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以对硝基苯胺与丁酮为原料,Cu-Cr-La/γ-Al2O3为催化剂,在高压釜中合成了N,N’-二仲丁基对苯二胺。考察了催化剂的选用、反应温度、反应时间、反应压力和反应物的配比对反应的影响。通过优化工艺,得到了合成N,N’-二仲丁基对苯二胺的适宜反应条件为:反应温度180℃、反应时间10 h、反应压力3.5 MPa、对硝基苯胺与丁酮的质量比为1∶4。此条件下得到的产品质量分数为97.0%,原料转化率达100%。催化剂循环套用3次,产品质量分数和原料转化率没有明显的下降。并在实验室小试的基础上,成功地进行了中试实验。
Using p-nitroaniline and methyl ethyl ketone as raw materials and Cu-Cr-La / γ-Al2O3 as catalyst, N, N’-di-sec-butyl-p-phenylenediamine was synthesized in an autoclave. The effects of catalyst selection, reaction temperature, reaction time, reaction pressure and reactant ratio on the reaction were investigated. The optimized reaction conditions were as follows: the reaction temperature was 180 ℃, the reaction time was 10 h, the reaction pressure was 3.5 MPa, the mass of p - nitroaniline and butanone The ratio is 1: 4. Under these conditions, the product mass fraction was 97.0% and the conversion rate of raw materials was 100%. Catalyst cycle applied three times, the product quality scores and the conversion rate of raw materials did not significantly decline. On the basis of the lab test, the pilot experiment was successfully carried out.