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以硝酸铋和氢氧化钠为原料、活性炭作载体,采用水热法合成了Bi2O3/C催化剂,并利用X-射线衍射(XRD)对其结构进行表征。XRD图谱分析表明,Bi2O3在催化剂中以δ形态存在。同时,利用该催化剂还原间硝基三氟甲苯制备间三氟甲基苯胺,考察不同负载量的催化剂、催化剂用量、投料比和温度等因素对还原间硝基三氟甲苯制备间三氟甲基苯胺反应产率的影响。实验结果表明,0.002 mol/4 g Bi2O3/C具有良好的催化活性。最佳反应条件为:25 m L乙醇回流,0.002 mol/4 g Bi2O3/C催化剂用量为0.3 g,80%的水合肼和间硝基三氟甲苯的物质的量比为2∶1。催化剂重复使用9次仍保持较高的催化活性,收率可达98%。XPS图谱表明,使用前后催化剂中的铋未流失,且铋的价态不发生改变。
Bi2O3 / C catalyst was synthesized by hydrothermal method using bismuth nitrate and sodium hydroxide as raw materials and activated carbon as support. The structure of the catalyst was characterized by XRD. XRD pattern analysis showed that Bi2O3 exists in the form of δ in the catalyst. At the same time, the use of the catalyst to reduce m - nitrobenzotrifluoride m - trifluoromethyl aniline, investigated the different loadings of catalyst, the amount of catalyst, feed ratio and temperature and other factors on the reduction of nitrobenzotrifluoride Preparation of m - trifluoromethyl Aniline reaction yield. The experimental results show that 0.002 mol / 4 g Bi2O3 / C has good catalytic activity. The optimal reaction conditions were as follows: 25 mL ethanol reflux, 0.002 mol / 4 g Bi2O3 / C catalyst was 0.3 g and 80% hydrazine hydrate and m-nitrobenzotrifluoride was 2:1. Reuse of the catalyst 9 times still maintain a high catalytic activity, the yield can reach 98%. The XPS pattern shows that the bismuth in the catalyst before and after use is not lost, and the valence of bismuth does not change.