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二乙醇胺催化脱氢合成亚氨基二乙酸的研究
Study on Catalytic Dehydrogenation of Diethanolamine for Iminodiacetic Acid
【作者】 温健麟;
【导师】 金杏妹;
【作者基本信息】 华东理工大学 , 工业催化, 2011, 硕士
【摘要】 本文对CuMnOx催化剂稳定性、CuFeOx催化剂制备条件及二乙醇胺脱氢工艺进行了研究。论文通过对CuMnOx催化剂的稳定性研究表明:采用分步沉淀法制备CuMnOx催化剂,经碱处理后具有更好二乙醇胺脱氢活性和碱性稳定性。CuFeOx催化剂的制备研究表明:采用共沉淀法制备CuFeOx催化剂,当Cu/Fe摩尔比为1,盐溶液浓度为0.4mol/L,沉淀pH值为10.0,沉淀温度为70℃,550℃下焙烧4h后,在210℃、60ml/min H2还原4h制得的CuFeOx催化剂;在反应温度150℃、压力0.7Mpa反应3h后,IDA收率可达91.1%;稳定性好,连续套用10次后,IDA的收率稳定在80%以上;TPR及XRD测试表明FeOx有助于表面活性Cu的分散,促进CuO的还原;通过适当引入Mn元素,有利于提高Cu/FeMn催化剂的二乙醇胺脱氢活性,当Cu:Fe:Mn=1:0.4:0.6时,IDA收率达94.8%。通过对二乙醇胺脱氢反应系统的分析,设计连续固定床脱氢反应器,并通过对反应过程分析,建立固定床脱氢反应工艺控制参数,在进料质量比为m(NaOH):m(DEA)=0.88,质量空速为2.0hr-1,反应温度为170℃,反应压力为0.8Mpa下连续反应60min, IDA收率达22.1%,设计固定床脱氢反应器及工艺参数可用于二乙醇胺连续脱氢反应。
【Abstract】 This thesis includes the Mn stability of CuMnOx catalyst,the preparation methods and preparation conditions of CuFeOx catalyst, and the process conditions of the catalytic dehydrogenation of diethanolamine.The different precipitation methods on preparing CuMnOx were compared, It is confirmed that the sequential precipitation method is better and when the CuMnOx catalyst pretreated by alkali will show more stability.The optimum preparation conditions of CuFeOx catalyst are that, molar ratio Cu/Fe of 1, the concentration of mix solution of 0.4mol/L,the pH of solution of 10, the temperature of precipitation of 70℃, the temperature of calcinations of 550℃, and the temperature of hydrogen reduction of 210℃,under the optimum process conditions for the catalytic dehydrogenation of diethanolamine:the reaction temperature of 150℃,the reaction pressure of 0.7Mpa, the reaction time of 3 hours, iminodiacetic acid(IDA) salt yield of 91.1% was obtained. During catalyst stabilization evaluation,it showed that over 80% of IDA yield,when Cu:Fe:Mn=l:0.4:0.6,the IDA yield can be upto 94.8%.Under the continuous Fix-bed process conditions for the catalytic dehydrogenation of diethanolamine:m(NaOH):m(DEA)=0.88, weight hourly weight velocity2.0hr-1, the reaction temperature of 170℃,the reaction pressure of 0.8Mpa,IDA yield of 22.1% was obtained,and it showed that the Fix-bed reactor and process can use for continuous catalytic dehydrogenating of diethanolamine.
【Key words】 diethanolamine; catalytic dehydrogenation; dehydrogenation catalyst; iminodiacetic acid salt; continous Fix-bed reactor;
- 【网络出版投稿人】 华东理工大学 【网络出版年期】2011年 07期
- 【分类号】TQ225.122
- 【下载频次】126