利用化学浸渍法将蔗糖负载到 SBA-15 介孔材料孔道内部, 高温炭化形成的多聚苯环经发烟硫酸气相磺化处理后, 得到磺酸基团功能化的新型碳-硅介孔复合材料. 发烟硫酸气相磺化处理是该材料合成的关键步骤. X 射线衍射、扫描电镜和氮气吸附结果表明, 碳-硅介孔复合材料经磺酸化处理保持了高度有序的介孔结构. 热重、傅里叶变换的红外光谱及吡啶吸附红外光谱结果证明, 磺酸功能基团成功的嫁接于碳-硅介孔复合材料孔道的内表面, 反应活性中心为 Br?nsted 酸, 酸密度在 0.09~0.70 mmol/g 可以有效调变. 当碳负载量为 35% 时, 该复合材料在生物柴油的绿色合成中显示出最优的催化性能, 且可重复使用 3 次以上.
A carbon-mesoporous silica(CS) composite functionalized with sulfonic acid(-SO3H) groups was prepared by controlled carbonization of sucrose impregnated in SBA-15 mesoporous silica and its subsequent sulfonation.The moderate vapor phase sulfonation of the CS composite with fuming sulfuric acid(H2SO4·20%SO3) was the key step in preparing the strong acid solid material(CS-SO3H).Structural analysis and reaction data revealed that sulfonic acid groups were successfully incorporated into the mesoporous CS composite,and the BrΦnsted acid site density was tunable from 0.09 to 0.70 mmol/g by tuning the carbon loading.The sample with 35 wt% carbon exhibited a remarkable catalytic activity for biodiesel production by the esterification of palmitic acid and the transesterification of soybean oil with methanol.