木质素基固体酸的制备与性能评价  

Preparation and performance evaluation of a lignin-based solid acid

作　　者：梁凤兵[1] 宋彦磊[1] 黄崇品[1] 陈标华[1] 

机构地区：[1]北京化工大学化工资源有效利用国家重点实验室,北京100029

出　　处：《化工新型材料》2014年第10期86-88,108,共4页New Chemical Materials

基　　金：国家自然科学基金(20806007);国家"973"计划(2010CB226902)

摘　　要：以木质素磺酸钠为原料,采用碳化缩聚法制得一种木质素基固体酸,研究了碳化温度对其性能的影响,同时通过酸碱滴定、X射线衍射分析、热重分析、傅立叶红外对木质素基固体酸进行了表征。结果表明,适宜的碳化温度为200~220℃;在碳化过程中,木质素分子中乙酰基和醚键等侧链结构发生断裂,并发生分子内或分子间缩聚交联,形成具有良好热稳定性的无定形芳香族高聚物,其负载磺酸基含量可高达0.35mmol/g。木质素基固体酸的催化活性通过乙酸的酯化反应来表征。酯化结果表明,较于强酸性离子交换树脂Amberlyst-15,此固体酸对乙酸与乙醇酯化反应表现出更好的催化活性。A lignin based solid acid has been prepared by carbonization of sodium lignosulfonate. The effect of car- bonization temperature on the properties of the acid was investigated. The results showed that the optimum temperature for preparation of the acid was from 200℃ to 220℃. Under this condition,the lignosulfonate molecules could underwent con- densation polymerization by the decomposition of the side units（mainly including acetyl groups and ether）and subsequent intermolecular or intramolecular crosslinking to form high molecular weight polymers. The acid was characterized by X-ray diffraction（XRD）, thermogravimetry analysis（TGA）and fourier transform infrared spectroscopy（FT-IR）, and the content of the sulfonic functional groups bound to the material was determined by acid-base titrimetric method. The results sugges- ted that the acid was composed of amorphous cross-linked phenylpropane-hased polymers and had high thermal stability, and the content of sulfonic groups on the material was 0.35mmol/g. The acid catalytic activities of the prepared samples were studied using the esterification of acetic acid with ethanol. The results showed that the acid catalyst exhibited higher activity for the formation of ethyl acetate than that of the conventional ion-exchange resin Amberlyst-15.

关 键 词：木质素磺酸盐 固体酸 碳化 酯化反应 

分 类 号：O636.2[理学—高分子化学]