亲水性形状记忆环氧树脂制备及表面浸润性调控

doi:10.7503/cjcu20180174

高等学校化学学报 ›› 2018, Vol. 39 ›› Issue (8): 1823.doi: 10.7503/cjcu20180174

亲水性形状记忆环氧树脂制备及表面浸润性调控

钱艺豪¹, 张东杰¹, 成中军²(), 康红军¹, 刘宇艳¹()

1. 哈尔滨工业大学化工与化学学院, 新能源转换与储存关键材料技术工业和信息化部重点实验室,2. 基础与交叉科学研究院, 哈尔滨 150001

收稿日期:2018-03-06 出版日期:2018-08-10 发布日期:2018-08-10
作者简介:联系人简介: 成中军, 男, 博士, 副研究员, 主要从事表面浸润性研究. E-mail: chengzhongjun@iccas.ac.cn;刘宇艳, 女, 博士, 教授, 主要从事形状记忆聚合物研究. E-mail: liuyy@hit.edu.cn
基金资助:
国家自然科学基金(批准号: 51573035, 21674030)资助.

Preparation of Hydrophilic Epoxy Resin and Its Wettability Regulation^†

QIAN Yihao¹, ZHANG Dongjie¹, CHENG Zhongjun^2,^*(), KANG Hongjun¹, LIU Yuyan^1,^*()

1. Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage,Ministry of Industry and Information Technology, School of Chemistry and Chemical Engineering,2. Academy of Fundamental and Interdisciplinary Sciences, Harbin Institute of Technology, Harbin 150001, China

Received:2018-03-06 Online:2018-08-10 Published:2018-08-10
Contact: CHENG Zhongjun,LIU Yuyan E-mail:chengzhongjun@iccas.ac.cn;liuyy@hit.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(Nos.51573035, 21674030).

摘要/Abstract

摘要：

采用聚乙二醇(PEG)对间苯二甲胺(MXDA)固化的TDE-85环氧树脂体系进行改性, 制备了亲水性形状记忆环氧树脂, 结合微形貌构筑和热响应方式对树脂表面浸润性进行智能调控. 结果表明, PEG的引入有效地增加了TDE-85环氧树脂的亲水性. PEG的最佳含量为20%(质量分数)时, 树脂表面的接触角为54°, 实现了环氧树脂从原始TDE-85/MXDA固化体系表面的疏水性(接触角为108°)到TDE-85/MXDA/PEG固化体系表面亲水性的转变; 改性后树脂的玻璃化转变温度T_g为71 ℃, 形状固定率和回复率分别为96.10%和99.97%, 表明得到的树脂具有良好的形状记忆性能. 进一步采用模板法在树脂表面构筑了微阵列结构, 基于形状记忆效应, 通过对表面微阵列形态的控制, 实现了环氧树脂表面介于亲水性(接触角为51°)与超亲水性(接触角为0°)间的可逆浸润性智能调控.

关键词: 环氧树脂, 亲水性, 微形貌, 形状记忆, 浸润性调控, 聚乙二醇

Abstract:

A hydrophilic shape memory epoxy resin was prepared by introducing polyethylene glycol(PEG) into the 4,5-epoxy cyclohexane-1,2-2-phthalate glycidyl ester(TDE-85) epoxy/m-phenylenediamine(MXDA) system, meanwhile, its surface wettability could be controlled by changing its pillar structure under external thermal-stimuli. The result shows that the introduction of PEG effectively increases the hydrophilicity of TDE-85 epoxy resin, and the optimal amount of PEG is 20%(mass fraction). In this condition, the water contact angle is about 54 °, indicating the realization of wetting conversion from the original hydrophobic TDE-85 epoxy resin/MXDA curing system(water contact angle is about 108°) to the hydrophilic TDE-85/MXDA/PEG system. The T_g of the obtained material is 71 ℃, and its shape fixed ratio and recovery ratio are 96.10% and 99.97%, respectively, meaning that the obtained material has a good shape memory property. The micropillars onto the surface by the template method, reversible wetting switching between the hydrophilicity(51°) and the superhydrophilicity(0°) can be realized based on the shape memory ability.

Key words: Epoxy resin, Hydrophilicity, Microstructure, Shape memory, Reversible wetting control, Polyethylene glycol

中图分类号:

O631
O647

TrendMD:

钱艺豪, 张东杰, 成中军, 康红军, 刘宇艳. 亲水性形状记忆环氧树脂制备及表面浸润性调控. 高等学校化学学报, 2018, 39(8): 1823.

QIAN Yihao, ZHANG Dongjie, CHENG Zhongjun, KANG Hongjun, LIU Yuyan. Preparation of Hydrophilic Epoxy Resin and Its Wettability Regulation^†. Chem. J. Chinese Universities, 2018, 39(8): 1823.

图/表 8

Fig.1 Statistic of the water contact angles of TDE-85 epoxy resin modified by diffe-rent amount of PEGInsets are shapes of a water droplet on the related surface.

Fig.2 Infrared spectra of TDE-85 epoxy resins modified by different amount of PEGMass fraction of PEG(%): a. 0; b. 4; c. 8; d. 12; e. 16; f. 20; g. 24.

Fig.3 Variation of Tg with the increasing of PEG amount in the TDE-85/MXDA/PEG curing system

Table 1 Shape fixed rate and shape recovery rate of TDE-85/MXDA/PEG curing system

Mass fraction of PEG(%)	Shape fixed rate(%)	Shape recovery rate(%)
4	100	99.76
8	99.10	99.70
12	98.20	99.65
16	97.30	99.71
20	96.10	99.97
24	93.20	98.90

Fig.4 Static thermal mechanical analysis of TDE-85 epoxy system modified with 20% PEG

Fig.5 Surface microstructure variation of TDE-85 epoxy curing system with 20% PEG(A)―(C) are SEM images of the surface microstructure at original state, crushed state after pressing and restored state after heating, respectively. Inset in (A) is the magnified image of one pillar corresponding to (A). (D)―(F) are 3D confocal microscopy images of the surface microstructure at original state, crushed state after pressing and restored state after heating, respectively. (G)―(I) are the profile pictures corresponding to (D), (E) and (F), respectively.

Fig.6 Variation of pillar height after cycle pressing and heating processes

Fig.7 Shapes of a water droplet on the surface with different pillar structures(A) Upright pillars; (B) collapsed pillars; (C) and(D) schematic illustration of different water/solid contact models for surface with different pillar structures; (E) change of water contact angle after cyclic pressing and heating the surface.

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亲水性形状记忆环氧树脂制备及表面浸润性调控

Preparation of Hydrophilic Epoxy Resin and Its Wettability Regulation^†

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亲水性形状记忆环氧树脂制备及表面浸润性调控

Preparation of Hydrophilic Epoxy Resin and Its Wettability Regulation†

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Preparation of Hydrophilic Epoxy Resin and Its Wettability Regulation^†