h‑MoO_(3)/SiO_(2)催化合成季戊四醇异辛酸酯  

Synthesis of pentaerythritol tetra(2‑ethylthylhexoate)catalyzed by h‑MoO_(3)/SiO_(2)

作　　者：谭益凤 曹平[1] 马楷[2] 李金桐 王雨恒 TAN Yifeng;CAO Ping;MA Kai;LI Jingtong;WANG Yuheng(College of Chemistry and Chemical Engineering,Chongqing University of Technology,Chongqing 400054,China;Southwest Branch of Sinopec Lubricant Co.,Ltd.,Chongqing 400039,China)

机构地区：[1]重庆理工大学化学化工学院,重庆400054 [2]中国石化润滑油有限公司西南分公司,重庆400039

出　　处：《无机化学学报》2024年第11期2155-2162,共8页Chinese Journal of Inorganic Chemistry

基　　金：重庆市教育委员会基于新工科背景的绿色化学教育教学研究项目(No.203335)资助。

摘　　要：采用固相研磨法,制备了一系列h-MoO_(3)/SiO_(2)催化剂,这些催化剂用于季戊四醇(PER)和异辛酸(i-EHA)反应,合成季戊四醇异辛酸酯(POE),并采用X射线衍射(XRD)、傅里叶红外光谱(FTIR)、X射线光电子能谱(XPS)、N2吸附-脱附、扫描电镜(SEM)、透射电镜(TEM)对催化剂进行表征测试。结果表明,h-MoO_(3)负载量为15%的(200)晶面择优取向的h-MoO_(3)/SiO_(2)是合成POE的优良催化剂。适宜的反应工艺条件(ni-EHA/nPER=4.3,mh-MoO_(3)/SiO_(2)/mPER=0.003,T=220℃,t=4 h)下,酯化率可达90.83%,POE的选择性可达100%。A series of h-MoO_(3)/SiO_(2) catalysts for the synthesis of pentaerythritol tetra(2-ethylthylhexoate)(POE)from pentaerythritol(PER)and 2-ethylhexanoic acid(i-EHA)were prepared by solid-phase milling and characterized and tested by X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),X-ray photoelectron spectroscopy(XPS),N2 adsorption-desorption,scanning electron microscope(SEM)and transmission electron microscope(TEM).The results showed that(200)crystalline facet-selectively oriented h-MoO_(3)/SiO_(2) with h-MoO_(3) loading of 15%is an excellent catalyst for the synthesis of POE.Under the suitable reaction process conditions(ni-EHA/nPER=4.3,mh-MoO_(3)/SiO_(2)/mPER=0.003,T=220℃,t=4 h),the esterification rate was up to 90.83%and the selectivity of POE was up to 100%.

关 键 词：h-MoO_(3)/SiO_(2) 晶面择优取向 季戊四醇 异辛酸 季戊四醇异辛酸酯 

分 类 号：O623[理学—有机化学] O624[理学—化学]