Abstract:

A novel sulfonated carbon from bamboo (SBC) was prepared by one-pot method using p-toluenesulfonic acid as sulfonating agent. The structure and property of SBC were characterized using elemental analysis, acid-base inverse titration, thermo-gravimetric analysis (TGA), X-ray photon spectroscopy (XPS), XRD and FTIR. Esterification of n-butanol with acetic acid was used as a standard reaction to evaluate the catalytic performance of SBC. The influences of catalyst amount, temperature and molar ratio of acid to alcohol were fully investigated．91.8% conversion of n-butanol with 99.5% selectivity was achieved under the following conditions: reaction temperature 80℃, reaction time 4 h, catalyst amount 10% (mass) of n-butanol, molar ratio of acetic acid to n-butanol 3.5:1. Above 80% conversion of n-butanol could still be reached after SBC was used for 5 times. Additionally, SBC showed comparable or superior catalytic activity in other esterification reactions in comparison with the commercial ion exchange resin Amberslyst-15, which demonstrated that SBC has a good prospect in industrial applications.

Key words: sulfonated carbon, bamboo, catalyst, butyl acetate, esterification, p-toluenesulfonic acid

摘要：

以竹粉为原料、对甲苯磺酸为磺化剂,一锅法制备合成了新型磺化竹炭材料(SBC)。利用元素分析、酸碱反滴定、热重分析(TGA)、X射线光电子能谱(XPS)、X射线衍射(XRD)和傅里叶红外(FTIR)等对所制备的SBC进行了表征。以乙酸和正丁醇的酯化反应为探针反应,评价了SBC的催化作用,考察了催化剂用量、反应温度、酸醇摩尔比等的影响。结果表明,在反应温度为80℃、反应时间4 h、SBC用量为正丁醇质量的10%、酸醇摩尔比为3.5:1的适宜条件下,正丁醇转化率达到91.8%,选择性99.5%。SBC重复使用5次,正丁醇转化率仍可达80%以上。此外,SBC催化其他酯化反应体系的实验结果表明,SBC催化活性接近或优于商品离子交换树脂Amberlyst-15。

关键词: 磺化竹炭, 竹材, 催化剂, 乙酸丁酯, 酯化反应, 对甲苯磺酸