新型阻燃剂乙二胺四甲撑四[双(2-羟基-3-氯丙基)]膦酸酯的合成及应用效果评价  

Synthesis of Ethylenediaminetetramethylenetetra[di(2hydroxyl3chloropropyl)]phosphonate and Evaluation of Its Performance on Fabric

作　　者：单玉华[1,2] 王旭 徐美英 钱三鸿[1,2] 毛翠霞 

机构地区：[1]江苏石油化工学院化工系 [2]常州市造漆厂质检处

出　　处：《精细化工》1998年第3期35-39,共5页Fine Chemicals

摘　　要：合成了新型阻燃剂乙二胺四甲撑四［双（２-羟基-３-氯丙基）］膦酸酯（ＦＲＳ）。合成中间产物乙二胺四甲撑膦酸（ＥＤＴＰ）的适宜条件是：甲醛∶亚磷酸∶乙二胺＝１．２∶０．６∶０．１６（摩尔比），反应体系初始ｐＨ＜１．５，室温滴加甲醛１５ｈ，回流反应２.５ｈ。ＥＤＴＰ收率为６８.８％。合成ＦＲＳ的适宜条件是：环氧氯丙烷∶ＥＤＴＰ＝１０∶１（摩尔比），反应体系初始ｐＨ＝４．０（用ＮＨ３调节），８０℃条件下２ｈ内滴加完环氧氯丙烷后继续反应１ｈ。ＦＲＳ的收率达９２.６％。ＦＲＳ对织物的阻燃能力超过四羟甲基氯化膦（ＴＨＰＣ），它与甲醚化三羟甲基三聚氰胺（ＴＭＭ）协同使用时其阻燃性能和耐洗性能都能得到提高。A new　type flame retardant ethylenediaminetetramethylenetetra[di(2hydroxyl3chloropropyl)]phosphonate(FRS) was prepared by (1)treatment of ethylenediamine and H 3PO 3 with formaldehyde to give ethylenediaminetetramethylenephosphonic acid (EDTP),and (2) treatment of EDTP with chloropropylene oxide to give FRS.Thus,formaldehyde(36%,1.2mol)was added dropwise over 1.5h to a solution of H 3PO 3 (0.6mol)and ethylenediamine (0.16mol)neutralized with HCl(36%,50ml)at room temperature,the mixture was refluxed for 2.5h to give 68.8% EDTP.Chloropropylene oxide (1mol)was added dropwise over 2h to a aqueous solution of EDTP(0.1mol) with initial pH=4.0(adjusted by NH 3)at 80℃ followed by 1h stirring to give 92.6%FRS.The application test on textile showed that the flame retardant presented had good fire retardancy.When it was used together with trihydroxymethylmelamine,its fire retardancy and washfastness could be enhanced.

关 键 词：阻燃剂 膦酸酯 乙二胺 四甲撑膦酸 织物 

分 类 号：TQ265.11[化学工程—有机化工] TS195.24[轻工技术与工程—纺织化学与染整工程]