磁性碳基固体酸微球催化剂的制备及其催化性能研究  

Preparation and catalysis of magnetic carbon-based solid acid micropheres

作　　者：王勋 曾丹林 丁枭 沈康文 裴阳 陈诗渊 王光辉 Wang Xun;Zeng Danlin;Ding Xiao;Shen Kangwen;Pei Yang;Chen Shiyuan;Wang Guanghui(School of Chemistry and Chemical Engineering,Hubei Key Laboratory of Coal Conversion and New Carbon Material,Wuhan University of Science and Technology,Wuhan 430081)

机构地区：[1]武汉科技大学化学与化工学院湖北省煤转化与新型炭材料重点实验室,武汉430081

出　　处：《化工新型材料》2018年第12期201-204,208,共5页New Chemical Materials

基　　金：国家自然科学基金(21473126);湖北省教育厅基金(B2014094);湖北省煤转化与新型碳材料重点实验室开放基金(WKDM201506)

摘　　要：采用水热法制备得到具有磁响应性能的碳基固体酸微球催化剂,采用扫描电镜、振动样品磁强计、X射线衍射仪、红外光谱仪、热重分析仪和Boehm滴定等手段对其进行表征,并探讨了催化剂制备条件对碳基固体酸微球催化剂催化性能的影响。结果表明:微球直径为1.1～1.3μm时,其饱和磁化强度为4.25emu/g,具有Fe_3O_4的特征衍射峰,且表面具有大量的酸性官能团;在磺化温度为120℃、磺化时间为8h、浓硫酸用量为15mL时,催化剂酸量达到2.84mmol/g。将催化剂应用于油酸与甲醇的酯化反应,当催化剂质量为油酸质量的7.5%,甲醇与油酸摩尔比为24∶1,酯化温度为90℃,酯化时间为3h时,酯化率达到89.43%。Magnetic carbon-based solid acid microphere catalysts were prepared by hydrothermal method and were characterized by scanning electron microscopy,vibrating sample magnetometer,X-ray diffraction,fourier transform infrared spectroscopy,thermogravimetric analysis and Boehm titration.The effect of preparation conditions on catalytic performance of micropheres was discussed.The results showed that the diameter and saturated magnetization of microspheres were 1.1 to 1.3μm and 4.25 emu/g,respectively.The characteristic diffraction peaks of ferric oxide can be observed and a large number of acid functional groups were present on the surface of micropheres.The maximum acid density was 2.84 mmol/g when the sulfonation temperature 90℃,the time 8 hand the amount of concentrated sulfuric acid 15 mL.The as-prepared catalyst was used to catalyze the esterification reaction of oleic acid and methanol.The results showed that when the mass of the magnetic solid acid catalyst was 7.5% of oleic acid,the molar ratio of methanol to oleic acid was 24∶1,the esterification temperature 90℃ and the esterification time 3 h,the esterification rate reached 89.43%.

关 键 词：磁响应性能 固体酸 微球 酯化 

分 类 号：O643.36[理学—物理化学]