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Prepn process of acrylate modified gamma-aminopropyl triethoxysilane

An aminopropyltriethoxysilane and acrylate technology, which is applied in the field of preparation of acrylate-modified γ-aminopropyltriethoxysilane, can solve problems such as insufficient heat resistance and water resistance, and achieve phase The effect of poor capacitance and uniformity, simple and feasible experiment, and stable modification process

Inactive Publication Date: 2007-06-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention utilizes the primary aminosilane coupling agent produced in large quantities to obtain a secondary aminosilane coupling agent with excellent performance and low cost through certain modification means, and applies it to polyurethane acrylic resin to solve its insufficient heat resistance and water resistance Shortcomings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Add 10g of γ-aminopropyltriethoxysilane (KH550) into a four-necked flask, connect a thermometer and a stirring paddle, pass high-purity nitrogen for 20 minutes, and heat up to 60°C; within 30 minutes, 3.89 g methyl acrylate was dropped, and then kept at 60° C. for 2 hours to obtain the modified silane coupling agent secondary aminosilane.

[0031] (2) Add 100g of polyether polyol (N-220) and 50g of acrylate resin into a four-necked flask, heat up to 60°C, mix for half an hour and then heat up to 110°C, pump under a vacuum of -0.1Mpa Water and acrylic acid monomer were removed from the mixture under vacuum for 2.5 hours until distillate free.

[0032] (3) Then cool down to 50°C, release the vacuum; add 30.62g of diphenylmethane diisocyanate (MDI) after 30 minutes of high-purity nitrogen gas, heat up to 80°C after the end of the exothermic peak, and degas after 3 hours of heat preservation Discharge, obtain light yellow urethane acrylate prepolymer.

[0033] (4) Add...

Embodiment 2

[0035] (1) Add 10g of γ-aminopropyltriethoxysilane (KH550) into a four-necked flask, connect a thermometer and a stirring paddle, pass high-purity nitrogen gas for 20 minutes, and heat up to 100°C; within 15 minutes, 4.52 g of ethyl acrylate was dropped, and then kept at 60° C. for 1 hour to obtain the modified silane coupling agent secondary aminosilane.

[0036] (2) Add 150g of polyether polyol (N-220) and 50g of acrylate resin into a four-necked flask, heat up to 60°C, mix for half an hour and then heat up to 110°C, pump under a vacuum of -0.15Mpa Water and acrylic acid monomer were removed from the mixture under vacuum for 2.5 hours until distillate free.

[0037] (3) Then cool down to 20°C, release the vacuum; add 30.76g of toluene diisocyanate (TDI) after 30 minutes of high-purity nitrogen gas, heat up to 60°C after the end of the exothermic peak, degas and discharge the material after the heat preservation reaction for 3 hours, A pale yellow urethane acrylate prepolyme...

Embodiment 3

[0040] (1) Add 10g of γ-aminopropyltriethoxysilane (KH550) into a four-necked flask, connect a thermometer and a stirring paddle, pass high-purity nitrogen gas for 20 minutes, and heat up to 40°C; within 60 minutes, 5.78g The butyl acrylate was dropped, and then kept at 60° C. for 3 hours to obtain the modified silane coupling agent secondary aminosilane.

[0041](2) Add 200g of polyether polyol (N-220) and 50g of acrylate resin into a four-neck flask, heat up to 60°C, mix for half an hour and then heat up to 110°C, pump under a vacuum of -0.2Mpa Water and acrylic acid monomer were removed from the mixture under vacuum for 2.5 hours until distillate free.

[0042] (3) Then cool down to 50°C, release the vacuum; add 41.08g of toluene diisocyanate (TDI) after 30 minutes of high-purity nitrogen gas, heat up to 70°C after the end of the exothermic peak, degas and discharge the material after the heat preservation reaction for 3 hours, A pale yellow urethane acrylate prepolymer wa...

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PUM

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Abstract

The present invention discloses preparation process of acrylate modified gamma-aminopropyl triethoxysilane. The preparation process includes: dropping acrylate monomer into primary amino gamma-aminopropyl triethoxysilane at 40-100 deg.c within 15-60 min, maintaining the temperature to react for 1-3 hr to obtain modified silane coupler, mixing polyether polyol and hydroxyl acrylic acid and vacuumizing to obtain mixture, adding diisocyanate into the mixture to produce exothermic reaction, heating to 60-100 deg.c after exothermic reaction to react for further 1-3 hr to obtain the pre-polymer of terminal isocyanate, dropping the modified silane coupler into the pre-polymer to react at 60-100 deg.c for 1-3 hr to obtain the acrylate modified gamma-aminopropyl triethoxysilane. The present invention has smooth modification process, simple operation and low cost, and the obtained modified silane coupler has low viscosity and high stability.

Description

technical field [0001] The invention relates to the modification of a silicone coupling agent, in particular to a preparation method of acrylate-modified γ-aminopropyltriethoxysilane. Background technique [0002] The silane coupling agent can form a strong and stable adhesive bond through the "molecular bridge" at the two weak adhesive interfaces, and connect two substances with different properties. The molecular structure of silane is generally expressed as follows: [0003] (RO) 3 Si-(CH 2 ) 3 -X [0004] R = alkyl (methyl, ethyl, etc.) [0005] X = organic functional group (mercapto, amino, epoxy, etc.) [0006] It can be seen from the above molecular structure that the silane coupling agent contains alkoxysilane that can undergo hydrolysis and silane polycondensation at a certain humidity, and the organic functional group X has certain compatibility with the organic resin. reactions or physicochem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08G18/48C08G18/62C08G18/10C08G18/83C08K5/5415
Inventor 修玉英王功海罗钟瑜
Owner SOUTH CHINA UNIV OF TECH
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