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Synthesis of Tris(β-chloropropyl)Phosphate Ester Catalyzed by Lewis Acid Ionic Liqiuds(PDF)

《南京师大学报（自然科学版）》[ISSN:1001-4616/CN:32-1239/N]

Issue:
2013年02期
Page:
48-51
Research Field:
化学
Publishing date:

Info

Title:
Synthesis of Tris(β-chloropropyl)Phosphate Ester Catalyzed by Lewis Acid Ionic Liqiuds
Author(s):
Hu Yun; Xia Kedan; Zhang Peng; Yang Jinfei; Zhi Huizhen
School of Chemisty and Materials Science,Nanjing Normal University,Nanjing 210097,China
Keywords:
ionic liquids; flame retardant; tris(β-chloropropy1)phosphate; synthesis
PACS:
O622.2
DOI:
-
Abstract:
Tris(β-chloropropyl)phosphate(TCPP)was synthesized with phosphorus oxychloride and propylene epoxside as raw materials,using ionic liquids Et3NHCl-x[AlCl3] made by ourselves as catalyst for the reaction.It was shown that the proper reaction conditions were:the molar ratio of propylene epoxide to phosphorus oxychloride was 1:3.3,reaction temperature was 60 ℃～65 ℃.The mass of catalyst was 0.03% of phosphorus oxychloride,and dropwise time of propylene oxide was 3 h.The yield of the product TCPP reached 98.5%.This technology has several advantages,such as small amount of catalyst,high yield and low cost.

References:

[1] Yang Yebo,He Wensen,Jia Chengsheng.Efficient synthesis of phytosteryl esters using the Lewis acidic ionic liquid[J].J Mol Catal A:Chem,2012,357:39-43.
[2]Dotterl M,Alt H G.Catalytic coupling and cracking reactions of alkanes in Lewis acidic chloroaluminate ionic liquids enhanced by molecular oxygen[J].Catal Commun,2012,19:28-30.
[3]Chen Min,Li Di,Luo Ying,et al.Synthesis of 5-benzoylacenaphthene in the presence of Lewis acidic ionic liquids[J].J Ind Eng Chem,2011,17:14-17.
[4]Ahmed E,Groh M,Ruck M.Room-temperature synthesis of the highly polar cluster compound Sn[SnCl][W3Cl13][J].Eur J Inorg Chem,2010,33:5 294-5 297.
[5]Chen Min,Di L,Luo Y,et al.Synthesis of 5-benzoylacenaphthene in the presence of Lewis acidic ionic liquids[J].J Ind Eng Chem,2011,17:14-17.
[6]齐国鹏,姜峰,孙学文.Et3NHCl-AlCl3催化苯与1-十二烯烃烷基化反应机理的研究[J].中国科学:化学,2010,40(5):461-466.
[7]Gerardus J,Kemperman B,TerHorst D Van de Goor,et al.The synthesis of substituted benzo[c]chromen-6-ones by a suzuki coupling and lactonization sequence using Ionic liquids from laboratory scale to multi-kilogram synthesis[J].Eur J Org Chem,2006,14:3 169-3 174.
[8] Bui T L T,Korth W,Jess A.Influence of acidity of modified chloroaluminate based ionic liquid catalysts on alkylation of iso-butene with butene-2[J].Catal Commun,2012,25:1-7.
[9]Kemperman G J,Roeters T A,Hilberink P W.Cleavage of aromatic methyl ethers by chloroaluminate ionic liquid reagents[J].Eur J Org Chem,2003,9:1 681-1 686.
[10]沈琦,周乐群,仇国才.TCPP阻燃剂制备方法:中国,200610038132.9[P].2007-08-01.
[11]T.Weiβ,Ilvesheim(DE); R.Elbert,Gladbach(DE).Preparation of phosphorus-containing propoxylation products by using aluminium trichloride:US,7820845B2[P].2010-10-26.

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Last Update: 2013-06-30