| 游奎一,曾珍,王良芥,刘平乐,吴剑,罗和安.D-72磺酸树脂催化环己酮肟液相贝克曼重排制己内酰胺[J].分子催化,2010,(4):0 |
| D-72磺酸树脂催化环己酮肟液相贝克曼重排制己内酰胺 |
| Liquid Phase Beckmann Rearrangement of Cyclohexanone Oxime into ε-Caprolactam Catalyzed by D-72 Sulfonic Acid Resin |
| 投稿时间：2010-05-14 修订日期：2010-07-12 |
| DOI： |
| 中文关键词: D-72磺酸树脂 二甲亚砜 液相贝克曼重排 环己酮肟 己内酰胺 |
| 英文关键词:D-72 sulfonic acid resin Dimethylsulfoxide Liquid phase Beckmann rearrangement Cyclohexanone oxime ε-Caprolactam |
| 基金项目:国家自然科学基金重点项目（20736009,20976148）；湖南省教育厅资助科研项目（09C955）；湘潭大学校级课题（08XZX14，08QDZ26） |
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| 中文摘要: |
| 在以二甲亚砜作溶剂，以D-72固体磺酸树脂为催化剂的两相体系中，实现了由环己酮肟液相贝克曼重排制备己内酰胺的反应。主要考察了环己酮肟在固体酸催化剂上的吸附热力学规律以及溶剂、反应温度、反应时间、催化剂用量以及催化剂的重复使用性等因素对重排反应的影响。结果表明，环己酮肟在磺酸树脂上的等温吸附过程符合Langmuir吸附模型，吸附等温线可用Langmuir等温方程和速率方程来描述。在二甲亚砜溶剂中，当反应温度在130 ℃，催化剂用量为0.5 g（催化剂:环己酮肟=1:2（质量比））的条件下反应6小时，环己酮肟的转化率高达100%，己内酰胺的选择性为86.2%，主要副产物为环己酮。该法对环境无害，反应条件温和，催化剂容易分离和可重复使用等优点。 |
| 英文摘要: |
| The liquid phase Beckmann rearrangement of cyclohexanone oxime into ε-caprolactam was successfully developed by using D-72 sulfonic acid resin as catalyst and dimethylsulfoxide as solvent in a two-phase system. The effects of solvent, reaction temperature, reaction time and amount of catalyst on the rearrangement of cyclohexanone oxime were examined. The results indicate that the adsorption behavior of cyclohexanone oxime on sulfonic acid resin accords with Langmuir adsorption model and can be described by Langmuir isotherm and speed equation. And the conversion of cyclohexanone oxime can reach 100% with 86.2% of selectivity to ε-caprolactam when the reaction was carried out at 130 ℃ for 6 h in dimethylsulfoxide solvent (m (catalyst): m (oxime) =1:2 (mass ratio)). This catalytic system involved is environmentally harmless, mild reaction conditions, and the catalyst can be conveniently recovered for recycled use. |
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