利用共沉淀法制备了四方晶系锌锰复合氧化物ZnMn_2O_4纳米催化剂,X射线粉末衍射(XRD)和透射电子显微镜(TEM)结果表明,所合成的催化剂为粒径均匀的纳米粒子,平均粒径在20～50 nm,具有较好的分散性,对乙酸正丁酯的合成有较高的催化活性. 确定了适宜的酯化反应条件,以焙烧温度为300 ℃制备的ZnMn_2O_4为催化剂,在催化剂用量为0.3%(以反应物总质量计)、n(酸):n(醇)=1.8:1、反应时间为4 h、酯化反应温度120 ℃的条件下,酯化率可达92.53%.
A zinc manganese oxide nano-catalyst was synthesized by a co-precipitation method. X-ray diffraction (XRD) and transmission electron microscopy ( TEM) results indicate that the sample can be indexed to tetragonal ZnMn_2O_4 and the particle size ranges from 20 to 50 nm. The obtained ZnMn_2O_4 nanoparticles were used as a catalyst for the esterification reaction between acetic acid and n-butanol. The experimental results show that ZnMn_2O_4 nanoparticles had a high catalytic activity on the synthesis of n-butyl acetate. The influential factors including catalyst calcination temperature, acid-to-alcohol molar ratio, dosage of the catalyst and reaction time on the yield of n-butyl acetate were also investigated, and the maximal esterification rate of up to 92.53% was achieved under the following conditions; catalyst calcination temperature =300 ℃, n( acid) :n( alcohol) =1.8:1, the dosage of the ZnMn_2 O_4 catalyst is 0. 3% (in total mass of reactants) , reaction time is 4 h and esterification reaction temperature is 120 ℃.
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