Study On The Catalytic Synthesis Of N-ethylethylenediamine And Ultraviolet Light Absorber UV-P

N-ethylethylenediamine is an important organic chemical intermediate for antibiotics drugs industries,such as piperacillin,cefoperazone,and cefbuperazone.N-ethylethylenediamine has been synthesized by many methods.However,almost of these methods suffer from the drawbacks,such as long reaction steps,the low yields of the desired products,harsh reaction conditions and unfriendly to the environment.So it is vital significant to design an effective,green and industrialized synthesis method.A green and effective synthesis of N-ethylethylenediamine synthesis process was studied in this thesis,and ethanol and ethylene diamine as raw materials.A series of catalysts were prepared and employed in the N-ethylation of ethylenediamine with ethanol in a fixed-bed reactor.The satisfied results were obtained using Cu-Zn-La/Al2O3 as a catalyst.In addition,Cu-Zn-La/Si O2,Cu-Zn-La/Al2O3 and Cu-Zn-La/HZSM-5 were characterized by BET,H2-TPR,XRD,TEM and NH3-TPD to investigate the influence of supports on catalytic performance.It was found that both of the BET surface area and the acidity of support were key factors to the catalytic performance.Moreover,reaction parameters,including temperature,hydrogen pressure and the feed rate of the raw material were optimized and the optimal conditions were obtained as followed: ethylenediamine to ethanol 1:5(molar ratio),temperature 175 ?,pressure 3Mpa,the feed rate of the raw material 0.3m L/min.Under optimal conditions,73.26% conversion of ethylenediamine and 71.23% selectivity of N-ethylethylenediamine were presented.Finally,the lifetime of catalyst was evaluated and the reaction could continuously proceed over 200 h.UV-P(2-(2'-hydroxy-5'-methyl-phenyl)-2H-benzotriazole)is a representative product of the light stabilizers.It has many advantages,such as discoloration resistance,oil resistance,high absorption efficiency,low toxicity,good compatibility with polymer.In addition,it can also be used for the synthesis of novel light stabilizers.Therefore developing a clean synthesis process is of great research value.In this thesis,reductive cyclization 2-nitro-2'-hydroxy-5'-methyl azobenzene to 2-(2'-hydroxy-5'-methyl-phenyl)-2H-benzotriazole using catalytic hydrogenation in fixed-bed reactor was studied.A series of catalysts were prepared and investigated in a fixed-bed reactor.The satisfied results were obtained using Pd1/Al2O3 as a catalyst.The palladium elemental was reaction active site.Moreover,reaction parameters,including temperature,hydrogen pressure were optimized and the optimal conditions were obtained as followed: temperature 110?,pressure 3.5Mpa,the feed rate of the raw material 0.3ml/min.Under optimal conditions,99.56% conversion of 2-nitro-2'-hydroxy-5'-methyl azobenzene and 61.45% selectivity of UV-P were presented.