响应面法优化AlCl3催化合成2-叔戊基蒽
Optimization of Lewis acid catalyzed synthesis of 2-tert-amylanthracene using response surface methodology
王妍 1靳海波 1黎京潭 1杨索和 1何广湘 1马磊1
作者信息
- 1. 北京石油化工学院新材料与化工学院燃料清洁化及高效催化减排技术北京市重点实验室,北京 102617
- 折叠
摘要
2-叔戊基蒽的制备是蒽醌法合成双氧水的关键,因此提高2-叔戊基蒽的收率具有重要意义.采用三氯化铝催化蒽烷基化制备2-叔戊基蒽,并通过单因素试验法探究反应时间、反应温度、催化剂用量、反应物摩尔比、溶剂用量对烷基化反应的影响.然后,选择影响较大因素,采用Box-Behnken Design进行进一步优化.验证模型具有代表性,能反应实验真实情况后,在溶剂用量为300 mL,n(蒽)∶n(叔戊醇)=1∶1.2条件下,以反应时间、反应温度、催化剂用量为变量,以2-叔戊基蒽收率为响应值,建立回归方程.经响应面优化,确定的最优条件为反应时间1.46 h、反应温度-11.7℃、n(蒽)∶n(三氯化铝)=1∶2.1.在此条件下,2-叔戊基蒽收率可达80.28％.
Abstract
The preparation of 2-tert-amylanthracene is the key to the synthesis of hydrogen peroxide by anthraquinone method,so it is important to increase the yield of 2-tert-amylanthracene.The preparation of 2-tert-amylanthracene by anthracylation catalyzed by aluminum trichloride was studied.The effects of reaction time,reaction temperature,amount of catalyst,molar ratio of reactants and amount of solvent on the alkylation reaction were investigated by single factor experiment.Then,the factors with greater influence were selected and Box-Behnken Design was adopted for further optimization.The verified model was representative and could reflect the real situation of the experiment.Under the conditions of 300 mL solvent,n(AN)∶n(C5H11OH)=1∶1.2,the regression equation was established with reaction time,reaction temperature and catalyst amount as variables,and the yield of 2-tert-amylanthracene as response value.After response surface optimization,the optimal conditions were determined as reaction time 1.46 h,reaction temperature-11.7 ℃,n(AN)∶n(AlCl3)=1∶2.1.Under the conditions,the yield of 2-tert-amylanthracene was 80.28％.
关键词
烷基化/2-叔戊基蒽/三氯化铝/Lewis酸/响应面Key words
alkylation/2-tert-pentylanthracene/aluminum trichloride/Lewis acid/response surface引用本文复制引用
基金项目
国家自然科学基金资助项目(91634101)
出版年
2024
国家科技期刊平台
NSTL
万方数据