Synthesis Of N-Ethylethy-Lenediamine By Two-step Process With Acetic Acid And1,2-Ethylenediamine

As an important organic intermediates, N-ethylethylenediamine(NEED) is wildly used in pesticides, medicines, surface active agents. Itcan be used to produce antibiotics, such as piperacillin, cephalosporins pullhydrazone and cefoperazone. At present, the main synthesis method ofNEED containing aminoethyl sulfate method, haloalkane ammonolysismethod, ethanolamine method and acetic acid method. Due to harshreaction conditions of aminoethyl sulfate method, the problems ofenvironment pollution and separation of haloalkane ammonolysis method,and the problem of high temperature and low product Yield ofethanolamine method and acetic acid method, a convenient synthesis ofNEED should be studied.This thesis presented a new method of synthesis of NEED andinvestigated the performance of different catalysts for the hydrogenolysisof C-N. In this experiment, acetic acid and ethanediamine were cyclized to2-methylimidazoline with the catalyzed cyclization of CaO. NEED wassynthesized by catalytic hydrogenolysis of2-methylimidazoline overheterogeneous catalysts. The effects of sort and amount of catalyst, loading of catalyst, reactionsolvent, reaction temperature, reaction pressure, reaction time and the ratioof material to solvent for NEED were investigated. Catalyzed by5wt%Pt/C, a Yield of NEED up to57.99%was obtained from1g2-methylimidazoline,15mL THF and0.04g5wt%Pt/C at160℃and5MPa.The mechanism of the hydrogenolysis of C-N with Pt/C was discussed,and the mechanism of the preparation of2-methylimidazoline, NEED andmain by-products were also reviewed. acetic acid and ethylenediaminewere firstly acylated to be N, N’-Diacetylethylenediamine, then the latterwas cyclized to2-methylimidazoline with the catalyzed cyclization of CaO.2-methylimidazoline was catalyzed to2-methylimidazolidine in thepresence of Pt/C, NEED was produced by catalytic hydrogenolysis of2-methylimidazolidine.The stability of Pt/C catalyst and the crystal, electrons, specificcapacitance of fresh and used catalysts were characterized. The activity ofused catalyst was decreased, but the activity of catalyst resumed rapidlywhen washed with methanol and water until neutrality. BET, XRD andXPS characterization indicates that the productor interacted with thecatalyst in somen way.