Preparation method of polyurethane acrylate oligomer surface modified silica

A polyurethane acrylic acid and acrylate-based technology, which is applied in the treatment of dyed low-molecular organic compounds, dyed high-molecular organic compounds, and fibrous fillers. The effect of simple operation steps and simple process

Active Publication Date: 2013-03-27
WUXI CHUANGDA ELECTRONICS
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  • Abstract
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  • Application Information

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Problems solved by technology

On the other hand, most of the monomers used in the polymers involved in the surface modif

Method used

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  • Preparation method of polyurethane acrylate oligomer surface modified silica
  • Preparation method of polyurethane acrylate oligomer surface modified silica
  • Preparation method of polyurethane acrylate oligomer surface modified silica

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Embodiment 1

[0022] (1) Synthesis of silica and its modification by sol-gel method: 600 mL of absolute ethanol, 34.8 mL of 28% ammonia water, and Ionized water 11.2mL, heat up to 50°C, then slowly add 22.4mL tetraethyl orthosilicate into the flask, stir and react at 50°C for 24 hours, and obtain a silica ethanol solution (particle size is about 70nm). Take 53mL of silicon dioxide ethanol solution and add it to a 100mL three-necked flask, raise the temperature to 50°C, slowly add 0.2mL of 3-aminopropyltriethoxysilane (APTES) dropwise, stir and react at a constant temperature of 50°C for 24h, then add absolute ethanol Repeated centrifugal washing 3 times, ultrasonically dispersed in dehydrated acetone to obtain silane-modified silica.

[0023] (2) Synthesis of isocyanate-terminated polyurethane acrylate oligomers: Add 0.055mol (12.4g) isophorone diisocyanate (IPDI) into a 100mL three-necked flask equipped with a stirrer, thermometer and reflux condenser , heated to 50°C, then slowly added 0...

Embodiment 2

[0026] (1) Synthesis of silica and its modification by sol-gel method: Add 600 mL of absolute ethanol, 34.8 mL of ammonia water, and 11.2 mL of deionized water into a 1000 mL three-necked flask equipped with a stirrer, thermometer and reflux condenser in sequence , raised the temperature to 50°C, then slowly added 22.4 mL of tetraethyl orthosilicate into the flask, stirred at 50°C for 24 hours, and then obtained the silica ethanol solution (particle size about 70nm). Take 53mL of silicon dioxide ethanol solution and add it to a 100mL three-neck flask, raise the temperature to 50°C, slowly add 0.2ml of 3-aminopropyltriethoxysilane (APTES) dropwise, stir and react at a constant temperature of 50°C for 24h, then add absolute ethanol Repeated centrifugal washing 3 times, ultrasonically dispersed in dehydrated acetone to obtain silane-modified silica.

[0027] (2) Synthesis of isocyanate-terminated polyurethane acrylate oligomers: Add 0.055mol (12.4g) isophorone diisocyanate (IPDI)...

Embodiment 3

[0030] (1) Synthesis of silica and its modification by sol-gel method: Add 600 mL of absolute ethanol, 34.8 mL of ammonia water, and 11.2 mL of deionized water into a 1000 mL three-necked flask equipped with a stirrer, a thermometer and a reflux condenser in sequence , raised the temperature to 50°C, then slowly added 22.4 mL of tetraethyl orthosilicate into the flask, stirred at 50°C for 24 hours, and then obtained the silica ethanol solution (particle size about 70nm). Take 53mL of silicon dioxide ethanol solution and add it to a 100mL three-necked flask, raise the temperature to 50°C, slowly add 0.2ml of 3-aminopropyltriethoxysilane (APTES) dropwise, stir and react at a constant temperature of 50°C for 24 hours, then repeat with absolute ethanol Wash by centrifugation for 3 times, and ultrasonically disperse into dehydrated acetone to obtain silane-modified silica.

[0031] (2) Synthesis of isocyanate-terminated polyurethane acrylate oligomers: Add 0.055mol (12.4g) isophoro...

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Abstract

A preparation method of polyurethane acrylate oligomer surface modified silica belongs to the technical field of nanoparticle surface modification. The method provided by the invention comprises steps of: first synthesizing nano silica by a sol-gel method, and modifying the nano silica with an amino silane coupling agent; reacting acrylate macromonomers with diisocyanate monomers to synthesize an isocyanate group-terminated polyurethane acrylate oligomer; and then reacting the oligomer with the amino silane coupling agent modified silica particles to obtain oligomer surface modified silica. The oligomer modified silica has good dispersion and stability in organic solvents, such as toluene and ethyl acetate and can be used as an additive and a crosslinking agent in the fields of photocuring coating, adhesive, plastic, rubber and novel nano composite material, with promising application prospect.

Description

technical field [0001] The invention relates to a preparation method of a novel oligomer surface-modified silicon dioxide, in particular to a preparation method of a polyurethane acrylate oligomer surface-modified silicon dioxide. The invention belongs to the technical field of nano particle surface modification. technical background [0002] In recent years, organic-inorganic composite materials have attracted extensive attention from academia and industry due to their characteristics of both organic polymers and inorganic nanoparticles, and have special properties unmatched by other common materials, and have gradually become a research hotspot. However, organic polymerization The compatibility problem between organic matter and inorganic nanoparticles has always been a major bottleneck restricting its excellent performance, and the surface modification of inorganic nanoparticles is an effective way to solve their dispersion and compatibility in organic substrates. way. ...

Claims

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Application Information

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IPC IPC(8): C09C1/28C09C3/08C09C3/10C08K9/04C08K3/36C08L75/14
Inventor 张胜文郭盟陈子栋张燕刘晓亚
Owner WUXI CHUANGDA ELECTRONICS
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