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中温快速固化粉末环氧胶粘剂的制备与表征

Preparation and characterization of fast-curing powder epoxy adhesive at middle temperature.

作者信息

Xu Jie, Yang Jiayao, Liu Xiaohuan, Wang Hengxu, Zhang Jingjie, Fu Shenyuan

机构信息

Zhejiang Provincial Collaborative Innovation Center for Bamboo Resources and High-efficiency Utilization, 666 Wusu Street, Hangzhou 311300, People's Republic of China.

School of Engineering, and Key Laboratory of Wood Science and Technology of Zhejiang Province, Zhejiang A&F University, 666 Wusu Street, Hangzhou 311300, People's Republic of China.

出版信息

R Soc Open Sci. 2018 Aug 15;5(8):180566. doi: 10.1098/rsos.180566. eCollection 2018 Aug.

Abstract

At present, the disadvantage of powder epoxy adhesive is the limited application area. In order to widen the application range of powder epoxy adhesive from heat-resistant substrates (such as metals) to heat-sensitive substrates (such as plastic products, cardboard and wood), it is necessary to decrease the curing temperature. In this article, a series of fast-curing powder epoxy adhesives were prepared by the melt blending method with bisphenol A epoxy resin (E-20), hexamethylenetetramine (HMTA) as a curing agent and 2-methylimidazole (2-MI) as an accelerant. The structure and properties of the E-20/HMTA/2-MI systems were characterized by Fourier transform infrared, thermogravimetric analysis, dynamic mechanical analyser and differential scanning calorimetry (DSC). 2-MI added into the E-20/HMTA systems can simultaneously enhance toughness, tensile strength, glass transition temperature () and thermal stability in comparison with the E-20/HMTA systems. The best mechanical properties were obtained at 100/8/0.6 weight ratio of the E-20/HMTA/2-MI systems. DSC experiments revealed that the exothermic peak of the E-20/HMTA/2-MI system was about 55°C lower than that of the E-20/HMTA system. The activation energy of the cure reaction was determined by both Kissinger's and Ozawa's methods at any heating rates. The activation energy and pre-exponential factor were about 100.3 kJ mol and 3.57 × 10 s, respectively. According to the KAS method, the curing time of the E-20/HMTA/2-MI systems was predicted by evaluating the relationship between temperature and curing time.

摘要

目前,粉末环氧胶粘剂的缺点是应用领域有限。为了将粉末环氧胶粘剂的应用范围从耐热基材(如金属)拓宽至热敏基材(如塑料制品、纸板和木材),有必要降低固化温度。在本文中,通过熔融共混法,以双酚A环氧树脂(E-20)、六亚甲基四胺(HMTA)作为固化剂以及2-甲基咪唑(2-MI)作为促进剂,制备了一系列快速固化粉末环氧胶粘剂。采用傅里叶变换红外光谱、热重分析、动态热机械分析仪和差示扫描量热法(DSC)对E-20/HMTA/2-MI体系的结构和性能进行了表征。与E-20/HMTA体系相比,向E-20/HMTA体系中添加2-MI可同时提高韧性、拉伸强度、玻璃化转变温度()和热稳定性。E-20/HMTA/2-MI体系在100/8/0.6重量比时获得了最佳机械性能。DSC实验表明,E-20/HMTA/2-MI体系的放热峰比E-20/HMTA体系的放热峰低约55°C。在任何加热速率下,均通过基辛格法和小泽法测定了固化反应的活化能。活化能和指前因子分别约为100.3 kJ/mol和3.57×10 s。根据KAS方法,通过评估温度与固化时间之间的关系,预测了E-20/HMTA/2-MI体系的固化时间。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/2c52/6124101/442470be70e3/rsos180566-g1.jpg

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