反应控制相转移催化环戊烯氧化制戊二酸机制研究

利用反应控制相转移催化剂π-C_5H_5NC_(16)H_(33)]_3{PO_4WO_4]_3}催化环戊烯合成高纯度戊二酸,并对其反应机理和催化剂回收循环机制进行了研究。确定以30%双氧水作为氧化剂时,该催化剂催化环戊烯氧化制戊二酸的较佳反应条件为:C_(H_2O_2):C_(cpe):C_(催化剂)=4.4:1:0.0037,反应温度90℃,反应时间6 h,在该条件下,戊二酸的收率在90%以上。通过GC-MS检测,确定了中间产物和最终产物组成,并以此对反应机理进行了研究。对反应后液体进行重结晶,制得了纯度在99.0%以上的戊二酸产品。利用红外光谱、XRD对新鲜催化剂以及重复利用的催化剂进行了结构表征,研究表明:催化剂在使用过程中活性结构保持不变。催化剂重复使用3次,戊二酸的收率在90%以上。

Study on Synthesis of Glutaric Acid From Cyclopentene Over Reaction-controlled Phase Transfer Catalyst

Glutaric acid with high purity was synthesized from cyclopentene by using reaction-controlled phase transfer catalyst π-C5H5NC16H33]3{PO4WO4]3}, the reaction and catalyst recycling mechanisms were also studied. The suitable reaction condition was determined as follow:CH2O2:Ccpe:Ccatalyst=4.4:1:0.0037, the reaction temperature 90℃ , reaction time 6 h, using 30% hydrogen peroxide as oxidant. Under this condition, the yield of glutraric acid can be over 90%. The compositions of intermediates and final products were determined by GC-MS testing, the reaction mechanism was proposed. The products with more than 99.0% purity could be obtained by recrystallization of the liquid after the reaction. The activity structure of the catalyst kept invariability in the process of using it. The yield of glutaric acid was over 90% in reusing of the catalyst.