一步炭化磺化法制备煤基固体酸催化剂及其表征  

Preparation of coal based solid acid catalyst by one-step carbonization sulfonation and its characterization

作　　者：王雪 王克冰[1] 钟源 刘玉玲 WANG Xue;WANG Kebing;ZHONG Yuan;LIU Yuling(College of Science,Inner Mongolia Agricultural University,Hohhot 010018,China)

机构地区：[1]内蒙古农业大学理学院,呼和浩特010018

出　　处：《中国油脂》2022年第6期100-104,共5页China Oils and Fats

基　　金：内蒙古自治区研究生科研创新资助项目(DC2000002108)。

摘　　要：以胜利褐煤为原料,通过浓硫酸一步炭化磺化法制备煤基固体酸催化剂,以油酸和甲醇的酯化反应评价催化剂的催化活性。采用单因素实验考察了固液比、磺化温度、磺化时间对催化活性的影响。采用红外光谱、元素分析、BET、SEM、XRD、热重分析等对煤基固体酸催化剂进行表征。结果表明,当磺化温度为110℃、磺化时间为90 min、固液比为1∶17时,煤基固体酸催化剂具有最优的催化活性,其催化油酸和甲醇的酯化反应的酯化率达到93.50%。煤基固体酸催化剂为具有较低石墨化程度的无定形碳结构,磺酸基已成功键合到了碳基载体上,同时具有丰富的含氧官能团,其表面呈现密集孔结构,且以介孔为主。煤基固体酸催化剂在低于140℃时具有较好的热稳定性,重复使用5次后,催化酯化率为57.21%。Using Shengli lignite as raw material,coal based solid acid catalyst was prepared by one-step carbonization sulfonation of concentrated sulfuric acid.The catalytic activity of the catalyst was evaluated by esterification reaction of oleic acid and methanol.The effects of solid-liquid ratio,sulfonation temperature and sulfonation time on the catalytic activity were investigated.The coal based solid acid catalyst was characterized by IR,EA,BET,SEM,XRD and TG-DTG.The results showed that when the sulfonation temperature was 110℃,the sulfonation time was 90 min,and the solid-liquid ratio was 1∶17,the coal based solid acid catalyst had the best catalytic activity with the esterification rate reaching 93.50%.The catalyst was amorphous carbon structure with low graphitization degree.The sulfonic acid group was successfully bonded to the carbon-based support.The catalyst had abundant oxygen-containing functional groups,and its surface presented dense pore structure,which was mainly mesoporous.The catalyst had better thermal stability below 140℃.After repeated use for 5 times,the esterification rate was 57.21%.

关 键 词：煤基固体酸 一步法 炭化磺化 催化剂 酯化反应 

分 类 号：TQ426[化学工程] TQ420.6