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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.
In a two-phase system using dimethylsulfoxide as solvent and D-72 solid sulfonic acid resin as catalyst, the caprolactam reaction from cyclohexanone-oxime liquid-phase Beckmann rearrangement was achieved. The effects of cyclohexanone oxime The thermodynamics of adsorption on solid acid catalyst and the influence of solvent, reaction temperature, reaction time, amount of catalyst and reusability of catalyst on the rearrangement reaction were investigated.The results showed that isothermal adsorption of cyclohexanone oxime on sulfonic acid resin The process is in accordance with the Langmuir adsorption model, and the adsorption isotherm can be described by the Langmuir isotherm equation and the rate equation. When the reaction temperature is 130 ° C and the catalyst amount is 0.5 g (dimethylsulfoxide solvent: cyclohexanone oxime = 1: 2 (Mass ratio)) for 6 hours, the conversion rate of cyclohexanone oxime was as high as 100%, the selectivity of caprolactam was 86.2% and the main byproduct was cyclohexanone.The method was not harmful to the environment and the reaction conditions were mild, Catalyst easy to separate and reusable advantages.