[1]罗轩,史红丽,周浩,等.离子液体催化合成阻燃剂3-羟基苯膦酰丙酸[J].南京师大学报(自然科学版),2012,35(01):54-57.
　Luo Xuan,Shi Hongli,Zhou Hao,et al.Synthesis of Flame Retardants 3-(Hydroxyphenylphosphinyl) Propionic Acid Catalyzed by Ionic Liquid[J].Journal of Nanjing Normal University(Natural Science Edition),2012,35(01):54-57.
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离子液体催化合成阻燃剂3-羟基苯膦酰丙酸()
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《南京师大学报（自然科学版）》[ISSN:1001-4616/CN:32-1239/N]

卷:
第35卷
期数:
2012年01期
页码:
54-57
栏目:
化学
出版日期:
2012-03-20

文章信息/Info

Title:
Synthesis of Flame Retardants 3-(Hydroxyphenylphosphinyl) Propionic Acid Catalyzed by Ionic Liquid
作者:
罗轩;史红丽;周浩;张士磊;杨锦飞;职慧珍;
南京师范大学化学与材料科学学院，江苏南京210097
Author(s):
Luo Xuan; Shi Hongli; Zhou Hao; Zhang Shilei; Yang Jinfei; Zhi Huizhen
School of Chemistry and Materials Science,Nanjing Normal University,Nanjing 210097,China
关键词:
离子液体; 苯膦二氯; 羟基苯膦酰丙酸; 阻燃剂
Keywords:
ionic liquid; dichlorophenylphosphine; 3-( hydroxyphenylphosphinyl) propionic acid; flame retardants
分类号:
TQ314.248
摘要:
采用两步法合成3-羟基苯膦酰丙酸(CEPPA),即以三氯化磷与苯为原料,在离子液体三乙基苄基氯化铵氯化铝([BnEt3N]Cl-xAlCl3)催化下,合成苯膦二氯(DCPP),再用DCPP与丙烯酸合成3-羟基苯膦酰丙酸(CEPPA).确定第一步最佳反应条件为:n(三氯化磷)∶n(苯)∶n([BnEt3N]Cl-xAlCl3)=3∶1∶0.025,回流温度为72℃～76℃,反应时间为6 h,产率达81.1%;第二步通过改变反应物滴加顺序及调整反应温度,得到最佳反应条件为:n(丙烯酸)∶n(DCPP)=1.3
Abstract:
3-( hydroxyphenylphosphinyl) propionic acid ( CEPPA) was synthesized by a two-step procedure: Phenyl phosphonic dichloride ( DCPP) was first synthesized using phosphorus trichloride and benzene as raw materials，and triethyl benzyl ammonium chloride-aluminum chloride( ［BnEt3N］Cl － xAlCl3 ) as catalyst． The optimum conditions for the first step are as follows: n( PCl3 ) ∶ n( C6H6 ) ∶ n( ［BnEt3N］Cl － xAlCl3 ) = 3∶ 1∶ 0. 025，At the reflux stage，the reaction temperature was 72℃—76℃，the reaction time was 6 h，and the yield of DCPP was up to 81. 1%． The optimum conditions for the second step by changing the order of the reactants and adjusting the reaction temperature were as follows: n ( acrylic acid) ∶ n( DCPP) = 1. 30∶ 1. 00; the reaction temperature was 70℃ － 80℃ and the reaction time was 1. 5 h － 2 h at the dropping stage; then reacting at 90℃ for 1 h; at the hydrolysis reaction stage，the reaction temperature was 92℃ － 95℃，and the reaction time was 4 h，the yield of CEPPA was up to 91%． The problem of agglomeration was easy to be solved in this procedure．

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备注/Memo

备注/Memo:
基金项目:江苏省科技厅产学研前瞻性联合研究资助( BY2010105) ．
通讯联系人:职慧珍，讲师，研究方向: 绿色有机合成、阻燃剂． E-mail: zhihuizhen@163． com
更新日期/Last Update: 2013-03-11