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Preparation method of vinyl polymer-coated nano-silica microspheres and modified epoxy resin

A technology of nano-silica and vinyl polymers, which is applied in the preparation of modified epoxy resins and vinyl polymer-coated nano-silica microspheres, which can solve the problems of difficult nuclear particle agglomeration and multi-core

Active Publication Date: 2019-04-02
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 of vinyl polymer-coated nano-silica microspheres and modified epoxy resin
  • Preparation method of vinyl polymer-coated nano-silica microspheres and modified epoxy resin
  • Preparation method of vinyl polymer-coated nano-silica microspheres and modified epoxy resin

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Experimental program
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preparation example Construction

[0034] see figure 1 , the preparation method of the vinyl polymer coating nano-silica microsphere of one embodiment, comprises the steps:

[0035] S10, placing the nano-silica microspheres in an organic solvent, uniformly dispersing, adding a coupling agent, stirring and reacting, and centrifuging and washing after the reaction, to obtain surface-modified nano-silica microspheres.

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

[0037] The organic solvent may be toluene or xylene or the like. 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 or vinyltriethoxysilane and the like.

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

[0040] The temperat...

Embodiment 1

[0079] 5g of nano-silica microspheres (500nm) were placed in 50mL of toluene, after stirring for a few minutes, γ-methacryloxypropyltrimethoxysilane was added, and the reaction was stirred at 145°C for 12 hours, wherein , the mass ratio of nano-silica microsphere particles to γ-methacryloxypropyltrimethoxysilane is 20:1, and after the reaction is completed, it is centrifuged and washed 4 times with ethanol to obtain surface-modified nano-silica Microspheres.

[0080] Weigh 1g of dried surface-modified nano-silica microspheres and place them in a mixed solution of 90g ethanol / water=65 / 35, and then ultrasonicate for 30min to disperse the silica microspheres evenly in the solution to form an emulsion a.

[0081] Then 10g of the above emulsion A, 0.25g buffer NaHCO 3 , the mass of the emulsifier SDBS is 0.01g, 0.03g, 0.05g mixed solution ultrasonic 10min, so that it is uniformly dispersed. Then put it into a three-neck flask equipped with a reflux condensing device and an elect...

Embodiment 2

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

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

[0087] Then 10g of the above emulsion B, 0.03g emulsifier SDBS, 0.25g buffer NaHCO 3 The mixed solution was ultrasonicated for 30 minutes to make it evenly dispersed. Then put 0.5mL, 2mL, and 3.5mL of monomeric styrene into a three-necked flask equipped with a reflux condensing device and an electric stirrer, stir at a c...

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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 nanocomposite materials, in particular to a method for preparing vinyl polymer-coated nano-silica microspheres and a modified epoxy resin containing the microspheres. Background technique [0002] Now people are increasingly demanding energy-saving, less-pollution, high-value-added, and high-functional products, and the requirements for materials are getting higher and higher. Therefore, composite materials have gradually become a research hotspot. Composite polymer emulsions, especially organic-inorganic composite 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 summary, when used as a coating, inorganic-organic co...

Claims

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Application Information

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Patent Type & Authority Patents(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