【作者】 叶洪平；

【导师】 段正康；

【作者基本信息】 湘潭大学 ， 化学工程， 2004， 硕士

【摘要】 亚氨基二乙酸盐(IDA)是一种应用很广的有机中间体，特别在合成草甘膦上需求量极大，其生产方法也很多，其中，二乙醇胺(DEA)催化脱氢法生成亚氨基二乙酸成本低、污染小、收率高，是一种具有前景的方法。本课题围绕二乙醇胺催化脱氢生成亚氨基二乙酸盐所用的催化剂展开研究。通过查阅文献资料，分析了反应机理，认为二乙醇胺脱氢生成酸是由两步反应组成─醇脱氢生成醛与醛的歧化，催化剂的性能是影响反应转化率、选择性及反应速度的主要因素，确定了采用沉淀法制备Cu/ZrO2做催化剂。论文通过正交试验设计与单因素实验相结合，得出共沉淀法制备催化剂的最佳工艺条件：沉淀时锆铜原子比取2、沉淀pH值为12、锆盐浓度为0.3 mol/L、锆铜氢氧化物在500℃焙烧4h、锆铜氧化物在230℃用氢气与氮气混合气还原4h；同时论文在催化剂性能测试中，通过单因数实验得出催化脱氢反应的最佳工艺条件：反应温度取165℃，控制压力在1.6MPa，碱的质量百分比取30％；论文最后通过对制备的催化剂进行了BET、XRD、SEM表征,制备的催化剂是粒径大小为6～15μｍ不规则的块状颗粒,其比表面积达116.53m2/g，催化剂载体ZrO2为四方晶相。在二乙醇胺催化脱氢反应中，当催化剂用量为二乙醇胺的20%（质量百分比）时，初次反应2.1h就可使产物亚氨基二乙酸钠的收率达到96.6%，催化剂9次重复使用时产物的平均收率为87.8%。更多还原

【Abstract】 Iminodiacetic salt is a kind of organic intermediate with many applications, especially there is great demand in the preparation of glyphosate. At the same time there are many preparation methods. The method of dehydrogenation of diethanolamine by catalysis is litte pollution, low cost, high yield. it is a kind of method with great prospect.This paper is about the study of catalyst used in the dehydrogenation from diethanolamine to Iminodiacetic salt. After analyzing the reaction mechanism through literature, we think the reaction from diethanolamine to iminodiatic salt is composed of two steps—reaction from alcohol to aldehyde and the disproportionation reaction of the aldehyde. The selectivity, conversion, rate of this reaction are mainly attributed to the capability of this catalyst. we use co-precipitation method to prepare the Cu/ZrO2 catalyst; Through the orthogonal design experiment and pricipal component experiment，we get the best production condition of catalyst preparation: C（Zr）=0.3 mol/L, NZr/NCu=2, pH=2, calcination for 4h at 500℃, reduction for 4h at 230℃；In the test of the catalyst capability, through the pricipal component experiment. We get the best production condition of dehydrogenation reaction by catalysis: the temperature at 165℃, the pressure at 1.6MPa, 30％（quality percentage） sodium hydroxide solution; At last, we characterize the catalyst through BET ,XRD, SEM. we can know the catalyst is a kind of irregular and massive particles with 6～15μｍ particle diameter and 116.53 m2/g BET surface area, the carrier ZrO2 of this catalyst is nanocrystalline. In the dehydrogenation from <WP=5>diethanolamine to Iminodiacetic salt, when the quality of catalyst is 20%( quality percentage) of diethanolamine quality, the product yield can be up to 96.6% in 2.1 hours at first reaction, the average yield is 87.8% in 9 repeat reaction.更多还原