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Silicon micro-powder with surface chemical modification, preparation method and application of same

A surface chemical and surface modification technology, which is applied in the field of surface modification of non-metallic materials, can solve the problems of high rigidity and easy delamination of epoxy adhesive, and achieve the effect of improving toughness and good dispersibility

Active Publication Date: 2017-12-22
BEIJING INST OF AEROSPACE CONTROL DEVICES
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  • Description
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Problems solved by technology

[0004] The purpose of the present invention is to provide a surface chemical modification solution for the existing inorganic fillers in epoxy potting adhesives, sealants and adhesives, which are easy to delaminate, settle, and make epoxy adhesives more rigid. Silica powder and its preparation method, so that the filler has better dispersion in the epoxy glue and can improve the low-temperature performance such as the toughness of the epoxy glue

Method used

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  • Silicon micro-powder with surface chemical modification, preparation method and application of same
  • Silicon micro-powder with surface chemical modification, preparation method and application of same
  • Silicon micro-powder with surface chemical modification, preparation method and application of same

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preparation example Construction

[0034] see figure 1 , the embodiment of the present invention provides a method for preparing surface chemically modified silicon micropowder, comprising the following steps:

[0035] Step (1), carrying out hydroxylation treatment on the surface of silicon micropowder;

[0036] Step (2), mixing and reacting the surface hydroxylated silicon micropowder with a coupling agent to obtain coupling agent modified silicon micropowder;

[0037] Step (3), adding organosilane to the coupling agent-modified silicon micropowder obtained in step (2) for reaction to obtain surface-modified silicon micropowder.

[0038] Specifically, the hydroxylation treatment described in step (1) includes:

[0039] Add silicon micropowder into dilute sodium hydroxide solution, reflux reaction under stirring condition for 1-5 hours, separate solid phase components, and then wash separated solid phase components with acidic alcohol solution to obtain surface hydroxylated silicon micropowder. In the embodi...

Embodiment 1

[0055] 1. The embodiment of the present invention provides a surface chemically modified silica powder, the specific preparation method is as follows:

[0056]10.0 g of microsilica filler was immersed in 50 ml of dilute sodium hydroxide solution with a mass fraction of 5%, and reflux reaction was carried out at 90° C. for 3 h under constant temperature and stirring. After the reaction is completed, centrifuge to obtain the solid phase components, and use an ethanol solution with a mass fraction of 3% and a pH value of 4 to wash the solid phase components. The number of times of washing is twice, and the consumption of each ethanol solution is 30ml to obtain a surface Hydroxylated silica powder.

[0057] Add 1.0 g of KH-550 silane coupling agent to 19.2 ml of ethanol aqueous solution (ethanol: water = 9:1, mass ratio), and adjust the pH of the system to 8. Add the surface-hydroxylated silicon micropowder into the coupling agent solution, stir evenly, and then reflux at 80° C. ...

Embodiment 2

[0069] 1. The embodiment of the present invention provides a surface chemically modified silica powder, the specific preparation method is as follows:

[0070] 10.0 g of microsilica filler was immersed in 50 ml of dilute sodium hydroxide solution with a mass fraction of 5%, and reflux reaction was carried out at 90° C. for 3 h under constant temperature and stirring. After the reaction is completed, centrifuge to obtain the solid phase components, use a mass fraction of 3%, and use an ethanol solution with a pH value of 4 to wash the solid phase components. The number of times of washing is twice, and the consumption of each ethanol solution is 30ml to obtain a surface Hydroxylated silica powder.

[0071] Add 5.0g KH-550 silane coupling agent to 96ml ethanol aqueous solution (ethanol:water=9:1, mass ratio), adjust the pH of the system to 8. Add the surface-hydroxylated silicon micropowder into the coupling agent solution, stir evenly, and then reflux at 80° C. for 3 hours. A...

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Abstract

The invention provides a silicon micro-powder with surface chemical modification, and a preparation method and an application of same, and belongs to the field of surface modification for non-metal-based materials. The preparation method includes the following steps: treating the surface of surface-hydroxylated silicon micro-powder with a silane coupling agent; and performing chemical grafting to the surface with epoxy group-terminated organosilane to form filler which has high surface toughness and has high compatibility and dispersibility in epoxy glue. Compared with silicon micro-powder without surface chemical modification, the preparation method enables the filler to have high dispersibility in epoxy glue, can effectively improve the toughness of the epoxy glue, and is very suitable for the fields of anti-low-temperature epoxy pouring sealants, sealing adhesives and bonding adhesives.

Description

technical field [0001] The invention relates to a surface chemically modified silicon micropowder and its preparation method and application, belonging to the field of surface modification of non-metal base materials. Background technique [0002] Metal bonding parts or ceramic component products infused with epoxy often encounter cracking during high and low temperature cycles, which affects the normal use of the product. The main cause of cracking is the mismatch of the coefficient of linear expansion between the epoxy adhesive and the bond or potting material. The adhesive joints are prone to accumulate a large amount of thermal stress under high and low temperature cycle conditions, resulting in cracking (especially in low temperature environments). Therefore, it is of great significance to reduce the linear expansion coefficient of the adhesive and improve the toughness of the adhesive. [0003] Adding fillers to epoxy adhesives is an important way to reduce the linea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/06C09C3/08C09C3/10C09C3/12C09J163/00C09J11/04C01B33/021
Inventor 李彦博梁涛陈永秀姚竹贤李宇梅于兰萍严小军
Owner BEIJING INST OF AEROSPACE CONTROL DEVICES
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