响应面法优化深共晶溶剂催化制备己二酸二异辛酯
Optimization of deep eutectic solvent-catalyzed preparation of diisooctyl adipate by response surface methodology
徐世洁 1胡志泉 1沈国良 1郑荣荣 1温瑞阳 1刘岳雷1
作者信息
- 1. 沈阳工业大学石油化工学院,辽宁辽阳 111003
- 折叠
摘要
深共晶溶剂作为新一代绿色溶剂,因合成纯化工艺简单、原料成本低、可再生、生物相容性好等特点而受到科技界的广泛关注.以对甲苯磺酸-甜菜碱制备的深共晶溶剂作为反应溶剂兼催化剂,催化合成增塑剂己二酸二异辛酯(DOA),解决传统催化剂的循环使用问题.采用响应面法,选取醇酸物质的量比、催化剂物质的量比和反应温度三个因素,以酯化率为响应值,利用Box-Behnken设计分析了各因素及其交互作用对酯化率的影响,得到了多项式回归方程模型.结果表明,最佳试验条件为醇酸物质的量比为3.217、催化剂物质的量比为2.310和反应温度为117.7℃.在该条件下,合成DOA的酯化率可以达到88.21%,与模型预测值(92.112%)接近.表明响应面法优化了深共晶溶剂催化合成DOA的工艺参数,具有较高的准确性和有效性.此外,该深共晶溶剂在循环测试8次后,酯化率仍保持在80%左右.经傅里叶变换红外光谱仪和核磁共振氢谱仪进行结构表征分析确定产物为DOA.
Abstract
Deep eutectic solvents,as a new generation of green solvents,have attracted the attention of the scientific and tech-nological community because of their unique properties,such as simple synthesis and purification process,low cost of raw materials,renewable,and good biocompatibility.Deep eutectic solvents were prepared from p-toluenesulfonic acid-betaine,which were used as reaction solvents cum catalysts to catalyze the synthesis of diisooctyl adipate(DOA)plasticizers,solving the recycling problem of conventional catalysts.Using response surface methodology,three factors,namely,molar ratio of alkyd,molar ratio of catalyst and reaction temperature were selected,and the effects of the factors and their interactions on the esterification rate were analyzed by using Box-Behnken design with the esterification rate as the response value,and a polynomial regression equation model was obtained.The experimental results show that the optimal experimental conditions are alkyd molar ratio of 3.217,catalyst molar ratio of 2.310,and reaction temperature of 117.7℃.Under these conditions,the esterification rate of the synthesized DOA can reach 88.21%,which is close to the model prediction(92.112%).It is shown that the response surface methodology optimizes the process parameters for the catalytic synthesis of DOA by deep eutectic solvent with high accuracy and effectiveness.In addition,the esterifi-cation rate of this deep eutectic solvent remain at 80%after 8 times of cyclic testing.The product was identified as DOA through Fourier transform infrared spectroscopy and nuclear magnetic resonance hydrogen spectrometry.
关键词
深共晶溶剂/催化剂/酯类增塑剂/酯化/绿色合成/响应面法Key words
deep eutectic solvent/catalyst/ester plasticizer/esterification/green synthesis/response surface methodology引用本文复制引用
基金项目
国家自然科学基金(52103225)
辽宁省教育厅一般项目(LJKZ0163)
辽宁省教育厅重点项目(LZGD2020005)
出版年
2024
NETL
NSTL
万方数据