新型含氮次膦阻燃剂的合成与应用  

Synthesis and Application of a New Phosphinic Flame Retardant Containing Nitrogen

作　　者：陈靖 严生 王彦林 CHEN Jing;YAN Sheng;WANG Yanlin(College of Biological Chemistry and Materials Engineering, Suzhou University of Science and Technology, Suzhou, Jiangsu 215009, China;Engineering Center of Halogen-Free Flame Retardant Plastic of Jiangsu Province,Suzhou,Jiangsu 215009,China)

机构地区：[1]苏州科技大学化学生物与材料工程学院,江苏苏州215009 [2]江苏省无卤阻燃塑料工程中心,江苏苏州215009

出　　处：《塑料》2018年第2期65-67,83,共4页Plastics

基　　金：江苏省研究生科研创新计划项目(CXLX11_0973)

摘　　要：以四氯甘脲和亚磷酸三乙酯为原料合成了新型含氮次膦阻燃剂四(O,O-二乙基磷酰基)甘脲。讨论了反应温度、反应时间、原料摩尔比对产率的影响,得到了最佳工艺条件:以二氧六环作为溶剂,四氯甘脲和亚磷酸三乙酯的摩尔比为1:5,反应时间为6 h,反应温度为100℃。收率为95.4%。通过红外光谱(FTIR)、核磁共振氢谱(~1H-NMR)、热分析(TG/DTA)和极限氧指数(LOI)对产物的结构和性能进行了表征。结果表明,该化合物的分解温度为300℃,具有良好的热稳定性能。将其应用于聚对苯二甲酸丁二醇酯(PBT)中时,共混物具有优良的阻燃成炭性能,且与氰尿酸三聚氰胺(MCA)、三聚氰胺聚磷酸(MPP)和二乙基次膦酸铝(1240)复配用于PBT中均具有良好的协同阻燃效果。Flame retardant tetra（ O, O-diethyl phosphonyl）glycoluril was synthesized from tetrachloroglycoluril and triethyl phosphite. The effects of reaction temperature,reaction time, and molar ratio on the yield were discussed. The results showed that the yield of 95.4% could be obtained under the conditions of molar ratio of tetrachloroglycoluril and triethyl phosphite 1：5,dioxane as solvent,and at 100 ℃ for 6 h. The structure and properties of the product were characterized by means of FTIR,IH-NMR,TG-DTA analysis and LOI test. The results showed that the decomposition temperature of the compound was 300 ℃ ,which meaned that it had an excellent thermal stability, the results showed that the product presented a good effect on antiflaming when it was applied to polybutylecetere-phthalate （PBT）. Otherwise, when it was mixed with melamine cyanurate（MCA）, melamine-phosphate （MPP） , aluminum diethylphosphinate （ 1240 ） and was applied to PBT, higher synergistic flame-retardance efficiency was found.

关 键 词：四氯甘脲 亚磷酸三乙酯 阻燃剂 四(O O-二乙基磷酰基)甘脲 成炭 协同效应 

分 类 号：TQ314.248[化学工程—高聚物工业]