有机含硫双磷杂环己烷SDPROP的合成及应用  

Synthesis and Application of Organic Sulfur-Containing Bisphosphonium SDPROP

作　　者：许梓轩 杨珂珂 王彦林 XU Zixuan;YANG keke;WANG Yanlin(School of Chemistry Biology and Material Engineering,Suzhou University of Science and Technology,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

出　　处：《塑料》2020年第1期77-80,共4页Plastics

摘　　要：以三羟甲基硫化膦和甲基膦酸二甲酯(DMMP)为原料,合成了一种有机含硫双磷杂环己烷阻燃剂,即1-硫代-1-羟甲基-3,5-二氧杂-4-氧代-4-甲基-1,4-二膦杂环己烷(SDPROP)。分析了不同摩尔比、反应温度以及反应时间对产率的影响,得出最佳反应条件。以甲醇为溶剂,甲醇钠为催化剂,在反应温度为95℃的条件下,反应6 h,摩尔比n(三羟甲基硫化膦)∶n(甲基膦酸二甲酯)=1∶1,SDPROP的产率为96.0%。通过红外光谱(FTIR)、核磁共振氢谱(1H-NMR)、热重-差热分析(TG-DTA)及极限氧指数测试(LOI)等对产物的结构及性能进行了表征。结果表明,产物具有良好的热稳定性,将其应用于不饱和聚酯树脂(UPR)和聚丙烯(PP),均具有较好的热稳定性和阻燃效应。An organic bisphosphacyclohexane flame retardant,1-thio-1-hydroxymethyl-3,5-dioxa-4-oxo-4-methyl-1,4-diphosphine(SDPROP)was synthesized from trimethylolsulfide phosphine and dimethyl methylphosphonate.Exploring the effect of the ratio of different substances,the reaction temperature and the reaction time on the yield were obtained as follows:Using methanol as solvent and sodium methoxide as catalyst,reacting at reaction temperature of 95℃for 6 h,molar ratio n(trisylmethylphosphine sulfide)∶n(dimethyl dimethyl phosphonate)=1∶1 and the product yield was 96.0%.The structure and flame retardance of the product were characterized by means of FTIR,1H-NMR,TG-DTA analysis and LOI test.The results showed that the product had good thermal stability,and its application to unsaturated polyester resin(UPR)and polypropylene(PP)showed good thermal stability and good flame retardant effect.

关 键 词：三羟甲基硫化膦 甲基膦酸二甲酯 有机含硫双磷杂环阻燃剂 阻燃剂 不饱和树脂 聚丙烯 

分 类 号：TQ314.248[化学工程—高聚物工业]