首页|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

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

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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0。8%(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。
Using Fe Modified Pt/C Catalyst on the Catalyst Hydrogenation of Mixed Nitrochlorobenzene Ammonolysis Products
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 cata-lysts 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 re-action conditions were determined as follows:the initial catalyst amount was 0.8%(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.Un-der these conditions,the reactant conversion rate is 100%,the yield of o,p-phenylenedia-mine 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 chemi-sorption and TEM.It was found that the specific surface area of the catalyst decreased sig-nificantly after deactivation,and it was determined that the blockage of catalyst pore was the main cause of catalyst deactivation.

Pt-Fe/Cphenylenediaminem-chloroanilinecatalytic hydrogenation

张健、丁军委、张效磊

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青岛科技大学 化工学院,山东 青岛 266042

Pt-Fe/C 苯二胺 间氯苯胺 催化加氢

山东省重点研发计划项目

2019GSF109055

2024

青岛科技大学学报(自然科学版)
青岛科技大学

青岛科技大学学报(自然科学版)

CSTPCD
影响因子:0.297
ISSN:1672-6987
年,卷(期):2024.45(5)