摘要
以三氯氧磷和三羟甲基氧化膦为原料,合成了一种新型高含磷量同环双膦阻燃剂,即1,4-二氧代-2,6,7-三氧杂-1,4-二磷杂双环[2.2.2]辛烷（DODPCP）,并通过红外光谱（FTIR）、核磁共振氢谱（1H-NMR）对产物的结构进行了表征分析。然后考察了反应温度、反应时间及物质量比等对产率的影响,结果表明,该阻燃剂最佳合成工艺条件如下：在氮气保护下,20℃将三羟甲基氧化膦与三氯氧磷按物质量比1：1加至反应瓶中,在25、45、80℃三个阶梯温度下分别反应2、2、4 h。产物DODPCP的产率达到95.8%,熔点为（211±2）℃,分解温度为（305±5）℃。差热分析结果表明,该合成产物具有良好的热稳定性。应用实验结果表明,当DODPCP在聚对苯二甲酸丁二醇酯（PBT）中的添加量为20%时,阻燃PBT试样的极限氧指数为29%,已达到难燃级别,且燃烧成炭无熔滴;将DODPCP与三聚氰胺聚磷酸盐（MPP）复配且添加量均为10%时,阻燃PBT试样的极限氧指数可达到28%,燃烧时成炭无熔滴,这说明DODPCP无论单独应用还是与MPP复配,均对PBT具有良好的阻燃效果。
A novel high phosphorus content bisphosphine homoannular flame retardant, 1,4-dioxo-2,6,7-trioxa-1,4-diphosphabicyclo[2.2.2]octane（DODPCP） was synthesized by trimethylolphosphine oxide and phosphorus oxychloride, and the structure of the product was characterized by FTIR and 1 H-NMR. The effects of reaction temperature, reaction time and molar ratio of reactants on the yield were investigated, and the optimum conditions for the synthesis of DODPCP were obtained as follows： under the protection of nitrogen, trimethylolpropane phosphine and phosphorus oxychloride were added to the reaction flask at a molar ratio of 1：1 under 20℃, and the reaction was controlled at 25, 45 and 80℃ respectively for 2, 2 and 4 h. The results indicate that, the yield, melting point and decomposition temperature of DODPCP can respectively reach 95.8%,（211±2）℃ and（305±5）℃, and the product shows good thermal stability. The experimental results show that when the content of DODPCP in PBT is 20%, the limit oxygen index can reach 29%, the material has good flame retardance. The limit oxygen index can reach 28% when adding 10% of DODPCP and melamine polyphosphate（MPP） with 1：1 ratio for PBT, no droplet is formed during combustion. Above all, the product has good flame retardancy both in PBT alone and in PBT after compounding with MPP.
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,Shzhou 215009,China)
出处
《塑料科技》
CAS
北大核心
2018年第10期117-121,共5页
Plastics Science and Technology
关键词
有机膦
高含磷量
协同效应
高效阻燃剂
Organic phosphine
High phosphorus content
Synergy
Efficient flame retardant
