第 37 卷第 6 期Vol. 37 No. 6
2007 年 12 月Dec 2007

所属栏目:染料、颜料及涂料

改性骨架镍催化邻硝基氯苯加氢制备2,2-二氯氢化偶氮苯
王 欢,梅 华,姚虎卿 (南京工业大学 化学化工学院,江苏 南京210009)
摘 要:通过对骨架镍催化剂添加第三金属M(Mo,Ti,Cr)制备改性骨架镍催化剂,并采用间歇加压釜式反应器对改性骨架镍催化剂进行活性评价,考察了不同添加金属、反应压力、温度、碱量、催化剂循环套用次数等工艺条件对催化加氢法制备2,2'-二氯氢化偶氮苯的影响。实验得到优惠的反应条件为:使用Mo-Ni-Al改性骨架镍催化剂,反应温度350 K,反应压力0.8 MPa,30%的氢氧化钠溶液40 mL。邻氯硝基苯的转化率达99.5%,2,2'-二氯氢化偶氮苯的收率可达90.5%。同时催化剂循环套用5次后其催化活性基本保持不变。结果表明,改性骨架镍催化剂较之普通骨架镍催化剂的活性、选择性及稳定性都有明显的提高,具有良好的工业应用前景。
关键词:改性骨架镍;催化加氢;循环;2,2'-二氯氢化偶氮苯
中图分类号:O643  文献标识码:A  文章编号:1009-9212(2007)06- 0048-04
Catalytic Hydrogenation for o-Chloronitrobenzene(o-CNB) Preparation of 2,2'-Dichlorohydrazobenzene(DHB)with Modified Skeletal Ni Catalyst
WANG Huan,MEI Hua,YAO Hu-qing (College of Chemistry and Chemical Engineering,Nanjing University of Technology,Nanjing 210009,China)
Abstract:Modified skeletal Ni catalyst was prepared by the addition of the third metal (Mo,Ti,Cr) on normal Skeletal Ni catalyst. The catalyst performance for the hydrogenation was evaluated in an autoclave reactor. The different addition metal,temperature,pressure,the dosage of sodium hydroxide,catalyst recycle times were investigated in hydrogenation of o-CNB to DHB. Under the optimal reaction conditions of temperature 350 K,pressure 0.8 MPa,Mo-Ni-Al modified skeletal Ni catalyst and 40 mL 30% sodium hydroxide. The o-CNB conversion exceeded 99.5% and the selectivity for DHB exceeded 90.5%. The catalytic activity of the modified skeletal Ni catalyst keeps the same level after recycling five times. The activities,catalytic selectivity,catalytic stability of catalyst are appreciably increasing,suggesting that the modified skeletal Ni catalyst has good industrial prospect.
Key words:modified skeletal Ni;catalytic hydrogenation;recycle;2,2'-dichlorohydrazobenzene
基金项目:江苏省高技术研究重大项目(BG2006041)。
作者简介:王 欢(1983-),男,江苏吴江人,硕士研究生,从事催化分离研究。(E-mail:wanghuangiggs@163.com)
收稿日期:2007-09-30