将螺环磷酸二氯和对甲苯酚在碱性条件下以水为溶剂反应得到螺环磷酸对甲苯酚酯。用对甲苯酚钠在277nm处的吸光度变化跟踪反应进程,并考察了温度、水的用量、反应物的摩尔比对合成的影响。结果表明,反应温度在5℃以下,反应时间为11h,反...将螺环磷酸二氯和对甲苯酚在碱性条件下以水为溶剂反应得到螺环磷酸对甲苯酚酯。用对甲苯酚钠在277nm处的吸光度变化跟踪反应进程,并考察了温度、水的用量、反应物的摩尔比对合成的影响。结果表明,反应温度在5℃以下,反应时间为11h,反应物摩尔比为1∶2.2,水的用量100 m l为最佳条件,产率为86.36%。用IR和磷元素分析表征产品结构,使用TG分析产品的热稳定性。展开更多
5,5-Dibromomethyl-2-chloro-2-oxo-1,3,2-dioxaphosphorinane)(Ⅱ)was prepared by reaction of dibromoneopentyl glycol and phospous oxychloride in the presence of triethylamine.Then bis(5,5-dibromomethyl-1,3,2-dioxanephosp...5,5-Dibromomethyl-2-chloro-2-oxo-1,3,2-dioxaphosphorinane)(Ⅱ)was prepared by reaction of dibromoneopentyl glycol and phospous oxychloride in the presence of triethylamine.Then bis(5,5-dibromomethyl-1,3,2-dioxanephosphoryl)bisphenol A(Ⅲ)was synthesized by compound Ⅱ and bisphenol A.The overall yield was 78.8%.The structure of the novel flame retardant was confirmed by elementary analysis,IR,MS and 1H NMR spectroscopy.The termogravimetry showed that the novel flame retardant had high thermal stability and excellent char-forming ability.The beginning temperature of the compound Ⅲ decomposition was above 264.2 ℃,and the char yield was about 17.50% at 600 ℃.展开更多
文摘采用P2O5为磷酸化试剂,研究了异辛醇聚氧乙烯醚[C8H17(EO)4OH]磷酸酯的合成工艺,取得了优化工艺条件:P2O5分批加料,加料温度≤40℃,原料配比n[C8H17(EO)4OH]n∶(P2O5)为2.61∶,70℃,酯化时间4h,水解温度80℃,水解时间2h.该产品性能:220g/L强烧碱溶液中不会产生漂油现象,渗透时间为4 s.
文摘将螺环磷酸二氯和对甲苯酚在碱性条件下以水为溶剂反应得到螺环磷酸对甲苯酚酯。用对甲苯酚钠在277nm处的吸光度变化跟踪反应进程,并考察了温度、水的用量、反应物的摩尔比对合成的影响。结果表明,反应温度在5℃以下,反应时间为11h,反应物摩尔比为1∶2.2,水的用量100 m l为最佳条件,产率为86.36%。用IR和磷元素分析表征产品结构,使用TG分析产品的热稳定性。
文摘5,5-Dibromomethyl-2-chloro-2-oxo-1,3,2-dioxaphosphorinane)(Ⅱ)was prepared by reaction of dibromoneopentyl glycol and phospous oxychloride in the presence of triethylamine.Then bis(5,5-dibromomethyl-1,3,2-dioxanephosphoryl)bisphenol A(Ⅲ)was synthesized by compound Ⅱ and bisphenol A.The overall yield was 78.8%.The structure of the novel flame retardant was confirmed by elementary analysis,IR,MS and 1H NMR spectroscopy.The termogravimetry showed that the novel flame retardant had high thermal stability and excellent char-forming ability.The beginning temperature of the compound Ⅲ decomposition was above 264.2 ℃,and the char yield was about 17.50% at 600 ℃.
