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１５ｈ，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 ethylenediaminetetramethylenetetra[di(2hydroxyl3chloropropyl)]phosphonate(FRS) was prepared by (1)treatment of ethylenediamine and H 3PO 3 with formaldehyde to give ethylenediaminetetramethylenephosphonic 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 washfastness could be enhanced.
出处
《精细化工》
EI
CAS
CSCD
北大核心
1998年第3期35-39,共5页
Fine Chemicals
关键词
阻燃剂
膦酸酯
乙二胺
四甲撑膦酸
织物
flame retardant
synthesis
ethylenediaminetetramethylenetetra[di(2hydroxyl3chloropropyl)phosphonate
ethylenediaminetetramethylenephosphonic acid
textile
