季戊四醇磷酸酯协同聚磷酸铵对环氧树脂阻燃抑烟性能的研究  

Synergistic effect of 1-oxo-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane and ammonium polyphosphate on flame retardancy and smoke suppression of epoxy composites

作　　者：冀美宇 赵逸哲 张文超 郭晓燕 杨荣杰 JI Meiyu;ZHAO Yizhe;ZHANG Wenchao;GUO Xiaoyan;YANG Rongjie(National Engineering Technology Research Center of Flame Retardant Materials,School of Materials Science&Engineering,Beijing Institute of Technology,Beijing 100081,China)

机构地区：[1]北京理工大学材料学院,国家阻燃材料工程技术研究中心,北京100081

出　　处：《中国塑料》2024年第11期1-7,共7页China Plastics

基　　金：国家自然科学基金(52373067)。

摘　　要：制备了一系列含有不同含量季戊四醇磷酸酯(PEPA)和聚磷酸铵(APP)及相同含量蒙脱土(MMT)的阻燃环氧树脂(EP)样品。通过对EP样品进行UL94,极限氧指数和锥形量热测试,揭示了APP和PEPA的协效阻燃。烟密度测试进一步验证了APP和PEPA的协同抑烟效果。在不同的阻燃剂样品中筛选出了阻燃抑烟效果最好的配方。实验结果表明,在环氧树脂中添加15%(质量分数,下同)的APP/PEPA/MMT(质量比69/25/6),复合材料的极限氧指数可由纯EP的23%提高到31.5%,UL94测试达到V-0等级。同时,热释放速率峰值(p-HRR)和总烟释放量(TSR)分别降低了73.6%和70%。通过锥形量热仪测得的热释放速率(HRR)、p-HRR、TSR结果,揭示了PEPA、APP和复配阻燃剂产生的气相阻燃及凝聚相阻燃效果。为了深入探讨协同阻燃和抑烟效果的机理,采用热重分析仪(TG)、红外光谱仪(FTIR)、目视观察和扫描电子显微镜(SEM)对含有APP和PEPA阻燃剂EP复合材料的气相和凝聚相进行了表征。A series of epoxy composites with different loadings of 1-oxo-4-hydroxymethyl-2,6,7-trioxa-l-phosphabicyclo[2.2.2]octane(PEPA)and ammonium polyphosphate(APP)and a fixed loading of montmorillonite(MMT)were prepared to enhance their flame-retardancy.The synergistic effect of APP and PEPA on the flame-retardant properties of the epoxy composites was evaluated by vertical burning experiment,limiting oxygen index,and cone calorimetry.A smoke density test was also carried out to demonstrate the collaborative smoke suppression effect of APP and PEPA.The experimental results indicated that when 15 wt% of APP/PEPA/MMT at a mass ratio 69/25/6 was incorporated into epoxy resin,the resultant epoxy composite obtained an improvement in limiting oxygen index up to 31.5% and reached the UL94 V-0 rating in the vertical burning test.Moreover,its peak heat release rate(HRR)and total smoke release(TSR)decreased by 73.6% and 70%,respectively.Based on the HRR,peak HRR,and TSR results obtained from cone calorimetric measurements,PEPA,APP,and their compounds can generate good flame-retardant effectiveness in both gas phase and condensed phase.To understand the synergistic mechanisms about the flame-retardant and smoke suppression effects deeply,thermal gravimetric analysis coupled with Fourier-transform infrared spectroscopy,visual observation,and scanning electron microscopy were conducted to characterize the gas and condensed phases of epoxy composites containing APP and PEPA flame retardants.

关 键 词：环氧树脂 复合材料 阻燃剂 聚磷酸铵 季戊四醇磷酸酯 

分 类 号：TQ322.4[化学工程—合成树脂塑料工业]