以太西煤基活性炭和聚苯胺为原料制备了煤基碳基固体酸,并采用SEM、XRD和TG对催化剂进行了表征。研究了催化剂对环己酮甘油缩酮反应的催化活性,通过单因素实验得到最佳工艺条件:环己酮与甘油物质的量比为1∶1.2,催化剂质量为反应物质量...以太西煤基活性炭和聚苯胺为原料制备了煤基碳基固体酸,并采用SEM、XRD和TG对催化剂进行了表征。研究了催化剂对环己酮甘油缩酮反应的催化活性,通过单因素实验得到最佳工艺条件:环己酮与甘油物质的量比为1∶1.2,催化剂质量为反应物质量的0.5%,带水剂用量为10 m L。在该条件下环己酮甘油缩酮收率达到96.5%,选择性达98.0%以上,催化剂重复使用5次后收率仍可达88.6%,说明该煤基碳基固体酸具有良好的催化活性和重复使用性。展开更多
Cyclohexanone L-ascorbic acid ketal is synthesized from the reaction of L-isoascorbic acid and cyclohexanone with p-toluene sulfonic acid as catalyst,N,N-dimethyl acetamide(DMAc) as solvent and cyclohexane as water ca...Cyclohexanone L-ascorbic acid ketal is synthesized from the reaction of L-isoascorbic acid and cyclohexanone with p-toluene sulfonic acid as catalyst,N,N-dimethyl acetamide(DMAc) as solvent and cyclohexane as water carrying agent.The optimal reaction conditions determined by orthogonal experiment are as follows:L-ascorbic acid 1.76 g(10 mmol),cyclohexanone 1.57 g(16 mmol),p-toluene sulfonic acid 0.38 g(2 mmol),DMAc 6 mL,cyclohexane 9 mL,reaction temperature 120～125℃ and reation time 2.5 h.The yield is 85.8% under these optimal conditions.The title compound is characterized by 1H NMR,FTIR and EI-MS.展开更多
文摘以太西煤基活性炭和聚苯胺为原料制备了煤基碳基固体酸,并采用SEM、XRD和TG对催化剂进行了表征。研究了催化剂对环己酮甘油缩酮反应的催化活性,通过单因素实验得到最佳工艺条件:环己酮与甘油物质的量比为1∶1.2,催化剂质量为反应物质量的0.5%,带水剂用量为10 m L。在该条件下环己酮甘油缩酮收率达到96.5%,选择性达98.0%以上,催化剂重复使用5次后收率仍可达88.6%,说明该煤基碳基固体酸具有良好的催化活性和重复使用性。
文摘Cyclohexanone L-ascorbic acid ketal is synthesized from the reaction of L-isoascorbic acid and cyclohexanone with p-toluene sulfonic acid as catalyst,N,N-dimethyl acetamide(DMAc) as solvent and cyclohexane as water carrying agent.The optimal reaction conditions determined by orthogonal experiment are as follows:L-ascorbic acid 1.76 g(10 mmol),cyclohexanone 1.57 g(16 mmol),p-toluene sulfonic acid 0.38 g(2 mmol),DMAc 6 mL,cyclohexane 9 mL,reaction temperature 120～125℃ and reation time 2.5 h.The yield is 85.8% under these optimal conditions.The title compound is characterized by 1H NMR,FTIR and EI-MS.
文摘采用DTA和吸附吡啶的FT-IR表征氯氧化锆的表面酸性,用Hamm ett指示剂测定其酸强度,以催化合成环己酮2,3-丁二醇缩酮为探针反应优化缩酮反应条件,并考察它对其他缩酮反应的催化活性,比较了不同催化剂对缩酮活性的影响。实验表明,氯氧化锆表面存在B r nsted酸中心,能使Hamm ett指示剂对-硝基苯胺(Ho=+0.99)变色,环己酮2,3-丁二醇缩酮产率可达96.5%,对其他缩酮化反应均具有良好的催化活性。且催化剂易回收,反应后处理简单,无废酸排放。
