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摘要
以三羟甲基硫化膦与亚磷酸三甲酯为原料,合成一种笼状有机磷阻燃剂4-硫代-2,6,7-三氧杂-1,4-二磷杂双环[2.2.2]辛烷 (SDPCP)。研究得出最佳工艺条件为:三羟甲基硫化膦与亚磷酸三甲酯的摩尔比为1,甲醇钠为催化剂,在氮气氛围下,缓缓升温至90℃保温反应7h,蒸馏出甲醇得到黏性油状粗产物,在0℃冰水洗涤得到产物,最终产物收率为96.1%。利用红外光谱、核磁氢谱、热重分析及极限氧指数等技术手段对该产物的结构及性能进行表征,并测试了产物的阻燃性能。结果表明:产物无论是单独应用于聚对苯二甲酸丁二醇酯 (PBT)中还是与三聚氰胺聚磷酸盐 (MPP)复配后应用于PBT中都有很好的阻燃效用。
Abstract
A cage like organic halogen free flame retardant was synthesized with three hydroxymethyl phosphine and trimethyl methacrylate as raw materials.The optimum conditions were:the molar ratio of three hydroxymethyl phosphine sulfide with trimethyl phosphite was 1,using sodium methoxide as catalyst,nitrogen atmosphere,slowly heating up to 90℃ for 7h reaction,distillation product of methanol were viscous crude oil,washed the obtained product at 0℃ in water,the final product yield was 96.1%.The structure and properties of the product were characterized by FT-IR,1H-NMR,thermogravimetric analysis and the limit oxygen index.Finally,the flame-retardant properties of the products were tested.The results showed that the products had good flame retardancy whether they were applied to PBT alone or combined with MPP in PBT.
关键词
三羟甲基硫化膦
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协效阻燃剂
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高含硫量
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亚磷酸三甲酯
Key words
three hydroxymethyl phosphine sulphide
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synergistic flame retardant
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high sulphur content
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trimethyl phosphite
阻燃剂三羟甲基硫化膦笼状亚磷酸酯的合成与应用[J].
化工新型材料, 2020, 48(2): 254-257 DOI:
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