介孔NiO的制备及其胺化苯制苯胺  

Preparation of Mesoporous NiO and Its Amination of Benzene to Aniline

作　　者：林笑寒 田宝 郭明慧 刘靖婷 夏云生[1] LIN Xiaohan;TIAN Bao;GUO Minghui;LIU Jingting;XIA Yunsheng(College of Chemical and Materials Engineering,Bohai University,Jinzhou 121013,China)

机构地区：[1]渤海大学化学与材料工程学院,辽宁锦州121013

出　　处：《合成化学》2024年第9期821-827,共7页Chinese Journal of Synthetic Chemistry

基　　金：一步法制备Co基复合氧化物催化剂项目(0523HX17902)。

摘　　要：传统的苯胺合成方法步骤多,条件苛刻,污染环境。选用草酸和硝酸镍为原料,通过一步直接热分解固体混合物过程,制得高比表面积的蠕虫孔状NiO催化剂,采用XRD、TEM、SEM和N_(2)吸-脱附技术表征了催化剂的物化性质,考察了以介孔NiO为催化剂、过氧化氢为氧化剂、氨水为胺化剂胺化苯一步合成苯胺。结果表明:热分解温度及原料配比影响介孔NiO粒子的结构;等物质的量之比的草酸和硝酸镍在400℃分解制得的介孔NiO催化剂(N4),在实验条件下可获得的苯胺最高收率为0.1%(5 mL原料苯制得4.7 mg苯胺),这与催化剂的高比表面积、发达的孔道结构和晶化物种的分散性有关。尽管苯胺收率不高,但介孔NiO催化剂的制备方法简便且具有普适性,并在温和条件下一步合成了苯胺,为探索高效、绿色合成苯胺新方法提供参考。The traditional aniline synthesis method includes many steps,the synthesis condition is harsh,and the environment is polluted.In this paper,oxalic acid and nickel nitrate were used as raw materials to prepare worm pore NiO catalyst with high specific surface area by one-step direct thermal decomposition of solid mixture.The physicochemical properties of the catalyst were characterized by XRD,TEM,SEM and N_(2)absorption-desorption techniques.Aniline was synthesized by aminating benzene with mesoporous nickel oxide as catalyst,hydrogen peroxide as oxidant and ammonia water as aminating agent.The results show that the thermal decomposition temperature and the ratio of raw materials affect the structure of mesoporous NiO particles.On the mesoporous NiO catalyst(N4)prepared by the decomposition of oxalic acid and nickel nitrate at 400℃,the highest yield of aniline was 0.1%(4.7 mg aniline was obtained from 5 mL of raw benzene),which was related to the high specific surface area of the catalyst,the developed pore structure and the dispersivity of the crystalline species.Although the yield of aniline is not high,the preparation method of mesoporous NiO catalyst is simple and universal,and aniline is synthesized under mild conditions,which provides a reference for exploring a new method of efficient and green aniline synthesis.

关 键 词：介孔材料 NIO 胺化 苯 苯胺 

分 类 号：O643.32[理学—物理化学]