| Aminophenol(MAP),an important chemical raw material and organic intermediates,widely used in chemical industry,pesticides,dyes,pharmaceuticals and many other fields.Now so many solutions are found for the map,including nitrobenzene sulfonated akkali fusion liquid ammonia solution,Resorcinol,mnitrophenol electrolysis,hydroxy aniline,benzene two amine,hydrolyzed by hydrochloric acid,but these techniques have many limitations,for example,outdated technology and serious pollution,high cost and low yield,high selectivity,equipment requirements.Therefore,this process has been systematically studied by using sulfuric acid hydrolysis of two.Reaction process,product distillation process and the heat integration of the whole system are mainly discussed.The main research contents and results are as follows:Through single factor and orthogonal experiments,from the reaction temperature,time,ratio of reactants,concentration of acid,the product selectivity factors determine the best condition of the reaction: reaction temperature 210?,the acid concentration control in 19%,acid ratio of 2.0,reaction time was 4h,under these conditions,mphenylenediamine conversion rate achieves 92.03%,yield of m-aminophenol was 40.94%,the selectivity reaches 58.76%.The by-product of resorcinol yield is 56.05%.The mass ratio between m-aminophenol and resorcinol as 1:1.And on the basis of the experimental data were reaction rate equation are derived,reaction temperature of the reaction rate equation was obtained,and the reaction process of the reactor for the preliminary design,reactor type,flow patterns,reaction residence time and reactor volume and other parameters were obtained.The resorcinol acid extraction and m-aminophenol neutral extraction were liquidliquid phase equilibrium study,balance method determination of the two groups of liquid liquid phase equilibrium data,analysis of the salt and tar on the extraction effect influence.And with the NRTL activity coefficient model and UNIQUAC activity coefficient model respectively to two groups of experimental phase equilibrium data were correlated.The model of the binary interaction parameter values were obtained,and calculated the the average relative error of and absolute average error of the regression values with the experimental value.The results show that the calculated values is agree well with the experimental values,which can meet the requirements of engineering design.The extraction process was simulated and optimized,and the optimal oil and water ratio and extraction series were obtained.Through the preparation of resorcinol and m-aminophenol extracted product distillation process by m-phenylenediamine hydrolysis with H2SO4,under the premise of satisfying the purity and yield of products and of the distillation column for design optimization,get the optimum plate number and feed position.Through the analysis of heat integration for whole system,combination curve of the system of cold and hot streams and cold and hot streams grand composite curve and the original for thermal network chart,and through the initial program of heat transformation and optimization,get the best for thermal network diagram and the best heat integration scheme,after optimized scheme than the initial scheme reduces the cold and hot utilities load Co 1505 kW,operating cost index to reduce the 17.6%,total annual cost index decreased by 15.9%,greatly saves the consumption of the process of the economy.In this paper,new technology of preparation of resorcinol and m-aminophenol in sulfuric acid hydrolysis were studied.The optimum process conditions on the reaction were optimized.Systematically Study on the phase equilibrium of the hydrolysis product of separation equilibrium method,simulation and optimization of the extraction and distillation process,and the optimization design of the heat integration scheme of the whole system.There is no domestic and foreign literature report,which provides reliable data support for the industrialization of this process. |
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