Nb_2O_5/坡缕石固体酸催化合成偏苯三酸三辛酯  

Catalyzed Synthesis of Trioctyl Trimellitate by Nb_2O_5/ Palygorskite Solid Acid

作　　者：孟小雷 孙士淇 刘婷[1] 杨发翠 常玥[1,2,3] 查飞[1] 

机构地区：[1]西北师范大学化学化工学院,甘肃兰州730070 [2]生态环境相关高分子材料教育部重点实验室,甘肃兰州730070 [3]甘肃省高分子材料重点实验室,甘肃兰州730070

出　　处：《精细化工》2016年第1期31-36,共6页Fine Chemicals

基　　金：国家自然科学基金项目(21161017)~~

摘　　要：利用离子交换法将Nb^(5+)引入坡缕石(Nb^(5+)/PG),经300℃培烧后得坡缕石负载Nb_2O_5的固体酸(300-Nb_2O_5/PG),运用X射线衍射、X射线光电子能谱、紫外漫反射、N_2吸附-脱附(BET)、ICP、NH_3-TPD对其结构、金属含量、酸强度进行表征。在催化合成偏苯三酸三辛酯(TOTM)中,当偏苯三酸酐与异辛醇的摩尔比为1∶4,300-Nb_2O_5/PG用量为酸酐质量的5%,210℃,反应5 h后,偏苯三酸三辛酯酯化率可达到95.3%,催化剂重复使用10次后,酯化率89.2%。Palygorskite was ion-exchanged with NbCl_5 and calcined at 300 ℃ to prepare solid acid of palygorskite supported Nb_2O_5（ 300-Nb_2O_5/ PG）. The structure of modified palygorskite,metal content and acidity strength were characterized by XRD,XPS,UV-Vis,N_2 adsorption / desorption,ICP and NH_3-TPD. The material was used in the esterification of trioctyl trimetabenzoate（ TOTM） as catalyst,and esterification yield of trioctyl trimetabenzoate was 95. 3% at 210 ℃ to reflux 5 h when catalyst amount was 5% of trimellitic anhydride（ mass fraction）,n（ trimellitic anhydride） ∶ n（ 2-ethyl hexanol） = 4 ∶ 1.The esterification yield was 89. 2% when the catalyst was reused 10 times.

关 键 词：坡缕石 NB2O5 负载 固体酸 偏苯三酸三辛酯 催化技术 

分 类 号：TQ426.8[化学工程] O643.36[理学—物理化学]