| 无溶剂法加氢还原制备3,4-二氯苯胺 |
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| 引用本文： | 鄢冬茂,李付刚,闫士杰,李文骁. 无溶剂法加氢还原制备3,4-二氯苯胺[J]. 染料与染色, 2014, 0(2): 34-36 |
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| 作者姓名： | 鄢冬茂 李付刚 闫士杰 李文骁 |
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| 作者单位： | 沈阳化工研究院有限公司,沈阳110021 |
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| 基金项目： | 国家十二五科技支撑计划资助项目（No：2011BAE07B07） |
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| 摘 要： | 以新型Pt/C为催化剂,无溶剂法加氢还原3,4-二氯硝基苯制备3,4-二氯苯胺,反应温度100℃,氢气压力1.0 MPa。实验结果:3,4-二氯苯胺含量99.75%(GC),脱氯副反应0.1%,收率99%。建立了反应过程的液相色谱中控分析方法,对中间产物进行了LC-MS表征,发现了中间体3,4-二氯苯基羟胺浓度随反应温度的变化规律。
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| 关 键 词： | 催化加氢 Pt/C -二氯硝基苯 -二氯苯胺 |
Preparation of 3, 4-Dichloronitrobenzene by Solvent-free Catalytic Hydrogenation |
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| YAN Dong-mao,LI Fu-gang,YAN Shi-jie,LI Wen-xiao. Preparation of 3, 4-Dichloronitrobenzene by Solvent-free Catalytic Hydrogenation[J]. Ranliao yu Ranse, 2014, 0(2): 34-36 |
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| Authors: | YAN Dong-mao LI Fu-gang YAN Shi-jie LI Wen-xiao |
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| Affiliation: | (Shenyang Research Institute of Chemical Industry Co. , Ltd. , Shenyang 110021, Liaoning China) |
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| Abstract: | 3, 4-Diehloroaniline was synthesized from 3, 4-dichloronitrobenzene with a new Pt/C catalyst by Solvent-free hydrogenation. The reaction temperature was 100 ~C, and the hydrogen pressure was 1.0 MPa. The purity of the product was 99. 75% （GC）, the side reaction of deehlorination 〈0. 1%, the yield 〉 99%. The reaction process was researched by liquid chromatography; the structures of intermediate were characterized by LC - MS. The relation between 3, 4-dichlorophenylhydroxylamine concentration and the reaction temperature was disclosed. |
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| Keywords: | catalytic hydrogenation Pt/C 3, 4-dichloronitrobenzene 3, 4-dichloroaniline |
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