改性骨架镍催化加氢3,4-二甲基硝基苯制备3,4-二甲基苯胺  

Catalytic Hydrogenation of 3,4-Dimethylnitrobenzene to 3,4-Dimethylaniline over Modified Skeletal Nickel

作　　者：胡少伟[1] 荣泽明[1] 刘益材[1] 郑飞跃[1] 杜文强[1] 吕连海[1] 

机构地区：[1]大连理工大学化工学院精细化工国家重点实验室,辽宁大连116012

出　　处：《精细化工》2010年第2期170-173,共4页Fine Chemicals

基　　金：国家高技术研究发展计划(863计划)资助项目(2007AA03Z345)~~

摘　　要：采用骤冷法制备了改性骨架镍,将其应用于3,4-二甲基硝基苯的催化加氢制备3,4-二甲基苯胺。考察了各反应参数的影响,结果表明,以甲醇为溶剂,3,4-二甲基硝基苯初始浓度1.0mol/L,催化剂质量为3,4-二甲基硝基苯质量的7%,在60℃和0.5MPa的条件下反应40min,3,4-二甲基硝基苯的转化率和3,4-二甲基苯胺的选择性均达到100%。反应过程中底物浓度与时间趋于线性关系,该反应近似表现为零级反应。反应中未检测到羟胺组分,仅有少量的亚硝基化合物以中间体形式产生,并最终完全转化为目标产物3,4-二甲基苯胺。The rapid-quenching technique was introduced into the production of modified skeletal Ni optimized conditions [ m （ catalyst ） /m （substract） = 7% in methanol, initial concentration of the substrate = 1.0 mol/L,60℃ and 0. 5 MPa] ,both the conversion of 3,4-dimethylnitrobenzene and the selectivity of 3,4-dimethylaniline can be up to 100% in 40 minutes. During the reaction process, the relationship of the reactant concentration versus reaction time was linear, which suggested that it is a pseudo-zero reaction. Arylhydroxylamine, which usually exists in the hydrogenation of nitroarenes, was not found in this process. The nitroso compound was detected as the main intermediate which can completely convert to the target product.

关 键 词：催化加氢 改性骨架镍 3 4-二甲基硝基苯 3 4-二甲基苯胺 骤冷法 医药与日化原料 

分 类 号：TQ466.2[化学工程—制药化工]