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Preparation method for vinyl polymer coated nano-silica microsphere and modified epoxy resin

A nano-silica, vinyl polymer technology, applied in the preparation and application of nano-composite materials, can solve the problems of difficult to solve nuclear particle agglomeration, multi-core and so on

Active Publication Date: 2017-04-26
SHENZHEN INST OF ADVANCED ELECTRONICS MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when coating nanoparticles, the agglomeration of nuclear particles is not easy to solve, and there is a multi-nuclear phenomenon.

Method used

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  • Preparation method for vinyl polymer coated nano-silica microsphere and modified epoxy resin
  • Preparation method for vinyl polymer coated nano-silica microsphere and modified epoxy resin
  • Preparation method for vinyl polymer coated nano-silica microsphere and modified epoxy resin

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preparation example Construction

[0034] See figure 1 , The preparation method of vinyl polymer coated nano silica microspheres in one embodiment includes the following steps:

[0035] S10. Place the nano-silica microspheres in an organic solvent, add a coupling agent after uniform dispersion, stir the reaction, and centrifuge and wash after the reaction is completed to obtain surface-modified nano-silica microspheres.

[0036] Wherein, the particle size of the nano-silica microspheres may be 70 nm-1000 nm.

[0037] The organic solvent may be toluene or xylene. The mass-volume ratio of nano-silica microspheres to organic solvent is 1:25g / mL-1:10g / mL.

[0038] The coupling agent may be a double bond type silane coupling agent. Specifically, the double bond type silane coupling agent may be γ-methacryloxypropyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, or the like.

[0039] The mass ratio of nano silica microspheres to coupling agent can be 20:1-20:8.

[0040] The temperature of the stirring reaction ...

Embodiment 1

[0079] Put 5g of nano-silica microspheres (500nm) in 50mL toluene, stir for a few minutes, add γ-methacryloxypropyltrimethoxysilane, and then stir and react at 145°C for 12 hours. The mass ratio of nano-silica microsphere particles to γ-methacryloxypropyltrimethoxysilane is 20:1. After the reaction is completed, it is centrifuged and washed with ethanol for 4 times to obtain surface-modified nano-silica Microspheres.

[0080] Weigh 1g of the dried surface-modified nano-silica microspheres in a mixed solution of 90g ethanol / water=65 / 35, and then sonicate for 30min to make the silica microspheres uniformly dispersed in the solution to form an emulsion A.

[0081] Then 10g of the above emulsion A, 0.25g buffer NaHCO 3 , The mixed solution of emulsifier SDBS with masses of 0.01g, 0.03g, and 0.05g is ultrasonicated for 10min to make it uniformly dispersed. Then it was put together with 2 mL of monomeric styrene into a three-necked flask equipped with a reflux condenser and an electric...

Embodiment 2

[0085] Put 5g of nano-silica microspheres (500nm) in 50mL of xylene, stir for a few minutes, add vinyltrimethoxysilane, and then stir and react at 145°C for 15 hours. Among them, nano-silica microspheres The mass ratio of the particles to the vinyltrimethoxysilane is 20:8, and after the reaction is completed, they are centrifuged and washed with ethanol for 5 times to obtain surface-modified nano-silica microspheres.

[0086] Weigh 1g of the dried surface-modified nano-silica microspheres in a mixed solution of 90g ethanol / water=65 / 35, and then sonicate for 15min to disperse the silica microspheres evenly in the solution to form an emulsion B.

[0087] Then 10g the above emulsion B, 0.03g emulsifier SDBS, 0.25g buffer NaHCO 3 The mixed solution is sonicated for 30min to make it evenly dispersed. Then respectively put 0.5mL, 2mL, 3.5mL of monomeric styrene into a three-necked flask equipped with reflux condenser and electric stirrer, stir at a certain speed, and perform pre-emulsif...

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Abstract

The invention provides a preparation method for a vinyl polymer coated nano-silica microsphere and a preparation method for a modified epoxy resin containing the vinyl polymer coated nano-silica microsphere. The preparation method for the vinyl polymer coated nano-silica microsphere comprises the following steps: using a coupling agent for modifying the surface of a nano-silica microsphere and then adding a vinyl monomer for performing emulsion polymerization coating, thereby acquiring the monodispersity vinyl polymer coated nano-silica microsphere. The preparation method has the advantages of low energy consumption, high product purity, high dispersity and no environmental pollution. The coating state of the vinyl polymer on the surface of the nano-silica microsphere can be controlled by changing the reaction condition. According to the preparation method for the modified epoxy resin, a composite microsphere is used for modifying the epoxy resin, so that the viscosity and dispersity of the epoxy resin matrix can be excellently improved and the problem of unmatched coefficient of thermal expansion in a bottom filling glue can be effectively solved, but most of all, the impact strength and fracture toughness of the epoxy resin composite can be obviously promoted.

Description

Technical field [0001] The invention relates to the technical field of preparation and application of nano composite materials, and in particular to a preparation method of vinyl polymer coated nano silica microspheres and a modified epoxy resin containing the microspheres. Background technique [0002] Now people are increasingly calling for products with energy saving, less pollution, high added value, and high functionality, and the requirements for materials are getting higher and higher. Therefore, composite materials have gradually become a hot spot for people to study. Hybrid polymer emulsions, especially organic-inorganic hybrid polymer emulsions, have attracted more and more attention due to their wide applications in coatings, adhesives, biomedicine, electronics, fiber and paper processing. Using this composite emulsion as a coating not only overcomes many shortcomings of general-purpose coatings, but also develops many new uses. In short, when used as a coating, inorg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/10C08K9/06C08K3/36C08G59/42C08L63/00C08F292/00C08F212/08
CPCC08F292/00C08G59/4215C08K3/36C08K9/06C08K9/10C08K2201/011C08L63/00C08F212/08
Inventor 孙蓉何亚川李刚朱朋莉赵涛
Owner SHENZHEN INST OF ADVANCED ELECTRONICS MATERIALS