Double-capsule self-repairing epoxy coating and preparation method thereof

An epoxy coating, self-healing technology, used in microcapsule preparations, microsphere preparation and other directions, can solve the problems of low encapsulation efficiency, inability to provide sufficient structural stability, emulsion droplet fusion, demulsification, etc., to improve the encapsulation efficiency. volume, improve repair efficiency, and prevent the effect of milk droplet fusion

Inactive Publication Date: 2016-08-10
SOUTH CHINA UNIV OF TECH
2 Cites 30 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Most traditional methods use emulsifier-stabilized emulsions to prepare microcapsules, but such emulsifier-stabilized emulsions often cannot provide sufficient...
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Abstract

The invention discloses a double-capsule self-repairing epoxy coating and a preparation method thereof. The preparation method mainly uses Pickering emulsion droplet template method and conducts an interface polymerization of interface isophorone diisocyanate and tetraethylenepentamine in water-oil of epoxy interface to prepare epoxy microcapsule and tetraethylenepentamine microcapsule; and the two microcapsules are added to epoxy resin microcapsules for the formation of double-capsule self-repairing epoxy coating. The Pickering emulsion droplet template method ensures the stability of the emulsion, prevents emulsion droplet blending, improves package amount and efficiency of the microcapsule core material; Pickering emulsion improves the repair efficiency of the double-capsule self-repairing epoxy coating; the introduction of nano silica particles and nano clay in the capsule walls of the epoxy microcapsule and tetraethylenepentamine microcapsule improves the mechanical strength and thermal stability of the microcapsule wall, but also improves the brittleness of the microcapsule and the releasing efficiency of the microcapsule core material, so as to ensure the repair performance of the double-capsule self-repair coating.

Application Domain

Microballoon preparationMicrocapsule preparation

Technology Topic

ChemistrySilicon dioxide +12

Image

  • Double-capsule self-repairing epoxy coating and preparation method thereof

Examples

  • Experimental program(5)

Example Embodiment

[0027] Example 1
[0028] (1) Add 1 g of polyvinyl alcohol (polymerization degree 2600) to 100 mL of deionized water, and magnetically stir for 12 h at 80°C to obtain an aqueous solution of polyvinyl alcohol. Add 30 mg of silica nanoparticles to 6 mL of polyvinyl alcohol aqueous solution for ultrasonic dispersion for 1 min, add 3 g of epoxy resin, mix the oil and water, and emulsify at 9000 rpm high-speed shear to obtain a stable oil-in-water skin of silica nanoparticles Kelin emulsion; then add 300 ml isophorone diisocyanate to Pickering emulsion and mix well to obtain a mixed solution. After dissolving 300 mL of tetraethylenepentamine in 3 mL of deionized water, add it to the mixed solution and let stand at room temperature for 40 minutes to obtain an epoxy microcapsule suspension. The suspension was washed 3 times with water, filtered, and dried at room temperature for 24 h , Get epoxy microcapsules.
[0029] (2) Add 1 g of polyisobutylene (molecular weight 2400) to 100 mL of xylene and stir magnetically for 12 h at 85°C to obtain a polyisobutylene xylene solution. In 8 mL of polyisobutylene xylene solution, 40 mg of nanoclay was added to ultrasonic dispersion for 1 min to form an oil phase. Dissolve 2 g of tetraethylenepentamine in 2 g of deionized water and then add it to the oil phase, mix the oil and water phase, and emulsify at 9000 rpm high-speed shear to obtain a nanoclay-stable water-in-oil Pickering emulsion. Dissolve 200 mL of isophorone diisocyanate in 2 mL of xylene and add the prepared water-in-oil Pickering emulsion, shake gently to mix. Let stand at room temperature for 40 min to obtain the tetraethylenepentamine microcapsule suspension, wash the suspension 3 times with xylene, filter, and dry in a fume hood at room temperature for 24 h to obtain tetraethylenepentamine microcapsules.
[0030] (3) Clean the iron sheet with ethanol, remove the grease on the surface, and polish it with sandpaper. After cleaning with ethanol, let it stand and dry at room temperature for later use. Mix 5 g of epoxy resin and 0.5 g of tetraethylene pentamine uniformly, as the matrix material of the self-healing material. Then add 10% epoxy microcapsules and 5% tetraethylenepentamine microcapsules relative to the mass fraction of the base material, mix them evenly and coat them on the spare iron sheet, and dry for 24 hours at room temperature to form a double-capsule self-healing epoxy coating . Such as figure 1 As shown, when the self-healing coating produces cracks, the microcapsules covering epoxy resin and tetraethylenepentamine will rupture as the cracks occur, and the repair agent will be released, which is formed by the reaction of epoxy resin and tetraethylenepentamine The new polyurethane can realize self-healing function.

Example Embodiment

[0031] Example 2
[0032] (1) Add 1 g of polyvinyl alcohol (polymerization degree 2600) to 100 mL of deionized water, and magnetically stir for 12 h at 80°C to obtain an aqueous solution of polyvinyl alcohol. Add 30 mg of silica nanoparticles to 6 mL of polyvinyl alcohol aqueous solution for ultrasonic dispersion for 1 min, add 1.8 g of epoxy resin to mix the oil and water, and emulsify at 3000 rpm high-speed shear to obtain a stable oil-in-water skin of silica nanoparticles Kling lotion. Then add 180 mL of isophorone diisocyanate to Pickering emulsion and mix well to obtain a mixed solution. After dissolving 150 mL of tetraethylenepentamine in 3 mL of deionized water, add it to the mixed solution. Let it stand for 40 min at room temperature to obtain an epoxy microcapsule suspension. The suspension was washed 3 times with water, filtered, and dried at room temperature for 24 h to obtain epoxy microcapsules.
[0033] (2) Add 1 g of polyisobutylene (molecular weight 2400) to 100 mL of xylene and stir magnetically for 12 h at 85°C to obtain a polyisobutylene xylene solution. In 8 mL of polyisobutylene xylene solution, 40 mg of nanoclay was added to ultrasonic dispersion for 1 min to form an oil phase. After dissolving 1.3 g of tetraethylenepentamine in 2 g of deionized water, adding the oil phase, mixing the oil and water phase, and emulsifying at 3000 rpm high-speed shear to obtain a nanoclay-stable water-in-oil Pickering emulsion. Dissolve 100 mL of isophorone diisocyanate in 2 mL of xylene and add the prepared water-in-oil Pickering emulsion, shake gently to mix. Let stand at room temperature for 40 min to obtain the tetraethylenepentamine microcapsule suspension, wash the suspension 3 times with xylene, filter, and dry in a fume hood at room temperature for 24 h to obtain tetraethylenepentamine microcapsules.
[0034] (3) Clean the iron sheet with ethanol, remove the grease on the surface, and polish it with sandpaper. After cleaning with ethanol, let it stand and dry at room temperature for later use. Mix 5 g of epoxy resin and 0.5 g of tetraethylene pentamine uniformly, as the matrix material of the self-healing material. Then add 10% epoxy microcapsules and 2% tetraethylenepentamine microcapsules relative to the mass fraction of the base material, mix them evenly and coat them on the spare iron sheet, and dry for 24 hours at room temperature to form a double-capsule self-healing epoxy coating . When the double-capsule self-healing epoxy coating of this embodiment cracks, the microcapsules enclosing epoxy resin and tetraethylenepentamine will break as the cracks occur, and the repairing agent will be released. The pentaamine reacts to form a new polyurethane, which can realize the self-repair function.

Example Embodiment

[0035] Example 3
[0036] (1) Add 1 g of polyvinyl alcohol (polymerization degree 2600) to 100 mL of deionized water, and magnetically stir for 12 h at 80°C to obtain an aqueous solution of polyvinyl alcohol. Add 30 mg of silica nanoparticles to 6 mL of polyvinyl alcohol aqueous solution for ultrasonic dispersion for 1 min, add 4.2 g of epoxy resin, mix the oil and water, and emulsify at 6000 rpm to obtain a stable oil-in-water skin of silica nanoparticles. Kling lotion. Then add 480 mL of isophorone diisocyanate to Pickering emulsion and mix well to obtain a mixed solution. After dissolving 450 mL of tetraethylenepentamine in 3 mL of deionized water, add it to the mixed solution. Let it stand for 40 min at room temperature to obtain an epoxy microcapsule suspension. The suspension was washed 3 times with water, filtered, and dried at room temperature for 24 h to obtain epoxy microcapsules.
[0037] (2) Add 1 g of polyisobutylene (molecular weight 2400) to 100 mL of xylene and stir magnetically for 12 h at 85°C to obtain a polyisobutylene xylene solution. In 8 mL of polyisobutylene xylene solution, 40 mg of nanoclay was added to ultrasonic dispersion for 1 min to form an oil phase. Dissolve 3 g of tetraethylenepentamine in 2 g of deionized water and then add the oil phase to mix the oil and water phase, and emulsify at 6000 rpm high-speed shear to obtain a nanoclay-stable water-in-oil Pickering emulsion. Dissolve 300 mL of isophorone diisocyanate in 2 mL of xylene and add the prepared water-in-oil Pickering emulsion, shake gently to mix. Let stand at room temperature for 40 min to obtain the tetraethylenepentamine microcapsule suspension, wash the suspension 3 times with xylene, filter, and dry in a fume hood at room temperature for 24 h to obtain tetraethylenepentamine microcapsules.
[0038] (3) Clean the iron sheet with ethanol, remove the grease on the surface, and polish it with sandpaper. After cleaning with ethanol, let it stand and dry at room temperature for later use. Mix 5 g of epoxy resin and 0.5 g of tetraethylene pentamine uniformly, as the matrix material of the self-healing material. Then add 5% epoxy microcapsules and 5% tetraethylenepentamine microcapsules relative to the mass fraction of the matrix material, mix them evenly and coat them on the spare iron sheet, dry at room temperature for 24 hours to form a double-capsule self-healing epoxy coating . When the double-capsule self-healing epoxy coating of this embodiment cracks, the microcapsules enclosing epoxy resin and tetraethylenepentamine will break as the cracks occur, and the repairing agent will be released. The pentaamine reacts to form a new polyurethane, which can realize the self-repair function.

PUM

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