A New Method to Synthesize Nucleating Agent of NA-11
ZHANG Bei~1,CHEN Guo-bin~1,SONG Jian~1,LI Xiao-jun~2(1.College of Pharmaceutical & Biotechnology,Tianjin University,Tianjin 300072,China;2.College of Chemical Engineering,Hebei University of Technology,Tianjin 300130,China)
(1.College of Pharmaceutical & Biotechnology,Tianjin University,Tianjin 300072,China;2.College of Chemical Engineering,Hebei University of Technology,Tianjin 300130,China
Abstract��
The optimum synthetic conditions of 2,2��-methylene-bis(2,4-di-tert-butylphenyl)phosphate sodium(NA-11)(��) was obtained in this paper.2,2��-methylene-bis(4,6-di-tert-butylphenol)(��) was prepared by condensation reaction of 2,4-di-tert-butylphenol(��) with formaldehyde in yield of 95.1% and in purity of 98.9%.Then �� reacted with POCl_3 in acetonitrile for 1 h,followed by hydrolysis for 0.5 h to give 2,2��-methylene-bis(4,6-di-tert-butylphenyl)phosphate(��) in yield of 90.2% and in purity of 94.8%.Finally,�� reacted with sodium hydroxide for 0.5 h in methanol/water to form 2,2��-methylene-bis(4,6-di-tert-butylphenyl)phosphate sodium(��) in yield of 99.5% and in purity of 99.9%.The overall yield was 84.6% based on 2,4-di-tert-butyl phenol.
ZHANG Bei~1,CHEN Guo-bin~1,SONG Jian~1,LI Xiao-jun~2.A New Method to Synthesize Nucleating Agent of NA-11[J]. Chemcial Industry and Engineering, 2007,24(4): 335-338
[1]
KAWAMOTO N,TOBITA E,URUSHIHARA T.Nucleating agent and crystalline polymer compositioncontaining the same:EP,1375582[P].2004-01-02.
[2]
MA Cheng-yin,YANG Chui-cun,CHEN Hong-mei,et al.Research advance on nucleating agents of PP[J].ModernPlastics Processing and Applications,2002,14(1):41-44.
[3]
MAI Kan-cheng,LI Zhang-jun.Crystallization behaviors andmechanical properties of polypropylene nucleated by variousnucleating agents[J].China Synthetic Resin and Plastics,1998,15(2):62-66.
[4]
CUI Hong-yue.The application of nucleating agent in PP[J].Manufacture and Application of Plastic,2001,23(2):43-46.
[5]
WANG Yi-zhong,YU Bing-sheng.Synthesis and applicationof polypropylene nucleating agent[J].China PlasticsIndustry,1999,27(5):29-31.
[6]
DIDIER J,MARTINE T.Preparation of amphiphilicpolyisobutylenes-b-polyethylene-amines by mannichreaction��.Study of Mannich reaction on model systems[J]..J of Polymer Sci,Part A:Polymer Chemistry.1993,31:1-
[7]
YURUGEN S.Preparation of pure cyclic diarylesterphophate:JP,63181493[P].1991-08-07.
[8]
TAJIMA K,TAKAHASHI M.Production of diarylphosphate metal salt:JP,61210090[P].1986-09-18.
[9]
SVARA J D.Process for the preparation of pure cyclicdiarylphosphoric acid esters:EP,0432505[P].1991-06-19.
[10]
TAKAHASHI M D.Nucleating agent:EP,1209190[P].2000-06-15.
2007, Vol. 24 
