磁性二氧化钛的磺化改性及其催化合成乙酰丙酸酯性能  

Sulfonating modification of magnetic titanium dioxide nanotubes and their catalytic performance for synthesis of alkyl levulinates

作　　者：施菁欣 汪娅琴 涂烁 刘贤响[1] Shi jingxin;Wang Yaqin;Tu Shuo;Liu Xianxiang(College of Chemistry and Chemical Engineering,Hunan Normal University,Changsha 410081,Hunan,China;Shuda College,Hunan Normal University,Changsha 410012,Hunan,China)

机构地区：[1]湖南师范大学化学化工学院,湖南长沙410081 [2]湖南师范大学树达学院,湖南长沙410012

出　　处：《工业催化》2021年第10期55-58,共4页Industrial Catalysis

基　　金：国家级大学生创新创业训练计划项目(S202010542033);湖南省大学生创新创业训练计划项目(202012652004)。

摘　　要：采用水热法合成TiO_(2)纳米管(TNTs),FeCl_(2)·4H_(2)O和稀氨水为原料原位合成磁性钛纳米管(TNTs/Fe_(3)O_(4)),通过氯磺酸对其表面进行改性制备了一类新型的磁性钛纳米管磺酸催化剂(TNTs-SO_(3)H/Fe_(3)O_(4))。采用FT-IR和TG等对催化剂表面官能团及热稳定性能进行表征。研究该催化剂在乙酰丙酸与正丁醇酯化反应中的催化性能。结果表明,在n(乙酰丙酸)∶n(正丁醇)=1∶4、反应温度118℃、反应时间6 h和催化剂用量为乙酰丙酸质量的8%时,乙酰丙酸正丁酯收率达95.8%。该催化剂即使在使用5次后仍具有强酸性位和高稳定性,因此具有工业应用潜力。催化剂可通过外加磁场实现回收再利用。A sulfonated magnetic titania nanotubes(TNTs-SO_(3)H/Fe_(3)O_(4))was prepared by synthesis of titania nanotubes(TNTs)via hydrothermal method,followed by in-situ synthesis of magnetic titania nanotubes(TNTs/Fe_(3)O_(4))using FeCl_(2)·4H_(2)O and diluted ammonia as the raw material,and finally modification by solfonation.Surface functional groups and thermal stability of the catalyst were characterized by FT-IR and TG.Catalytic behaviors of the(TNTs-SO_(3)H/Fe_(3)O_(4))for esterification of levulinic acid with n-butanol were studied.n-Butyl levulinate yield of 94.6%was obtained under the following condition:n(levulinic acid)∶n(n-butyl alcohol)=1∶4,dosage of catalyst=8%(based on mass of levulinic acid),118℃for 6 h.TNTs-SO_(3)H/Fe_(3)O_(4) exhibited strong acid sites and high stability even after using for five times and is promising as a potential commercial catalyst.The catalyst can be recovered by external magnetic field.

关 键 词：精细化学工程 磁性钛纳米管 磺化改性 乙酰丙酸酯合成 

分 类 号：O643.32[理学—物理化学] TQ426.94[理学—化学]