江汉大学学报(自然科学版) ›› 2015, Vol. 43 ›› Issue (1): 19-23.

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磷-氮协效型烷基次膦酸盐阻燃剂的合成及其在PBT中的应用

杜大江,曹芳利,陈 佳* ,刘继延   

  1. 江汉大学 光电化学材料与器件省部共建教育部重点实验室, 化学与环境工程学院,湖北 武汉 430056
  • 出版日期:2015-02-28 发布日期:2015-03-05
  • 通讯作者: 陈 佳
  • 作者简介:杜大江 (1991—) , 男, 研究方向: 二烷基次膦酸盐阻燃剂。
  • 基金资助:
    国家、 省级大学生创新训练计划项目 (201311072009) ; 武汉市科技攻关计划项目 (2013011001010479)

Synthesis of P-N Synergistic Alkyl Phosphinate Flame Retardants and Its Application on PBT

DU Dajiang,CAO Fangli, CHEN Jia* ,LIU Jiyan   

  1. Key Laboratory of Optoelectronic Chemical Materials and Devices of Ministry of Education,School of Chemistry and Environmental Engineering,Jianghan University,Wuhan 430056,Hubei,China
  • Online:2015-02-28 Published:2015-03-05

摘要: 以2-甲基-2, 5-二氧-1, 2-氧磷杂环戊烷 (OP) 为原料, 经酰胺化和成盐两步反应制备得到β- (N-苯基甲酰胺) 乙基甲基次膦酸铝 (Al (CEMP) ) 这种含特征官能团的烷基次膦酸盐阻燃剂。采用1 H-NMR、 FTIR以及XRD等技术表征了产物结构。作为阻燃剂应用于聚对苯二甲酸丁二醇酯 (pdy butylene terephthalate, PBT) 时, 添加20 wt%的Al (CEMP) 可使PBT的极限氧指数 (LOI) 由16. 6%提高至28. 4%, 垂直燃烧测试达到UL94 V-0级别; 此外, 微型量热测试证实Al (CEMP) 对PBT的热释放速率 (HRR) 抑制作用明显。

关键词: 烷基次膦酸盐, 阻燃剂, 磷-氮协效, PBT

Abstract: A kind of alkyl phosphinate flame retardant named aluminum β-(N-phenyl carboxamide) ethyl methylphosphinate(Al (CEMP) )which containing characteristic functional group was synthesizedthrough 2-methyl-2, 5-dioxo-1, 2-oxaphospholane (OP)by two-step reaction of amidation and salification. The structure of the product was characterized by 1 H-NMR、 FTIR and XRD. As the flame retardant being used in PBT,the limit oxygen index (LOI)of PBT with 20wt% Al (CEMP)improves from 16. 6% to 28. 4%,and the vertical burning test reaches UL94 V-0 rating. The test of microcalorimeter confirmed that Al (CEMP)has a strong inhibition effect on heat release rate (HRR)of PBT.

Key words: alkyl phosphinate, flame retardant, P-N synergist, PBT

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