微波辅助H_(2)SO_(4)/AC催化合成香豆素的研究

H_(2)SO_(4)/AC Catalyzed Synthesis of Coumarin by Microwave Assisted Catalysis

以煤基活性炭负载浓硫酸为催化剂合成香豆素,采用单因素和响应面实验获得较佳的工艺条件。结果表明,该催化剂对香豆素收率影响大小程度依次为:反应温度(C)>反应时间(B)>微波功率(D)>催化剂用量(A)。较佳反应条件为:原料配比苯酚∶丙烯酸为1∶2、催化剂用量15wt%,反应时间为10 min,反应温度为143℃,微波功率为317 W,香豆素产率为87.80%。催化剂重复使用5次后,催化收率仍可达74.31%。响应面实验回归拟合模型为:y=87.86+0.2875A+1.35B+3.75C+0.8542D+1.02AB-0.475AC-0.2475AD-1.47BC-0.52BD-0.395CD-4.77A^(2)-5.64B^(2)-6.67C^(2)-4.18D^(2)。

Coumarin was synthesized with concentrated sulfuric acid supported by coal-based activated carbon as catalyst.The optimum conditions were obtained by single factor and response surface experiments.The results showed that the effect of the catalyst on the yield of coumarin was as follows:reaction temperature(C)>reaction time(B)>microwave power(D)>catalyst dosage(A).The best reaction conditions were:raw material ratio phenol∶acrylic acid 1∶2,catalyst dosage 15wt%,reaction time 10 min,reaction temperature 143℃,microwave power 317 W,coumarin yield 87.80%.The catalytic yield reached 74.31%after repeated use of the catalyst for 5 times.The regression fitting model of response surface experiment was:y=87.86+0.2875A+1.35B+3.75C+0.8542D+1.02AB-0.475AC-0.2475AD-1.47BC-0.52BD-0.395CD-4.77A^(2)-5.64B^(2)-6.67C^(2)-4.18D^(2).