanate group silane coupling agents is very expensive, There are very few domestic production applications, most of which are imported from abroad, and the preparation is complicated
Some commercially available primary amino silanes are used to block and modify isocyanate-terminated polyurethane prepolymers. However, primary amino silanes have high primary hydrogen atom activity, strong ammonia odor, and strong alkalinity. When the isocyanate-terminated polyether / polyurethane prepolymer is end-capped or modified, it is prone to gel phenomenon; and the sealant prepared by using this type of silane-modified polyether is prone to yellowing

Method used

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  • A kind of secondary aminosilane modified polyether polymer and preparation method thereof
  • A kind of secondary aminosilane modified polyether polymer and preparation method thereof

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preparation example Construction

[0040]In a specific embodiment, the present invention provides a method for preparing a secondary amino silicone modified polyether polymer, comprising the steps of:

[0041](1) Dehydrating the polyether polyol under vacuum conditions of 90 to 130 ° C, degassing from 1 to 4 h, then cooling to 50 to 80 ° C, adding diisocyanate and catalyst to polyether polyol, control diisocyanate The molar ratio of the hydroxyl group of the cyananate and the polyether polyol is from 1.1 to 2: 1; high purity nitrogen gas is introduced, stirred well, and then at 50 to 90 ° C for 1 to 6 h, and the terminal isocyanate-based polyether prepolymer is obtained.

[0042](2) Mix the end isocyanate-based polyether prepolymer and secondary amino silisily mixed with secondary amino group and isocyanate molar ratio of 0.9 to 1.2: 1, at 30 to 90 ° C, high purity nitrogen protection reaction 1 ~ 6h until the system ends the reaction when there is no sanocyanate, then the bubbles were removed in the reaction temperature, ...

Embodiment 1

[0059](1) In the four-mouth flask equipped with a stirrer, a constant voltage drip funnel, and a gas tube, an endone-eatel polyether (S1010, Shanghai Dongda Chemical Co., Ltd.) is sequentially added. Getting nitrogen and stirring, add γ-aminopropyltrimethoxysilane, olelene polyether and gamma-aminopropyltrimethoxysilane in 1: 1, 30 minutes by weight at 40 ° C. After completion, then warmed to 90 ° C, reaction for 4 h, resulting in a secondary aminoisilyl coupling agent.

[0060](2) Polyether polyol (C2160, Shanghai Dongda Chemical Co., Ltd.) dehydrated under vacuum conditions at 110 ° C, degassing to 60 ° C, then cool down to 60 ° C, then cool down to 60 ° C, then add TDI (diisocyanate) The molar ratio of the hydroxyl group of isocyanate and the polyether polyol is 2: 1), dibutyltin (0.1% of the polyether polyol mass) in Dihuo (0.1% of the polyether polyol), and the mixing is uniform, The reaction was reacted at 90 ° C for 1 h to obtain an end isocyanate-based polyether prepolymer, and...

Embodiment 2

[0063](1) In the four-mouth flask equipped with a stirrer, a constant voltage drop, the gas tube, a 10-parts having average molecular weight of 1000 is sequentially added, and nitrogen gas is introduced into nitrogen and the stirring, 40 ° C The γ-aminopropyltriethoxysilane, the olelene polyether and the γ-aminopropyltriethoxysilane were added to 1: 1, 30 minutes, and then heated to 90 ° C , The reaction is 4 h to obtain a secondary aminoisilyl coupling agent.

[0064](2) Polyether polyol (C2060, Shanghai Dongda Chemical Co., Ltd.) will be dehydrated under vacuum conditions at 110 ° C under vacuum conditions at 110 ° C, then cool down to 60 ° C, then add TDI (diisocyanate) The molar ratio of the hydroxyl isocyanate and the polyether polyol of 1.3: 1), dibutyltin (0.1% of the mass polyol mass), and passed into high purity nitrogen as reaction protective gas, stir well. The reaction was at 50 ° C for 6 h, and the terminal isocyanate-based polyether prepolymer was obtained, and the NCO co...

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Abstract

This application relates to a preparation method of secondary aminosilane-modified polyether polymer, which includes (1) dehydrating and degassing polyether polyol under vacuum conditions of 90-130°C for 1-4 hours, and then lowering the temperature to 50-80°C ℃, add diisocyanate and catalyst to polyether polyol, pass inert gas, stir evenly, and then react at 50-90 ℃ for 1-6h to obtain isocyanate-terminated polyether prepolymer; (2) Mix the isocyanate-terminated polyether prepolymer with secondary aminosilane, react at a temperature of 30-90°C and under the protection of an inert gas for 1-6 hours, until the system is titrated without the presence of isocyanate, and then the reaction Air bubbles are removed in vacuum at high temperature to obtain the secondary aminosilane-modified polyether polymer. The present application also relates to a secondary aminosilane modified polyether polymer. The present application also relates to a secondary aminosilane. The preparation process of the silane-modified polyether polymer of the present application is easy to control, and no gel phenomenon will occur, and the sealant thus prepared is not prone to yellowing.

Description

Technical field[0001]The present application relates to the field of sealant technology, and in particular, a secondary amino silicone modified polyether polymer and a preparation method thereof.Background technique[0002]In recent years, the research is increasingly increased by seal modification of the silane coupling agent to the end isocyanate-based polyether prepolymer. The silane-modified polyether polymer is transformed into a silane oxide group of the prepolymer to a silane oxide, and the end-based silane oxide can hydrolyze the crosslinking reaction, so that the silane modified polyether polymer solidification is formed with Si-O-Si. Elastomer of the mesh structure. Further, only a small amount of alcohol is released in the hydrolysis crosslinking process, which is small to environmentally pollution. The silane-modified polyether polymer can be cured with a strong chemical adhesion to the surface of the non-porous substrate (such as glass, metal, etc.). Silane modified polye...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/48C08G18/50C08G18/73C08G18/75C08G18/76C09J175/08C09J11/04C09J11/06
CPCC08G18/48C08G18/482C08G18/5096C08G18/73C08G18/755C08G18/7671C08K2003/265C08K2201/014C09J11/04C09J11/06C09J175/08C08K13/02C08K3/26C08K5/12C08K5/544C08K5/5425
Inventor 徐军何志强李欣怡聂永倩
Owner SHANGHAI DONGDA CHEM
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