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Preparation method of silica powder for epoxy resin system

A technology of epoxy resin system and silicon micropowder, which is applied in the field of composite material preparation, can solve the problems of agglomeration, uneven dispersion, influence of material properties, etc.

Active Publication Date: 2021-08-27
JIANGSU NOVORAY NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when microsilica powder is directly used as an organic phase filler, the material performance is not ideal in many cases, mainly due to the existence of silanol groups on its surface, which leads to poor affinity with polymeric organic materials, uneven dispersion when used as a filler, and even formation of group, which has a great impact on the properties of the material, so it is necessary to modify its surface

Method used

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  • Preparation method of silica powder for epoxy resin system
  • Preparation method of silica powder for epoxy resin system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: Experiment 1 for the preparation method of silicon micropowder in epoxy resin system

[0029] Add 1.5kg of silicon micropowder into the high-speed mixing modifier, set the temperature at 140°C, add the pre-hydrolyzed γ-(2,3-glycidyloxy)propyltrimethoxysilane mixed solution (7.5g coupling agent, 7.5g ethanol and 15g deionized water, the hydrolysis time is 20min, and the hydrolysis pH is 4.0), modified for 20min to obtain primary modified silica powder; add 1.5kg primary modified silica powder to the wet modification machine, Add the pre-hydrolyzed N-phenyl-γ-aminopropyltrimethoxysilane mixture (7.5g coupling agent, 7.5g ethanol and 15g deionized water, the hydrolysis time is 20min, the hydrolysis pH is 7.5), and the temperature is set At 80°C, modify for 60 minutes to obtain hydrophobic silicon micropowder for epoxy resin.

[0030] refer to figure 1 middle, figure 1 Medium, 474 cm -1 The bending vibration absorption peak at Si-O-Si bond; 798 cm -1 The ...

Embodiment 2

[0031] Embodiment 2: The preparation method experiment two that is used for epoxy resin system silicon micropowder

[0032] Add 1.5kg of silicon micropowder into the high-speed mixing modifier, set the temperature to 150°C, add the pre-hydrolyzed γ-(2,3-glycidyloxy)propyltrimethoxysilane mixture (7.5g coupling agent, 7.5g ethanol and 15g deionized water, the hydrolysis time is 20min, and the hydrolysis pH is 4.0), modified for 20min to obtain primary modified silica powder; add 1.5kg primary modified silica powder to the wet modification machine, Add the pre-hydrolyzed N-phenyl-γ-aminopropyltrimethoxysilane mixture (7.5g coupling agent, 7.5g ethanol and 15g deionized water, the hydrolysis time is 20min, the hydrolysis pH is 7.5), and the temperature is set At 80°C, modify for 60 minutes to obtain hydrophobic silicon micropowder for epoxy resin.

Embodiment 3

[0033] Embodiment 3: Experiment 3 for the preparation method of silicon micropowder in epoxy resin system

[0034] Add 1.5kg of silicon micropowder into the high-speed mixing modifier, set the temperature to 150°C, add the pre-hydrolyzed γ-(2,3-glycidyloxy)propyltrimethoxysilane mixture (7.5g coupling agent, 7.5g ethanol and 15g deionized water, the hydrolysis time is 20min, and the hydrolysis pH is 4.0), modified for 20min to obtain primary modified silica powder; add 1.5kg primary modified silica powder to the wet modification machine, Add the pre-hydrolyzed N-phenyl-γ-aminopropyltrimethoxysilane mixture (7.5g coupling agent, 7.5g ethanol and 15g deionized water, the hydrolysis time is 20min, the hydrolysis pH is 7.5), and the temperature is set at 90°C and modified for 60 minutes to obtain hydrophobic silicon micropowder for epoxy resin.

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Abstract

The invention relates to a preparation method of silica powder for an epoxy resin system, which adopts a silane coupling agent for two-step modification, that is, firstly, gamma-(2, 3-epoxypropoxy) propyltrimethoxysilane is adopted for dry modification of silica powder to obtain primary modified silica powder; and by carrying out wet modification on the primary modified silica powder by adopting N-phenyl-gamma-aminopropyl trimethoxy silane, the modified silica powder is obtained . The method disclosed by the invention is simple in process, the prepared modified silica powder is high in activation degree, good in hydrophobicity and low in surface hydroxyl group content, the characteristic of poor hydrophobicity of single modified silica powder of an epoxy coupling agent is made up, when the modified silica powder is applied to an epoxy resin system, the viscosity is greatly reduced, and the dispersity in resin is greatly improved.

Description

technical field [0001] The invention belongs to the field of composite material preparation, and relates to a method for preparing silicon micropowder for epoxy resin systems. Background technique [0002] Compared with other common inorganic fillers such as attapulgite, microsilica powder exhibits better mechanical properties, heat resistance, dispersibility, and electrical properties. However, when microsilica powder is directly used as an organic phase filler, the material performance is not ideal in many cases, mainly due to the existence of silanol groups on its surface, which leads to poor affinity with polymeric organic materials, uneven dispersion when used as a filler, and even formation of Groups have a great impact on the properties of materials, so it is necessary to carry out surface modification. Contents of the invention [0003] The object of the present invention is to provide a method for modifying silicon micropowder in epoxy resin system. The method c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/06C08K3/36C08L63/00
CPCC08K9/06C08K3/36C08L63/00
Inventor 曹家凯孙小耀刘亚飞王聿东周垒周紫文
Owner JIANGSU NOVORAY NEW MATERIAL CO LTD