三种尿素衍生物的合成工艺研究

【作者】 刘鑫；

【导师】 茹淼焱； 朱维群；

【作者基本信息】 山东大学 ， 应用化学， 2010， 硕士

【摘要】 本文以尿素为主要原料,合成了三聚氰酸、铜酞菁和缩二脲。从反应物配比,反应温度,反应时间等方面研究了影响反应的因素和条件,并通过多种分析方法验证了产品纯度。1.利用尿素在微波反应条件下合成了三聚氰酸,通过观察使用不同微波功率,不同反应时间,以及反应物的配比变化,得到最佳反应条件：在微波反应条件下,尿素和助熔剂氯化铵以质量比36：1的配比混合,反应10min,精制后可得到工业标准的三聚氰酸,收率可达70%。进行了工业放大反应,得到与实验室小试相同的结果。2.在微波反应条件下合成了铜酞菁,得到的最佳反应条件为将尿素、苯酐、氯化亚铜以摩尔比15：5：1,钼酸铵的使用量为苯酐质量的4%,在微波反应条件下以高火(约700w)引发反应,后使用中火500W(约500w)反应5min,反应产率61.1%,产品纯度为90%。3.使用溶剂法合成缩二脲,考察了不同反应时间,温度以及溶剂使用量,得到最佳反应条件为尿素与乙二醇二丁醚以质量比1：1混合加热到145℃反应3.5h,可制得含量为64.1%缩二脲,产率为35.6%。根据尿素反应中放出大量氨的特点,提出了尿素反应与脱硫脱硝用氨的联产方法,在制备尿素衍生物的同时将放出的氨气经净化处理后直接用于脱硫脱硝。该工艺既可解决了液氨法在运输和储存上的危险问题,又可解决尿素制氨运行成本高的问题。更多还原

【Abstract】 In this paper,three reaction products of urea have been studied:Cyanuric acid、Phthalocyanine blue and biuret.Influnence factors and reaction conditions of the synthesi reaction have been studied from the molar ratio of reactants,reaction temperature and reaction time. By a series of analysis and detection methods,the purity of ptoducts has been verified.1、The reaction that urea was heated by microwave to prepare cyanuric acid was chosen to investigate the effect of the mass ratio of reactants, power of microwave and reaction time on itself, through which came into being the best reaction condition that the mixture of urea and ammonium chloridethe, with the mass ratio of the former to the latter of 36:1, was heated by high power microwave for ten minutes and then refined by boiling in acid solution, with the productive rate of 70%. Industrial amplification reaction carried out the same results with the laboratory small scale, there is the potential for industrial scale.2、The reaction that reactants was heated by microwave to prepare CuPc was chosen to investigate the effect of the mass ratio of reactants, power of microwave and reaction time on itself, through which came into being the best reaction condition that the mixture of urea, phthalic anhydride and CuCl, Ammonium molybdatewith the malor ratio of the former to the latter of 15:5:1.The weight of ammonium molybdate was 15% of phthalic anhydride. Reaction triggered by the high fire,and then heated by high power microwave for 5 minutes.The reaction yield can reach 61.1%,and the product purity 90%.3、The reaction that urea was heated by solven to prepare biuret. The optimum reaction conditions of the reaction:the weight ratio of urea and ethylene glycol dimethyl ether was 1:1,the reaction temperature is 145℃,the time is 3.5h.The yield was 35.6%, and the product purity 64.1%.A new method was proposed to prepare the derivative of urea and simultaneously generate ammonia according to the characteristics of evolution of considerable ammonia in the preparaing of urea derivatives. The reaction of urea derivatives can replace the existing method of preparation of ammonia by ammonia or urea. The technology has solved the risk problem in transportation and storage of liquid ammonia,and the problem of high running costs of the method of urea.更多还原