Tan Yi, Shao Zhu-Bao, Chen Xue-Fang, Long Jia-Wei, Chen Li, Wang Yu-Zhong
†Center for Degradable and Flame-Retardant Polymeric Materials, College of Chemistry, State Key Laboratory of Polymer Materials Engineering, National Engineering Laboratory of Eco-Friendly Polymeric Materials (Sichuan), Sichuan University, Chengdu 610064, China.
‡National Engineering Research Center of Electronic Circuits Base Material, Guangdong Shengyi Technology Limited Corporation, Dongguan 523039, China.
ACS Appl Mater Interfaces. 2015 Aug 19;7(32):17919-28. doi: 10.1021/acsami.5b04570. Epub 2015 Aug 6.
A novel multifunctional organic-inorganic hybrid was designed and prepared based on ammonium polyphosphate (APP) by cation exchange with diethylenetriamine (DETA), abbreviated as DETA-APP. Then DETA-APP was used as flame-retardant curing agent for epoxy resin (EP). Curing behavior, including the curing kinetic parameters, was investigated by differential scanning calorimetry (DSC) and X-ray photoelectron spectroscopy (XPS). The flame retardance and burning behavior of DETA-APP cured EP were also evaluated. The limiting oxygen index (LOI) value of DETA-APP/EP was enhanced to 30.5% with only 15 wt % of DETA-APP incorporated; and the UL-94 V-0 rating could be easily passed through with only 10 wt % of the hybrid. Compared with DETA/EP, the peak-heat release rate (PHRR), total heat release (THR), total smoke production (TSP), and peak-smoke production release (SPR) of DETA-APP/EP (15 wt % addition), obtained from cone calorimetry, were dropped by 68.3, 79.3, 79.0, and 30.0%, respectively, suggesting excellent flame-retardant and smoke suppression efficiency. The flame-retardant mechanism of DETA-APP/EP has been investigated comprehensively. The results of all the aforementioned studies distinctly confirmed that DETA-APP was an effective flame-retardant curing agent for EP.
基于聚磷酸铵（APP），通过与二乙烯三胺（DETA）进行阳离子交换，设计并制备了一种新型多功能有机-无机杂化物，简称为DETA-APP。然后将DETA-APP用作环氧树脂（EP）的阻燃固化剂。通过差示扫描量热法（DSC）和X射线光电子能谱（XPS）研究了固化行为，包括固化动力学参数。还评估了DETA-APP固化的EP的阻燃性和燃烧行为。仅加入15 wt%的DETA-APP，DETA-APP/EP的极限氧指数（LOI）值提高到30.5%；仅加入10 wt%的该杂化物就能轻松通过UL-94 V-0等级测试。与DETA/EP相比，锥形量热法测得的DETA-APP/EP（添加15 wt%）的热释放峰值速率（PHRR）、总热释放量（THR）、总产烟量（TSP）和产烟速率峰值（SPR）分别下降了68.3%、79.3%、79.0%和30.0%，表明其具有优异的阻燃和抑烟效率。对DETA-APP/EP的阻燃机理进行了全面研究。上述所有研究结果都明确证实DETA-APP是一种有效的EP阻燃固化剂。
