碳纳米球基氮-磷-硫复合阻燃剂的合成及其对环氧树脂的阻燃性能  

Synthesis of Carbon Nanosphere-Based Nitrogen-Phosphorus-Sulfur Compound Flame Retardant and Flame Retardancy of CNSs-H-D Reinforced Epoxy Resin

作　　者：季亚明 杨雅茹 姚勇波 李佳倩 沈小军[1,2] 刘淑强 JI Yaming;YANG Yaru;YAO Yongbo;LI Jiaqian;SHEN Xiaojun;LIU Shuqiang(School of Materials and Textile Engineering,Jiaxing University,Jiaxing 314001,China;Zhejiang Key Laboratory of Yarn Material Forming and Composite Processing Technology,Jiaxing 314001,China;School of Textile Engineering,Taiyuan University of Technology,Jinzhong 030600,China)

机构地区：[1]嘉兴学院材料与纺织工程学院,嘉兴314001 [2]浙江省纱线材料成型与复合加工技术研究重点实验室,嘉兴314001 [3]太原理工大学纺织工程学院,晋中030600

出　　处：《材料研究学报》2021年第12期918-924,共7页Chinese Journal of Materials Research

基　　金：浙江省自然科学基金(LQ21E030008);全国大学生创新创业培训计划(CD851920510);嘉兴学院大学生研究与培训项目(CD8517203298);浙江省纱线材料成形与复合加工技术重点实验室开放项目(MTC2020-09)。

摘　　要：以碳纳米球(CNSs)为核、六氯环三磷腈(HCCP)和氨基二苯砜(DDS)为桥梁和接枝剂制备一种碳纳米球基氮-磷-硫复合阻燃剂(CNSs-H-D)并表征其形貌结构和热稳定性,研究了这种复合阻燃剂对环氧树脂(EP)的阻燃性能和机理。结果表明:合成的CNSs-H-D是直径为80 nm的球状颗粒,热稳定性优异;CNSs-H-D添加量(质量分数)为5%的CNSs-H-D/EP,其LOI从EP的20.0%提高到27.5%,阻燃等级为V-2级,热释放速率峰值和火灾危险性指数比EP分别降低16.8%和42.2%;CNSs-H-D可显著提高EP的热稳定性和成炭性,CNSs-H-D/EP的初始分解温度比EP高40℃,高温残炭量提高了144.7%。CNSs-H-D/EP具有典型的凝聚相阻燃机理,其炭层的致密性和连续性好,初始失重温度比纯EP的炭层高190℃,800℃的剩余质量高达94.5%。Carbon nanosphere based nitrogen-phosphorus-sulfur composite flame retardant(CNSs-H-D)was synthesized with the desired carbon nanospheres(CNSs)as core,hexachlorocyclotriphosphazene(HCCP)as bridge and amino diphenyl sulfone(DDS)as grafting agent.The morphology and thermal stability of CNSs-H-D were characterized.Afterwards,the composite of CNSs-H-D reinforced epoxy resin(EP)(CNSs-H-D/EP)was made and its flame retardancy and the relevant mechanism were investigated.Results show that the synthesized CNSs-H-D displayed a spherical morphology with a mean diameter of 80 nm and excellent thermal stability.Specifically,the LOI of CNSs-H-D/EP increased from 20.0%(of pure EP)to 27.5%(with addition of 5%(mass fraction)CNSs-H-D/EP),thus its flame retardance reached grade V-2 and its peak value of heat-release rate and fire-risk index reduced by 16.8%and42.2%,respectively.Moreover,CNSs-H-D could significantly improve the thermal stability and char formation of EP.The initial decomposition temperature and high-temperature char residue of CNSs-H-D/EP increased by 40℃and 144.7%respectively,in comparison with the pure EP.Furthermore,the initial weight loss temperature of CNSs-H-D/EP was 190℃higher than that of EP.With good compactness and continuity of char layer,the CNSs-H-D/EP exhibited a typical condensed phase flame-retardant mechanism,where the char residue was as high as 94.5%at 800℃.

关 键 词：复合材料 氮-磷-硫复合阻燃剂 碳纳米球 环氧树脂 阻燃 

分 类 号：TB332[一般工业技术—材料科学与工程]