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Epoxy microcapsule with polyurea as wall material and preparation method thereof

A microcapsule and wall material technology, which is applied in the field of epoxy microcapsules and its preparation, can solve the problems of unsuitable epoxy microcapsule wall material and loss of repair function, etc., and achieve simple shape control, smooth surface and good sphericity Effect

Inactive Publication Date: 2013-10-02
SHENZHEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In industry, microcapsules with polyurea as wall material have been widely used in the fields of spices, pesticides, phase change energy storage, etc., but in the field of self-healing materials, polyurea is generally not used as wall material to cover Oxygen, because the polyamine used in the preparation of polyurea is also a curing agent for epoxy resin. In the process of reacting with polyisocyanate to form polyurea wall material, polyamine will also cure epoxy and lose its repair function.
Moreover, especially linear polyurea, because of its good elasticity, is not suitable as a wall material for epoxy microcapsules

Method used

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  • Epoxy microcapsule with polyurea as wall material and preparation method thereof
  • Epoxy microcapsule with polyurea as wall material and preparation method thereof
  • Epoxy microcapsule with polyurea as wall material and preparation method thereof

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preparation example Construction

[0015] Embodiments of the present invention also provide a method for preparing epoxy microcapsules using polyurea as a wall material, which includes the following steps:

[0016] S01: Disperse polyisocyanate and liquid epoxy resin in water containing surfactant to obtain a mixed solution, wherein the polyisocyanate and liquid epoxy resin are the oil phase, and the water containing surfactant is the water phase , the polyisocyanate includes ternary or more than ternary polyisocyanate, the mass ratio of the oil phase to the water phase is 1:5-10, and the mass ratio of the polyisocyanate to the liquid epoxy resin in the oil phase is 1 : 1~2.3, the concentration of surfactant in the water phase is 0.5~3%;

[0017] S02: Stir the mixed solution at 25-90° C. for 0.5-5 hours, filter, wash and dry to obtain the epoxy microcapsules with polyurea as the wall material.

[0018] Wherein, in step S01, the polyisocyanate is 4,4′,4″-triphenylmethane triisocyanate (TTI), tris(4-isocyanatophe...

Embodiment 1

[0029] Mix 8g of TTI (molecular weight 367), 10g of epoxy E-51, and 1.5g of acetone evenly, add to a three-necked flask containing 100g of 1% PVA solution, and emulsify at 60°C and 1000rpm for 30min. Reduce the rotation speed to 400 rpm, add 0.03 g of catalyst dibutyltin dilaurate (DBTDL), and keep the reaction at 60°C for 3 hours. The reaction solution was filtered, washed with distilled water, filtered again, and repeated three times, and then dried at 45° C. for 12 hours to obtain a white powder of polyurethane-coated epoxy microcapsules. SEM observation confirmed that microcapsules with a particle size distribution of 20-70 μm and a wall thickness of 800-1000 nm were obtained, such as figure 1 shown. Fourier transform infrared spectroscopy (FTIR) analysis found that at 1640cm -1 There is a strong urea C=O group absorption peak, which proves that the wall material is polyurea. After the microcapsules are crushed with a mortar, observed with an optical microscope, it can ...

Embodiment 2

[0031]Weigh 8g DTTI (molecular weight 436), add a small amount of ethyl acetate to make a solution, mix it with 10g epoxy E-51 evenly, add it to a three-necked flask with 100g 1% SMA (Scripset520) solution, at 15°C, 1000rpm After emulsifying for 10 minutes, reduce the rotation speed to 400 rpm, add 0.03 g of catalyst DBTDL after mixing evenly, raise the temperature to 60 ° C, and keep it warm for 3 hours. The reaction solution was filtered, washed with distilled water, filtered again, and repeated three times, and then dried at 45° C. for 12 hours to obtain a white powder of polyurethane-coated epoxy microcapsules. SEM observation shows microcapsules with a particle size distribution of 20-80 μm and a wall thickness of 800-900 nm. FTIR spectrum confirmed that the wall material was polyurea. Observation of the pulverized microcapsules with an optical microscope reveals sticky liquid epoxy flowing out.

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Abstract

The invention relates to the technical field of self repair materials and provides an epoxy microcapsule with polyurea as a wall material. The core material of the microcapsule comprises liquid epoxy resin, the wall material of the microcapsule is crosslinked polyurea prepared by carrying out an interface reaction on polyisocyanate and water, and the polyisocyanate comprises polyisocyanate containing three elements or more than three elements. The invention also provides a preparation method of the epoxy microcapsule with polyurea as the wall material. The preparation method of the epoxy microcapsule with polyurea as the wall material comprises the following steps of: dispersing polyisocyanate and liquid epoxy resin into water containing a surface active agent to obtain a mixed solution, stirring the mixed solution for 0.5-5 hours at the temperature of 25-90 DEG C, filtering, washing, and drying, so that the epoxy microcapsule with polyurea as the wall material is obtained. The preparation method of the epoxy microcapsule with polyurea as the wall material is simple and practicable and is applicable to industrial production.

Description

technical field [0001] The invention belongs to the technical field of self-repairing materials, and in particular relates to an epoxy microcapsule with polyurea as a wall material and a preparation method thereof. Background technique [0002] The self-healing material is to pre-embed the repair agent in the polymer or concrete matrix. When cracks occur inside the matrix, the stress concentration at the tip of the crack releases the repair agent, penetrates into the crack under capillary action, and undergoes a curing reaction to repair the crack. . Epoxy resin has become the first choice of repair agent because of its good adhesion, low shrinkage during curing, stable performance, and long storage period. The method of embedding epoxy resin is to microencapsulate it. [0003] Polyurea is a polymer commonly used as the wall material of microcapsules. It is usually formed by polycondensation of polyisocyanate and polyamine compound. In industry, microcapsules with polyure...

Claims

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Application Information

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IPC IPC(8): B01J13/14C08G18/30
CPCB01J13/14B01J13/16C08G18/305C08G18/7657C08G18/7664C08G18/776C08G59/188C08L63/00C08L75/02
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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