摘要
在间歇反应器中,对尿素醇解法合成碳酸二乙酯(DEC)的控制步骤——氨基甲酸乙酯(EC)与乙醇合成DEC的反应进行了研究。采用热分解法制备了一系列金属氧化物催化剂,对其催化EC与乙醇合成DEC的反应性能进行了评价。实验结果表明,氧化铅的催化活性最高。确定了氧化铅催化剂的适宜制备条件:以PbCO3为前体,在300℃下焙烧4h。活性评价结合X射线衍射分析结果表明,四方晶相PbO有利于EC与乙醇合成DEC。氧化铅催化剂催化合成DEC的优化反应条件为:n(乙醇):n(EC)=10、催化剂用量1%(占总物料量的质量分数)、反应温度180℃、反应时间7h。在此条件下,EC转化率为36.0%,DEC选择性为45.0%,DEC收率为16.2%。
Synthesis of diethyl carbonate （DEC） from ethyl carbamate （EC） and ethanol, which is the control step in alcoholysis of urea for preparation of DEC, was studied in a batch reactor. Several metal oxides were prepared by calcination as catalysts used in the reaction, among which PbO showed the best catalytic activity. PbCO3 was taken as starting material, calcined at 300 °C for 4 h. Activity evaluation and XRD analysis concluded that the obtained tetragonal PbO was favorable to DEC synthesis. Under optimal reaction conditions： reaction temperature 180 °C, reaction time 7 h, catalyst dosage 1% （mass fraction based on total mass of system） and n（ethanol） ： n（EC） 10, conversion of EC is 36.0%, selectivity to DEC is 45.0% and yield of DEC is 16.2%.
出处
《石油化工》
CAS
CSCD
北大核心
2009年第2期139-144,共6页
Petrochemical Technology
基金
国家自然科学基金资助项目(20576025)
河北省自然科学基金资助项目(B2007000010)
河北省科学技术研究与发展计划项目(07215602D)
