Box-Behnken法优化[Bmmim]OH催化合成三羟甲基丙烷

摘要 [Bmmim]Br和KOH为原料在甲醇中反应24 h合成了离子液体[Bmmim]OH,并进行了纯化,产率为87.39%。将合成的碱性离子液体[Bmmim]OH作为催化剂,甲醛正丁醛作为反应底物,合成了三羟甲基丙烷。在单因素实验基础上,探究了Cannizzaro反应时间、HCHO与CH₃CH₂CH₂CHO物质的量之比、CH₃CH₂CH₂CHO投料速度对三羟甲基丙烷产物浓度的影响。采用Box-Behnken响应面法,以三羟甲基丙烷的产物浓度为响应值,建立数学模型,3者相互影响次序为:甲醛和正丁醛物质的量之比>投料速度>Cannizzaro反应时间。由此建立最适宜工艺条件为甲醛和正丁醛物质的量之比为3.074,Cannizzaro反应时间为37.21 min,投料速度为10.45 r·min^-1。实验值与预测值的偏差为2.65%,拟合度良好。

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	苏奇意
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	全宏冬
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关键词： [Bmmim]OH 离子液体三羟甲基丙烷响应曲面分析

Abstract： [Bmmim] OH was synthesized by reacting [Bmmim] Br and KOH in methanol for 24 h and purified with a yield of 87.39%. Trimethylolpropane was synthesized using the synthesized [Bmmim]OH as catalyst and formaldehyde and butanal as substrates. Based on the single factor experiments, the effects of Cannizzaro reaction time, molar ratio of HCHO to CH₃CH₂CH₂CHO, and CH₃CH₂CH₂CHO drop acceleration on the product concentration of trimethylolpropane were investigated. A Box-Behnken response surface method is used to establish a mathematical model by taking the product concentration of trimethylolpropane as the response value. The order of interaction among the three was: molar ratio of formaldehyde and butanal > CH₃CH₂CH₂CHO drop acceleration > Cannizzaro reaction time. The optimal process conditions were as follows: the molar ratio of formaldehyde to butanal was 3.074, the Cannizzaro reaction time was 37.21 min, and the drop acceleration was 10.45 r·min^-1. The deviation between the experimental value and the predicted value is 2.65%, indicating a good fit.

Keywords： [Bmmim]OH ionic liquid trimethylolpropane response surface method

Received 2023-03-15;

Fund:国家重点研发计划“固废资源化”重点专项(2018YFC1900206);贵州省科技计划项目(黔科合平台人才[2019]5409)。

Corresponding Authors: 解田,研究员,E-mail:627476227@qq.com。 Email: 627476227@qq.com

About author: 苏奇意(1997—),女,硕士研究生,现从事多元醇合成方面的研究。

引用本文:

苏奇意, 解田, 全宏冬, 杨秀国, 李鸿雁.Box-Behnken法优化[Bmmim]OH催化合成三羟甲基丙烷[J]. 化学工业与工程, 2024,41(6): 26-33

SU Qiyi, XIE Tian, QUAN Hongdong, YANG Xiuguo, LI Hongyan.Optimization of synthesis of trimethylolpropane catalyzed by [Bmmim]OH by Box-Behnken method[J]. Chemcial Industry and Engineering, 2024,41(6): 26-33

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