磺酸磁性石墨烯固体酸的制备、表征及初步应用研究  

Synthesis,Characterization and Application of Sulfonated Magnetic Graphene Solid Acid

作　　者：王小双[1] 将传真 王敦[1] 孙中亮[1] 

机构地区：[1]海南大学材料与化工学院化学工程与工艺系,海南海口570228

出　　处：《广州化工》2014年第21期79-82,共4页GuangZhou Chemical Industry

基　　金：海南大学青年基金项目(qnjj1164);海南自然科学基金项目(513142)

摘　　要：以氧化石墨烯,Co(NO3)2·6H2O和Fe(NO3)3·9H2O为离子源利用水热法一步制备磁性石墨烯(Co Fe2O4-h GO),用磺酸重氮盐将其重氮化制得磺酸磁性石墨烯固体酸,采用FT-IR、XRD、VSM和酸碱反滴定法测对其进行了表征。结果表明,链接石墨烯的Co Fe2O4为单相立方尖晶石结构,平均粒径为27 nm,饱和比磁化强度MS为29.7 A·m2/kg,其表面酸量为2.7 mmol/g。用乙酸与正己醇的酯化反应初步评估其催化性能:在90℃,乙酸与正丁醇摩尔比为1∶1,催化剂用量为3wt%,反应时间为4 h的条件下,乙酸转化率为59.1%。A novel sulfonated magnetic graphene solid acid catalyst was prepared by combining the magnetic graphene which was in-situ obtained by hydrothermal method using graphene oxide,Co（ NO3）2·6H2O and Fe（ NO3）3·9H2O as ingredients and sulfonic acid azide salt via diazonium reaction. The character of solid acid catalyst was determined by FT-IR,XRD,VMS and Base-Acid titration method. The results showed that the total acid value was2. 7 mmol / g,the Co Fe2O4 anchored to the graphene was the nanocrystal with cubic spinel structure,the size was 27 nm,and the saturation magnetization intensity（ Ms） was 29. 67 emu·g-1. The solid catalyst exhibited moderated activity for esterification of acetic acid,whose conversion reached 59. 1% at 90 ℃ for 4 h.

关 键 词：铁酸钴 磁性石墨烯 固体酸 酯化反应 

分 类 号：TQ139.2[化学工程—无机化工]