含胺类固化剂的聚甲基丙烯酸甲酯微胶囊的制备及其表征

Preparation and Characterization of Polymethyl Methacrylate Microcapsules Containing Amine Curing Agents

本文以固化剂聚醚胺(D230)为芯材,聚甲基丙烯酸甲酯(PMMA)为壳材,采用溶剂挥发法制备了包裹胺类固化剂的微胶囊,并研究了芯-壳质量比、表面活性剂类型、搅拌速度、温度、稳定剂浓度等不同因素对微胶囊平均粒径和芯材含量的影响。同时,采用傅里叶变换红外(FTIR)、光学显微镜、差示扫描量热法(DSC)和热重分析(TGA)等对微胶囊的化学结构、形貌及热力学性能进行了表征。实验结果表明:当芯-壳质量比为2:1~4:1、采用复合型表面活性剂、温度为40℃、搅拌速度为1000 rpm、稳定剂浓度为2 wt%时,制备的微胶囊较理想。将该微胶囊加入环氧树脂中可制得外援型自修复环氧材料。随着微胶囊添加量的增加,损伤样品膜表面的裂纹自修复效果逐渐明显。当添加量为10 wt%时,复合材料具有较好的自修复性能。

In this paper, a series of microcapsules containing amine curing agents was prepared by the solvent volatilization method with polyether amine(D230) as core material and polymethyl methacrylate(PMMA) as shell material.The influence of different factors, such as the core shell mass ratio, the types of surfactant, stirring speed, temperature, and concentration of stabilizers, on the average particle size and core material content of the microcapsules was systematically studied. Meanwhile, Fourier transform infrared(FTIR), optical microscopy, differential scanning calorimetry(DSC),dynamic mechanical analysis(DMA) and thermogravimetric analysis(TGA) were also used to characterize the chemical structure, morphology and thermodynamic properties of the microcapsules. The experimental results show that when the core-shell mass ratio was 2:1-4:1, the optimal microcapsules could be obtained with the employment of compound surfactant at 40 ℃ under the stirring speed of 1000 rpm after the addition of 2 wt.% stabilizer. The extrinsic self-healing epoxy resin composites materials were successfully prepared by adding the microcapsule into epoxy resins. With the increase in the amount of microcapsules, the self-healing effect of cracks on the damaged membrane was gradually obvious. The composite exhibited good self-healing properties when addition amount reached 10 wt.%.