摘要
通过膨化淀粉和对甲基苯磺酸混合物的部分炭化制备碳基固体酸催化剂,用XRD、红外光谱、元素分析和热分析进行了表征,研究了碳基固体酸催化剂在环己酮甘油缩酮合成中的催化性能,考察环己酮与甘油摩尔比、催化剂用量和反应时间等因素的影响。XRD分析和酸碱电位滴定结果表明,膨化淀粉和对甲基苯磺酸混合物部分炭化生成含有高密度-SO3H基团的芳香碳薄层组成的无定形炭。在n(环己酮)∶n(甘油)为1∶1.2、催化剂的质量分数为10%、环己烷15mL和回流反应时间为120min的条件下,环己酮甘油缩酮的收率可达到99.2%。催化剂重复使用6次后,活性下降很小。
Amorphous carbon material prepared from expanded starch and p-toluene sulfonic acid has been examined as a novel strong solid acid catalyst.The catalytic performances were studied on condensation of cyclohexanone with glycerol.The effects of molar ratio of glycerol with cyclohexanone,catalyst concentration and reaction time were discussed.The results of XRD and acid-base titration indicated the incompletely carbonization of the mixtures of expanded starch and p-toluene sulfonic acid results in amorphous carbon consisting of small polycyclic aromatic carbon sheets with high density of -SO3H groups.When the condensation reaction was carried out with n（cyclohexanone）∶n（glycerol） 1∶1.2,mass fraction of catalyst 10%,cyclohexane 15 mL and refluxe time 120 min,the maximum yield of ketals was 99.2%.There was very little change in the catalytic activity of the regenerated catalyst,even after six cycles.
出处
《香料香精化妆品》
CAS
2011年第3期17-20,28,共5页
Flavour Fragrance Cosmetics
基金
辽宁省教育厅资助项目(05L299)
关键词
碳基固体酸
缩合
环己酮
甘油
缩酮
carbon-based solid acid condensation cyclohexanone glycerol ketal
