Study On Reductive Amination Process Of Alcohols

With the rapid development of petrochemical industry,the demand of amine products represented by EDA is increasing in the market,which has great potential for development.MEA hydro-amination process is the main process for the synthesis of EDA at present,It's a clean process.However,there is a common disadvantage that synthetic pressures above 15 MPa are required.In this context,we want to develop highly selective amination catalysts to make the reaction conditions milder,Adapt to the application of existing organic amine equipment.?1?The preparation of amination catalyst is one of the key points in this experiment.CaO/Al₂O₃ composite formed by chemical modification and crystal transformation was used as the carrier.CuO and NiO were as the active components of the amination catalyst,and the catalyst composition was optimized.?2?The optimum preparation conditions were determined by screening and formula optimization of nitrate impregnation method and ammonia complex impregnation method:use Ca?NO₃?₂ as a chemical modifier of?-Al₂O₃,immersing in a concentration of 4.0%Ca?NO₃?₂ aqueous solution at 60?for 4 h,dry at 120?for12 h,and calcination at 960?for 4 h;The carrier was immersed in a mixed solution of Ni?NO₃?₂ and Cu?NO₃?₂ at a mass ratio of 1:0.091 for 4 h at 60?,dry at 120?for 12 h,and calcined at 450?for 4 h.Determine the optimized formula as:The content of NiO,CuO and CaO in the catalyst is 19.12²0.66%,2.15².30%and2.0%respectively.?3?Optimization of ethyleneamine synthesis process conditions.After the catalyst is determined,the process conditions for the synthesis of EDA were optimized in a single-tube fixed-bed reactor,and the optimal reaction conditions were:n?MEA?:n?NH3?=1:8,T:220?,P:2.5 MPa,and the space velocity:0.10 h^-1.?4?Under the conditions of amination catalyst and optimal synthesis process,the conversion of MEA can reach 43.52%,the selectivity of EDA is up to 64.25%,and the total selectivity of EDA is stable at about 96%.Through the 1000 h stability test,it was found that the conversion rate and selectivity were both stable and the catalyst performance was reliable.