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| 用硝化与常压催化加氢法由三氟甲基苯制备间三氟甲基苯胺 | |
| 引用本文： | 王艳勇,杨东鹏,张鸿鹏,周黎明,龚小平. 用硝化与常压催化加氢法由三氟甲基苯制备间三氟甲基苯胺[J]. 精细石油化工, 2003, 0(1): 40-43 |
| 作者姓名： | 王艳勇 杨东鹏 张鸿鹏 周黎明 龚小平 |
| 作者单位： | 1. 中国人民解放军防化指挥工程学院化工所,北京,102205 2. 中国人民解放军防化指挥工程学院12教,北京,102205 3. 中国人民解放军防化指挥工程学院分析中心,北京,102205 |
| 摘 要： | 以三氟甲基苯为起始原料 ,经硝化和常压催化加氢制备间三氟甲基苯胺 ,总收率达 89% ,纯度 99%以上。硝化反应的优化条件为 :n(PhCF3 )∶n(HNO3 )∶n(H2 SO4) =1∶1.0 5∶1.3,间三氟甲基硝基苯收率 90 .7% ,纯度 98.0 % ;最佳氢化条件 :催化剂用量 2 % ,原料配比为 0 .10mol间三氟甲基硝基苯 / 10 0mL无水乙醇 ,氢化温度 4 5℃ ,搅拌速度 2 4 0r/min ,间三氟甲基苯胺收率 98.5 % ,纯度 99.3%。 |
| 关 键 词： | 三氟甲基苯 硝化 催化加氢 间三氟甲基苯胺 |
| 修稿时间： | 2002-03-24 |
PREPARAION OF m-TRIFLUOROMETHYLANILINE FROM BENZOTRIFLUORIDE BY NITRATION AND NORMAL PRESSURE CATALYTIC HYDROGENATION |
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| Wang Yanyong ,Yang Dongpeng ,Zhang Hongpeng ,Zhou Liming and Gong Xiaoping l. PREPARAION OF m-TRIFLUOROMETHYLANILINE FROM BENZOTRIFLUORIDE BY NITRATION AND NORMAL PRESSURE CATALYTIC HYDROGENATION[J]. Speciality Petrochemicals, 2003, 0(1): 40-43 | |
| Authors: | Wang Yanyong Yang Dongpeng Zhang Hongpeng Zhou Liming Gong Xiaoping l |
| Affiliation: | Wang Yanyong 1,Yang Dongpeng 2,Zhang Hongpeng 2,Zhou Liming 3 and Gong Xiaoping l |
| Abstract: | m -Trifluoromethylaniline was prepared from benzotrifluoride (phCF_3) by nitration and normal pressure catalytic hydrogenation. The purity was above 99% and the total yield reached to 89%. The optimum ratio of nitrating agent is PhCF_3∶HNO_3∶H_2SO_4=1∶1.05∶1.3(mol), the purity and yield of m -trifluoromethyl nitrobenzene were 98.0% and 90.7% respectively. The optimum conditions of catalytic hydrogenation are as follows: weight of 5% Pd/C catalyst used in the substrate=2%, trifluoromethyl nitrobenzene∶absolute ethanol=0.10 mol∶100 mL, reaction temperature 45 ℃, stirring speed 240 r/min, the purity and the yield of m -trifluoromethylaniline were 99.3% and 98.5% respectively. |
| Keywords: | benzotrifluoride nitration catalytic hydrogenation m -trifluoromethylaniline |
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