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Nanometer composite epoxy resin self-repairing microcapsule and preparation method thereof

A technology for self-healing microcapsules and epoxy resins, applied in microcapsule preparations, microsphere preparations, etc., can solve the problems of low encapsulation efficiency, unstable thermodynamics and dynamics of emulsion droplets, and inability to provide structural stability, etc. The effect of improving mechanical strength and thermal stability, improving repair efficiency, and improving brittleness

Inactive Publication Date: 2012-07-25
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this emulsifier-stabilized emulsion droplet is thermodynamically and kinetically unstable, and it cannot provide sufficient structural stability to prevent the emulsion droplets from merging, resulting in inefficient encapsulation and the prepared microcapsules are also inefficient. can appear irregular in shape
Therefore, the stability of the emulsion is facing a huge challenge during the preparation of the capsule.

Method used

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  • Nanometer composite epoxy resin self-repairing microcapsule and preparation method thereof
  • Nanometer composite epoxy resin self-repairing microcapsule and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 50 mg of fumed silica nanoparticles were ultrasonically dispersed in 5 ml of deionized water, and 50 mg of PPG-TDI was shaken and dissolved in 5 ml of ethyl phenylacetate. The oil-water phase is mixed, shaken and emulsified by hand to obtain an oil-in-water Pickering emulsion stabilized by silica nanoparticles. Add 3.35ml of 37 wt% formaldehyde solution, 2ml of triethanolamine, 10ml of water and 1.75g ​​of melamine to a 50ml two-necked flask in turn, and stir magnetically at 60°C for 30min to obtain an aqueous solution of melamine-formaldehyde prepolymer. Add the oil-in-water Pickering emulsion obtained above dropwise into the aqueous solution of melamine-formaldehyde prepolymer, adjust the pH to 4 with acetic acid, heat to 50 °C at a heating rate of 5 °C / min, mechanically stir at 400 rpm, and react for 4 h . Cool down to room temperature at a rate of 2°C / min. The resulting suspension was washed three times with water, filtered, and dried at room temperature for 24 h ...

Embodiment 2

[0025]37.5 mg of fumed silica nanoparticles were ultrasonically dispersed in 5 ml of deionized water, and 5 mg of PPG-TDI was shaken and dissolved in 5 ml of ethyl phenylacetate. The oil-water phase is mixed, shaken and emulsified by hand to obtain an oil-in-water Pickering emulsion stabilized by silica nanoparticles. Add 3.35ml of 37 wt% formaldehyde solution, 2ml of triethanolamine, 10ml of water and 1.75g ​​of melamine to a 50ml two-necked flask in turn, and stir magnetically at 60°C for 30min to obtain an aqueous solution of melamine-formaldehyde prepolymer. Add the oil-in-water Pickering emulsion obtained above dropwise into the aqueous solution of melamine-formaldehyde prepolymer, adjust the pH to 3 with acetic acid, heat to 60 °C at a heating rate of 5 °C / min, mechanically stir at 200 rpm, and react for 3 h . Cool down to room temperature at a rate of 2°C / min. The resulting suspension was washed three times with water, filtered, and dried at room temperature for 24 h ...

Embodiment 3

[0027] 25 mg of fumed silica nanoparticles were ultrasonically dispersed in 5 ml of deionized water, and 100 mg of PPG-TDI was shaken and dissolved in 5 ml of ethyl phenylacetate. The oil-water phase is mixed, shaken and emulsified by hand to obtain an oil-in-water Pickering emulsion stabilized by silica nanoparticles. Add 3.35ml of 37 wt% formaldehyde solution, 2ml of triethanolamine, 10ml of water and 1.75g ​​of melamine to a 50ml two-necked flask in turn, and stir magnetically at 60°C for 30min to obtain an aqueous solution of melamine-formaldehyde prepolymer. Add the oil-in-water Pickering emulsion obtained above dropwise into the aqueous solution of melamine formaldehyde prepolymer, adjust the pH to 5 with acetic acid, heat to 40°C at a heating rate of 5°C / min, and mechanically stir at 600 rpm, and react for 5zz h . Cool down to room temperature at a rate of 2°C / min. The resulting suspension was washed three times with water, filtered, and dried at room temperature for ...

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Abstract

The invention discloses a nanometer composite epoxy resin self-repairing microcapsule and a preparation method of the microcapsule. The preparation method comprises the following steps: dispersing silicon dioxide nanometer particles in water, dissolving oil-soluble cross-linking agent into ethyl phenylacetate, mixing oil with water, and shaking by hand to vibrate and emulsify into Pickering latex; dripping the Pickering latex into melamine formaldehyde pre-polymer solution, and finally obtaining a target product by carrying out in-situ cross-linking polymerization of the pre-polymer at the surface of the latex drops under an acidic condition. Due to use of the stable Pickering latex drops as the template of the prepared microcapsule, the prepared microcapsule is regularly spherical, the size distribution is featured with polydispersity; the silicon dioxide particles doped in the capsule wall effectively enhance the mechanical strength and the thermal stability of the microcapsule, and synchronously increase the brittleness of the microcapsule; in this way, better releasing effect is obtained when the capsule of core material ethyl phenylacetate is broken.

Description

technical field [0001] The invention relates to the field of intelligent polymer materials, in particular to a microcapsule wrapped with an epoxy resin repair agent prepared by a Pickering emulsion droplet template method and a preparation method thereof. Background technique [0002] Thermosetting resins based on epoxy resins are used in a variety of fields, such as the automotive industry, aerospace, and electronics industries. However, epoxy-based composites are brittle due to their inherent properties, and are prone to microcracks inside the matrix when subjected to sustained loading. If these cracks are allowed to grow, it will inevitably lead to structural failure of the entire material. Therefore, it is imminent to prepare a smart responsive composite material that can automatically repair cracks to maintain structural integrity and prolong service life. According to literature reports (Nature, 2001, 409: 794-797), White successfully prepared a microcapsule for epox...

Claims

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Application Information

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IPC IPC(8): B01J13/18C08G59/50
Inventor 王朝阳杨宇童真
Owner SOUTH CHINA UNIV OF TECH
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