铜锆复合金属氧化物催化还原对硝基苯甲醚

FACILE SYNTHESIS OF COPPER ZIRCONIUM COMPOSITE OXIDE AND ITS APPLICATION FOR THE CATALYTIC REDUCTION OF NITROBENZENE METHYL ETHER

以氯化铜、氯化锌、氯化钙、氯化铝、氧氯化锆为原料,氢氧化钠为沉淀剂,采用顺加共沉淀法合成CuZn-Ca-Al-ZrO_2复合氧化物催化剂。考察了不同焙烧温度、不同金属配比对催化剂合成的影响,并用XRD、SEM、O2-TPD、NH3-TPD等测试手段对试样进行了表征,确定了催化剂较佳合成条件。实验结果表明:在焙烧温度为450℃,金属氧化物CuO、ZnO、CaO的总质量比为20%,其中n(Cu)∶n(Zn)∶n(Ca)=2∶1∶1,Al_2O_3质量分数为10%条件下制备的催化剂性能最佳,在催化还原工艺中于110℃、0.6 MPa下反应4h,对氨基苯甲醚收率大于98%,选择性还原大于99%。

With copper chloride,zinc chloride,calcium chloride,aluminium chloride and oxygen zirconium chloride as raw material,sodium hydroxide as the precipitator,Cu-Zn-Ca-Al-ZrO_2 composite oxide catalysts were successfully prepared by a coprecipitation method.XRD、SEM O2-TPD and NH3-TPD techniques were performed to characterize the samples.The effect of calcination temperature and proportions of raw material on the morphology and reaction performance of the catalysts was systematically investigated and thus the optimatized synthesis condition was obtained.Results show that The content for metal oxide CuO,ZnO and CaO was set at 20% of the total catalyst weight,while n（Cu）∶n（Zn）∶n（Ca）was 2∶1∶1 and Al2 O3 content was 10%.The metal oxides composite catalyst was obtained after a heat treatment at 450 ℃in a muffle furnace.The calcination temperature is 450 ℃,total mass ratio of metal oxide ZnO,CuO and CaO is 20%,the n（Cu）∶n（Zn）∶n（Ca）= 2∶1∶1,under the condition of Al_2O_3 content was 10%prepared catalyst showed best performance,after 4 hof reaction at 0.6 MPa and 110℃,the final product of p-methoxyaniline was obtained with a yield higher than 98%,and the catalyst activity is stability,the selectivity of target product is more than 99%.