新型无卤阻燃剂乙二胺双磷酸二苯酯的合成

摘要

报道了一种新型无卤双磷酸酯阻燃剂乙二胺双磷酸二苯酯(ENDP),其分子结构中含有膨胀型阻燃剂的酸源和气源,具有磷氮协效作用,阻燃效率高且兼具增塑功能.其合成采用氯化磷酸二苯酯(DPCP)和乙二胺为原料,以4-(N,N-二甲基)氨基吡啶(DMAP)为催化剂,以三乙胺为缚酸剂,并考察了溶剂、反应温度、反应时间和催化剂用量对ENDP产品收率的影响.得到的最佳反应条件为:以四氢呋喃(THF)为溶剂,反应温度45℃,反应时间8h,催化剂DMAP与DPCP的质量比为3％,反应收率可达88.0％.产品结构经红外图谱(FT-IR)、核磁氢谱(1H NMR)和质谱(MS)等进行了确证；热分析表明,产品具有很高的热稳定性,其初始热分解温度为265℃,最大热分解温度为365℃,并在450℃以上时仍有20％的质量残余.%A novel halogen-free flame retardant ethylenediamine bis ( diphenylphosphate ) ( ENDP) was synthesized, using diphenylchlorophosphate (DPCP) and ethylenediamine as the raw materials, 4-(/V,iV-dimethyl) aminopyridine as the catalyst and triethylamine as the acid-binding agent. The molecule of ENDP contains both acid source and gas source, which are the crucial components of the intumescent flame retardant (IFR). The synergistic effect of phosphor and nitrogen in ENDP imparts high efficiency to the flame retardant, and the existence of diphenylphosphate groups gives rise to the plastification. The effects of solvent, reaction temperature, reaction time, and catalyst dosage on the ENDP yield were investigated. The optimum reaction conditions are as follows-, tetrahydrofuran (THF) as the solvent, at 45 ℃ for 8 h, the mass ratio of DMAP to DPCP is around 3% , and the yield of ENDP can reach up to 88. 0%. The structure of ENDP was characterized by FT-IR, 1H NMR and MS. The thermal analysis of ENDP indicates that the product possesses high thermal stability. The onset decomposition temperature and maximum decomposition temperature are 265 ℃ and 365℃, respectively, and the char residue at 450 ℃ still remains 20%.