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过程工程学报 ›› 2018, Vol. 18 ›› Issue (6): 1340-1346.DOI: 10.12034/j.issn.1009-606X.218104

• 材料工程 • 上一篇    

玻纤增强聚酰胺6/次磷酸钇复合材料的制备及其阻燃性能

唐 刚1,3,4*, 姜浩浩1 ,陈丽娟2, 张 浩1, 刘纯林1, 周子健1   

  1. 1. 安徽工业大学建筑工程学院,安徽 马鞍山 243032 2. 皖西学院材料与化工学院,安徽 六安 237012 3. 中国科学技术大学火灾科学国家重点实验室,安徽 合肥 230026 4. 博硕科技(江西)有限公司,江西 吉安 330000
  • 收稿日期:2018-01-03 修回日期:2018-07-31 出版日期:2018-12-22 发布日期:2018-12-19
  • 通讯作者: 唐刚 tanggang@ahut.edu.cn
  • 基金资助:
    国家自然科学基金资助项目;中国博士后科学基金;中国博士后科学基金;火灾科学国家重点实验室开放课题;皖西学院校青年基金项目

Preparation of glass fiber reinforced polyamide 6/yttrium hypophosphite composites and their flame retardant properties

Gang TANG1,3,4*, Haohao JIANG1, Lijuan CHEN2, Hao ZHANG1, Chunlin LIU1, Zijian ZHOU1   

  1. 1. School of Civil Engineering and Architecture, Anhui University of Technology, Ma?anshan, Anhui 243032, China 2. College of Materials and Chemical Engineering, West Anhui University, Lu?an, Anhui 237012, China 3. State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, Anhui 230026, China 4. ASAP Technology (Jiangxi) Co., Ltd., Ji?an, Jiangxi 330000, China
  • Received:2018-01-03 Revised:2018-07-31 Online:2018-12-22 Published:2018-12-19
  • Supported by:
    The National Natural Science Foundation of China

摘要: 以六水合氯化钇(YCl3?6H2O)和次磷酸钠(NaH2PO2)为原料,采用共沉淀法制备了一种新型稀土金属次磷酸盐—次磷酸钇(YHP),对其进行了表征;以YHP为阻燃剂,采用熔融共混法制备了系列玻纤增强聚酰胺6(GFPA)/次磷酸钇复合材料(GFPA/YHP),采用热重、极限氧指数(LOI)、UL-94垂直燃烧和微型量热测试研究了YHP添加量对复合材料热稳定性、阻燃性能及燃烧性能的影响. 结果表明,YHP已成功制备,其具有棒状结构,长度为20?100 ?m,宽度为5?20 ?m,热稳定性很高,降解温度T5%为410℃,最大热失重速率温度Tmax为412℃,750℃下热解的残炭率为90.8wt%. 加入YHP降低了GFPA/YHP复合材料的热分解温度,但提高了其成炭率和高温稳定性,YHP添加量为20wt%时,复合材料的热分解温度为373℃,最大热失重速率温度为414℃,700℃下热解的残炭率为50.42wt%;YHP可有效提高复合材料的阻燃性能,极限氧指数(LOI)达27.5vol%,垂直燃烧级别达UL-94 V-1级;YHP可有效降低复合材料燃烧过程的热释放速率峰值(PHRR)和总放热(THR)量,二者分别降至327 W/g和15.8 kJ/g,比GFPA分别下降了14.1%和25.4%,表明YHP有效降低了GFPA/YHP复合材料燃烧的火灾危险性.

关键词: 次磷酸钇, 聚酰胺6, 复合材料, 阻燃, 热稳定性

Abstract: A novel rare earth hypophosphite—yttrium hypophosphite (YHP) was synthesized by co-precipitation method using yttrium(III) chloride hexahydrate (YCl3?6H2O) and sodium hypophosphite (NaH2PO2) as raw materials, and it was characterized by XRD, FT-IR, SEM and TGA. Furthermore, YHP was used as flame retardant to prepare a series of glass fiber reinforced polyamide 6/yttrium hypophosphite composites (GFPA/YHP) by melting bending method. TG, limiting oxygen index (LOI) test, underwriters laboratories (UL) 94 (UL-94) testing and microscale combustion calorimetry (MCC) were used to investigate the effects of YHP loading on thermal stability, flame retardany and combustion properties of GFPA/YHP composites. The results showed that YHP was prepared, it presented rod-like structures with a size of 20?100 ?m in length and 5?20 ?m in width, and presented high thermal stability with degradation temperature (T5%) of 410℃, maximal mass loss rate temperature (Tmax) of 410℃ and char residue at 750℃ of 90.8wt%. The addition of YHP decreased T5% but increased char residue and thermal stability in high temperature of GFPA/YHP composites. When 20wt% YHP was loaded, GFPA/YHP20 presented T5% of 373℃ with Tmax of 414℃ and char residue at 700℃ of 50.42wt%. YHP could significantly enhance flame retardancy of the composites, GFPA/YHP20 (with 20wt% YHP) reached UL-94 V-1 rating with limiting oxygen index (LOI) of 27.5vol%. YHP could significantly decrease heat release rate (PHRR) and total heat release (THR) of GFPA/YHP composites in combustion process. PHRR and THR values of GFPA/YHP20 were decrease to 327 W/g and 15.8 kJ/g, which were reduced 14.1% and 25.1% compared with GFPA, indicating YHP could effectively reduce fire hazard of GFPA/YHP composites in combustion process.

Key words: yttrium hypophosphite, polyamide 6, composites, flame retardancy, thermal stability