Chem. J. Chinese Universities ›› 2003, Vol. 24 ›› Issue (11): 2099.

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Synthesis and Characterization of Polystyrene-grafted Molybdenum (Ⅵ) Schiff Base Complex and Its Catalytic Activity in Epoxidation of Cyclohexene

ZHANG Ya-Dong, GAO Xiao-Lei, JIANG Deng-Gao, CHEN Xia, WANG Zi-Jian   

  1. College of Chemical Engineering, Zhengzhou University, Zhengzhou 450002, China
  • Received:2002-10-30 Online:2003-11-24 Published:2003-11-24

Abstract: Molybdenum(Ⅵ) Schiff base complex derived from salicylaldehyde and ethylenediamine grafted in polystyrene-divinyl benzene(PS) supporter, was synthesized and characterized by IRspectra.The macromolecule Schiff base acts as uninegative bidentate ligand and bonding occurs through the hydroxyl oxygen and nitrogen atoms.The Mo(Ⅵ) complex grafted in polystyrene as the catalyst has been used in epoxidation process of cyclohexene, and its catalytic activity and selectivity have also been investigated.The experimental results show that the complex possesses an excellent activity and selectivity for epoxidation of cyclohexene.The effects of many factors on the graft process of PSsupporter and synthesis of cyclohexene oxide have also been discussed.New analysis method of amount of Mo in the catalyst and gas chromatogram (GC) method of epoxycyclohexane analysis have been set up.The optimum reaction condition has been obtained by orthogonal experiment design, that is, according to n(t-BuOOH)=0.1 mol, n(C6H10)∶n(t-BuOOH)=3∶1, volume of solvent is about 5mL, reaction temperature 80 ℃, reaction time 60 min, and weight of molybdenum in the catalyst is 2.08×10-2g.Under this condition, based on amounts of t-BuOOH, the yield of epoxycyclohexane is more than 99.2%, purity of epoxycyclohexane is about 99.5% by GCanalysis.The catalyst after being used circularly for 5 times still possesses higher catalysis activity and selectivity, the yield of cyclohexene oxide approaches 99% under the above-mentioned reaction condition.

Key words: Molybdenum (Ⅵ) Schiff base complex, Cyclohexene, Epoxycyclohexane, Polystyrene

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