The Preparation And Characterization Of N,N'-Alkylbispyrrolidinone

At present,the aromatics extraction agent has been used in petroleum chemical industry and other fields of fine chemicals,including glycol,sulfolane,N-Methylpyrrolidone(NMP)widely used by domestic and international attention.However,the boiling point of the above extraction agent is similar to the dry point of gasoline and the boiling point of heavy aromatic hydrocarbon.In this paper,We synthesized N,N'-Alkylbispyrrolidinone,the boiling point of N,N'-Alkylbispyrrolidinone is higher than traditional aromatics extraction agent and the solubility of aromatic hydrocarbon is similar to traditional aromatics extraction agent?Firstly,N,N'-Ethylbispyrrolidinone ? N,N'-Propylbispyrrolidinone ? N,N'-Butylbispyrrolidinone and N,N'-Hexyllbispyrrolidinone were synthesised under the same condition.The yield of above product was 70.21%,64.59%,59.90%,56.01%.Secondly N,N'-Ethylbispyrrolidinonea and N,N'-Hexylbispyrrolidinone were synthesized systematically.The effects of reaction conditions on the synthesis reaction,such as molar ratio of 1,6-Diamine to 1,4-Butyrolactone,reaction time,reaction temperature and the Reaction pressure,were investigated and the optimal conditions were obtained.Under the optimized conditions with molar ratio of 1:2.2,reaction time of 3 h,reaction temperature of 200?,the yield of N,N'-Hexyllbispyrrolidinone reached 70.11%,esterification rate of Ethylenediamine reached 100%;Under the optimized conditions with molar ratio of 1:2.5,reaction time of 2 h,reaction temperature of 280?,the yield of N,N'-Hexyllbispyrrolidinone reached 76.22%,esterification rate of 1,6-Diaminohexane reached 100%.And then the products were analyzed by the characterization methods of GC?MS?HNMR?IR,etc.In this paper,HZSM-5 with silica alumina ratio of 25 the as the best catalyst was selected Then this paper applied catalyst prepared to the synthesis reaction of N,N'-Hexylbispyrrolidinone.Under the optimized conditions with molar ratio of 2.2:1,reaction time of 1-2 h,reaction temperature of 280?,the yield of N,N'-Hexyllbispyrrolidinone reached 75.65%.The N,N'-Alkylbispyrrolidinone was carried on the preliminary application test,then the phase diagram of Liquid-liquid equilibrium was draw.The N,N'-Alkylbispyrrolidinone has the high aromatic hydrocarbon selectivity by research.Finally,the synthesis reaction of N,N'-Propylbispyrrolidinone was applied to the fixed bed reactor and a preliminary inquiry was made for the industrial continuous production of N,N'-Propylbispyrrolidinone.