Box-Behnken法优化[Bmmim]OH催化合成三羟甲基丙烷  

Optimization of synthesis of trimethylolpropane catalyzed by[Bmmim]OH by Box-Behnken method

作　　者：苏奇意 解田[1,2,3,4] 全宏冬 杨秀国 李鸿雁 SU Qiyi;XIE Tian;QUAN Hongdong;YANG Xiuguo;LI Hongyan(School of Chemistry and Chemical Engineering,Guizhou University,Guiyang 550025,China;Chifeng Ruiyang Chemical Co.,Ltd.,Chifeng,Inner Mongolia 024076,China;Key Laboratory of Polyol Chemical New Materials Enterprises of Inner Mongolia Autonomous Region,Chifeng,Inner Mongolia 024076,China;National Key Laboratory for Efficient and Comprehensive Utilization of Medium and Low Grade Phosphate Rock and Its Associated Resources,Guiyang 550016,China)

机构地区：[1]贵州大学化学与化工学院,贵阳550025 [2]赤峰瑞阳化工有限公司,内蒙古赤峰024076 [3]内蒙古自治区多元醇化工新材料企业重点实验室,内蒙古赤峰024076 [4]中低品位磷矿及其共伴生资源高效利用国家重点实验室,贵阳550016

出　　处：《化学工业与工程》2024年第6期26-33,共8页Chemical Industry and Engineering

基　　金：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)

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CH_(3)CH_(2)CH_(2)CHO物质的量之比、CH_(3)CH_(2)CH_(2)CHO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。[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 CH_(3)CH_(2)CH_(2)CHO,and CH_(3)CH_(2)CH_(2)CHO 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>CH_(3)CH_(2)CH_(2)CHO 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.

关 键 词：[Bmmim]OH 离子液体 三羟甲基丙烷 响应曲面分析 

分 类 号：TQ223.1[化学工程—有机化工]