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Preparation method for epoxy microcapsule by taking polyurethane as wall material

A polyurethane and microcapsule technology, applied in the field of self-healing concrete and self-healing materials, can solve problems such as difficult to achieve, and achieve the effects of uniform wall thickness, good sphericity and smooth surface

Inactive Publication Date: 2014-03-19
SHENZHEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] There is a document [Research on the Reaction Law of Isocyanate with Alcohol and Water, Gu Jiyou, Gao Zhenhua, Science Technology and Engineering, 3(5), 2003, 462-463] further shows that the reaction rate of isocyanate and water is faster than that of alcohol. In the presence of both, the concentration of alcohol must be much higher than the concentration of water (more than 10 times) to make the main product polyurethane. Obviously, this condition is difficult to achieve in the oil-in-water emulsion system

Method used

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  • Preparation method for epoxy microcapsule by taking polyurethane as wall material
  • Preparation method for epoxy microcapsule by taking polyurethane as wall material

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preparation example Construction

[0011] The invention provides a kind of preparation method that takes polyurethane as the epoxy microcapsule of wall material, comprises the following steps:

[0012] S1: Preparation of polyurethane prepolymer terminated with isocyanate;

[0013] S2: Mix the isocyanate-terminated polyurethane prepolymer with epoxy resin, add emulsifier and water, stir and emulsify to make an oil-in-water emulsion;

[0014] S3: heating up, the interface reacts to form the capsule wall;

[0015] S4: filtering, rinsing the sediment with water, and drying to obtain microcapsules with polyurethane as the wall material and epoxy resin as the core material.

[0016] Specifically, the process of step S1 is: mix the hydroxyl compound, isocyanate, solvent, and catalyst, heat up to 50-80°C, stir and react at a speed of 100-500rpm for 2-3 hours to obtain a polyurethane prepolymer; the hydroxyl compound Dihydroxyl compounds or polyhydroxyl compounds are included; the isocyanate includes diisocyanate or p...

Embodiment 1

[0030] Take 1.38g of glycerol, 10g of IPDI, 5g of acetone, and 0.03g of catalyst DBTDL, mix them evenly, add them into a three-necked flask, stir and react at 60°C and 300rpm for 2-3h, and obtain a polyurethane prepolymer terminated with isocyanate; After mixing the prepolymer with 18g of epoxy E-51 evenly, add it to a three-necked flask filled with 100g of 1wt% PVA aqueous solution, emulsify at 20°C and 1000rpm for 10min, and keep it at 60°C for 1-2h. After cooling, the reaction solution was filtered, the filter cake was washed with distilled water, and then filtered three times, and then dried at 45°C for 12 hours to obtain polyurethane-coated epoxy microcapsules. Fourier transform infrared analysis was carried out on the microcapsules, and the experimental results are as follows: figure 1 As shown, there are characteristic absorption peaks of ester bonds (O=C-O) in polyurethane at 1720, 1650 and 773 cm-1, which proves that the wall material of the microcapsules prepared by ...

Embodiment 2

[0032] Take 3g of polyethylene glycol, 6g of IPDI, 5g of acetone, and 0.03g of catalyst DBTDL, mix them evenly, add them into a three-necked flask, stir and react at 60°C and 300rpm for 2-3 hours, and obtain a polyurethane prepolymer terminated with isocyanate; After mixing the prepolymer with 10g of epoxy E-51 evenly, add it to a three-necked flask filled with 100g of 1wt% PVA aqueous solution, emulsify at 20°C and 1000rpm for 10min, and keep it at 60°C for 1-2h. After cooling, the reaction solution was filtered, the filter cake was washed with distilled water, and then filtered three times, and then dried at 45°C for 12 hours to obtain polyurethane-coated epoxy microcapsules.

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Abstract

A disclosed preparation method for an epoxy microcapsule by taking polyurethane as a wall material mainly comprises the following steps: preparing an isocyanate-terminated polyurethane prepolymer; mixing the isocyanate- terminated polyurethane prepolymer with epoxy resin, adding an emulsifier and water, stirring and performing an emulsification reaction to prepare an oil-in-water emulsion; heating and performing an interface reaction to form a capsule wall; and filtering, rinsing the precipitate with water and drying to obtain the microcapsule by taking polyurethane as the wall material and taking epoxy resin as the core material. The prepared epoxy microcapsule by taking polyurethane as the wall material is good in epoxy microcapsule sphericility, smooth in surface and uniform in wall thickness, and is applicable to prepare microcapsule type self-repair materials.

Description

technical field [0001] The invention relates to the field of self-repairing materials, in particular to the field of self-repairing concrete. Specifically, it relates to the preparation of microcapsule epoxy resin repair agent in self-healing materials. Background technique [0002] Self-healing material is a kind of smart material, which can automatically repair defects such as cracks and voids in it when it is damaged. Microcapsule self-healing concrete refers to a structural composite material in which a liquid repair agent is microencapsulated and then pre-embedded in a cement matrix together with coarse and fine aggregates. When micro-cracks occur in concrete components, the stress at the tip of the cracks breaks the microcapsules, and the repair agent flows out, allowing the cracks to heal autonomously. Epoxy resin is often used as a repair agent in engineering, so the preparation of epoxy microcapsules is the most important step in realizing the self-repair of micro...

Claims

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Application Information

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IPC IPC(8): B01J13/14C08G18/75C08G18/32C08G18/48
CPCB01J13/14C08G18/10C08G18/58
Inventor 朱光明邬治平汤皎宁董必钦王险峰韩宁旭邢峰
Owner SHENZHEN UNIV
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