The Study On The Preparation Of Morpholine

With a fast development in fine chemicals, morpholine are mostly applied in many research fields as intermediate of many organic product, such as rubber assistant, medicine, pesticides and so onl. There are mainly two methods to synthesize morpholine, cyclodehydration of diethanol amine (DBA) with sulfuric acid and cyclocondensation of diethylene glycol(DEG) with NHs in the presence of catalyst. For there are some shortages for these two methods, a lower yield of morpholine with DEA , unstable performance and a lower activity of catalyst, so it has an important significance to perfect production technology, speed up the industrial program, reduce the production cost, meet the market demand.Firstly, with a single-factor experiment and the final yield of morpholine as the testing target, the appropriate reaction condition for preparation of morpholine by cyclodehydration of diethanol amine were: reaction temperature 200 C, n(diethanol amine)/n(sulfuric acid) 1:1.8, reaction time 90minutes, the morpholine yield reached 79.3%. The optium separation condition for separating morpholine from solution from its preparation were: when the ratio of m(addition of sodium hydroxide solution( 45%)) to m(reaction solution) is 1:1.5, themorpholine yield has a efficient result, the concentration of fraction is about 21.5%. Moreover, with a increasing addition of liquid sodium hydroxide, the content of morpholine in fraction has a efficient result, reaching 93.4% in 80%(the content of sodium hydroxide). Based on the experimental data, a method was put forward to deal with the relic solution.Secondly, with temperature of 180~200 C and pressure of 2~4MPa, the morpholine preparation by DEG were investigated which were carried out in a 1L high-pressure autoclave. The influence of composition of catalyst on reaction was mearsured with a uniform design method. By setting the yield of morpholine as target, the optimum composition of catalyst regressed by computer based on the experiment data were: 3.99%TiO2, 6.47%NiO, 24.80%ZnO, 29.09%CuO, 35.65%Al2O3, the yield of morpholine reached 18.5%.