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The Synthesis Of Morpholine By Diethylene Glycol

Posted on:2006-01-28Degree:MasterType:Thesis
Country:ChinaCandidate:J D ZhengFull Text:PDF
GTID:2121360152494429Subject:Chemical processes
Abstract/Summary:PDF Full Text Request
With the development of petro-chemical industry, morpholine, as an important intermediate of fine chemicals, has been widely used for preparation of rubber, medicine, pesticide and so on. Due to increasing requirement for morpholine, it becomes one a kind of good-sale chemicals in present. By now, the main process to synthesize morpholine is based on the reaction of diethylene glycol (DEG) with ammonia (NH3) in the presence of catalysts. However the major problem of the synthesis process mentioned above is that catalysts prepared by different methods are of lower activities. So it is important to develop the methods and conditions to prepare high activities catalysts for preparation of morpholine.In this paper two aspects of catalysts preparation, components and their amounts in catalyst, were chosen to investigate by uniform design. Experiments were performed according to the design of limited component. Catalysts were prepared by the coprecipitation and sol-gel methods, and its calciation temperature was determined by (TG/DTA) analysis and X-rays diffractionanalysis. The reduction temperature was obtained by the experiment. The results showed that the optimum calciation temperature was about 400 ℃ and the optimum reduction temperature was about 300℃.Under the conditions of 210-240℃ and 2.0-3.0MPa, the preparation experiment of morpholine by DEG was carried out in an 0.5L autoclave in the presence of the catalysts prepared by two different methods respectively. The product was analyzed by gas chromatograpHy. The yield of morpholine was set as target function based on the experiment. The experimental data was regressed. The experiment results showed that coprecipitation method is better than the sol-gel method in preparing catalysts for synthesis of morpholine. The optimum prescription of catalyst was got as follows: 4.30%TiO2, 22.89%NiO, 17.06%ZnO, 13.89%CuO, 41.86%A12O3. The yield of morpholine can be reached 55.2% under this condition.Finally the optimum conditions of the reaction pressure and temperature were searched. The experiment results showed that the optimum temperature is 230~240℃ and pressure is 2.4-2.6 Mpa.
Keywords/Search Tags:morpholine, diethylene glycol, catalyst, coprecipitation method, sol-gel method
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