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文章编号： 1672-6987（2024）05-0022-10； DOI： 10.16351/j.1672-6987.2024.05.003
张健， 丁军委*， 张效磊(青岛科技大学 化工学院， 山东 青岛 266042)
摘要： 使用浸渍-还原法分别制备了3%Pd/C、3%Pt/C和3%Pt-Fe/C催化剂，通过ICP、TEM、XPS等方法对催化剂的金属含量、表面形态、电子状态进行了表征。将制备的催化剂用于以混合硝基氯苯氨解后产物邻、对硝基苯胺和间硝基氯苯为原料，催化加氢合成邻、对苯二胺和间氯苯胺反应。通过对比3种催化剂，得到3%Pt-Fe/C催化剂催化效果最好。以3%Pt-Fe/C为催化剂，考察了各因素对混合硝基氯苯氨解产物加氢反应的影响,确定了反应的最优条件:起始催化剂用量08%（以反应原料的质量分数计），m（甲醇）∶m（水）=50∶50为溶剂，温度85 ℃，压力2 MPa，搅拌转速600 r·min-1。在此条件下，反应物转化率为100%，邻、对苯二胺和间氯苯胺的总收率可以达到99%以上，催化剂可重复使用19次。对新鲜和失活的Pt-Fe/C催化剂进行BET、CO化学吸附、TEM等表征，发现失活后催化剂的比表面积大幅下降，判定催化剂孔道堵塞是导致催化剂失活的主要原因。
关键词： Pt-Fe/C； 苯二胺； 间氯苯胺； 催化加氢
中图分类号： Q 612.1文献标志码： A
引用格式： 张健， 丁军委， 张效磊. Fe改性Pt/C催化剂催化混合硝基氯苯氨解产物加氢的研究［J］. 青岛科技大学学报(自然科学版), 2024, 45（5）： 22-31.
ZHANG Jian, DING Junwei, ZHANG Xiaolei. Using Fe modified Pt/C catalyst on the catalyst hydrogenation of mixed nitrochlorobenzene ammonolysis products［J］. Journal of Qing-dao University of Science and Technology（Natural Science Edition), 2024， 45（5）： 22-31.
Using Fe Modified Pt/C Catalyst on the Catalyst Hydrogenation of
Mixed Nitrochlorobenzene Ammonolysis Products
ZHANG Jian, DING Junwei, ZHANG Xiaolei
(College of Chemical Engineering,Qingdao University of Science and Technology, Qingdao 266042, China)
Abstract: The 3%Pd/C, 3%Pt/C and 3%Pt-Fe/C catalysts were prepared by impregnation-reduction method. The metal content, surface morphology and electronic state of the catalysts were characterized by ICP, TEM and XPS. The prepared catalyst was used to catalyze the hydrogenation of o, p-nitroaniline and m-nitrochlorobenzene from the products of mixed nitrochlorobenzene ammoniolysis to synthesize o, p-phenylenediamine and m-chloroaniline. By comparing 3%Pd/C, 3%Pt/C and 3%Pt-Fe/C catalysts, the 3%Pt-Fe/C catalyst has the best catalytic effect. Using 3% Pt-Fe/C as catalyst, the influences of various factors on the hydrogenation of mixed nitrochlorobenzene aminolysates were investigated. The optimal reaction conditions were determined as follows: the initial catalyst amount was 08% (based on the mass fraction of reactive materials), m(methanol)∶m (water) =50∶50 is solvent, the temperature is 85 ℃, the pressure is 2 MPa, and the stirring speed is 600 r·min-1. Under these conditions, the reactant conversion rate is 100%, the yield of o, p-phenylenediamine and m-chloroaniline can reach more than 99%, and the catalyst can be reused for 19 times. The fresh and deactivated Pt-Fe/C catalysts were characterized by BET, CO chemisorption and TEM. It was found that the specific surface area of the catalyst decreased significantly after deactivation, and it was determined that the blockage of catalyst pore was the main cause of catalyst deactivation.
Key words: Pt-Fe/C; phenylenediamine; m-chloroaniline; catalytic hydrogenation
收稿日期： 2023-11-23
基金项目： 山东省重点研发计划项目（2019GSF109055）.
作者简介： 张健（1998—），男，硕士研究生.*通信联系人.
