有机含硫双磷杂环己烷SDPROP的合成及应用

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。

Synthesis and Application of Organic Sulfur-Containing Bisphosphonium SDPROP

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.