连续流光反应器中连续制备环丁烷四羧酸二酐

Synthesis of Cyclobutane-1,2,3,4-Tetracarboxylic Dianhydride in Continuous Flow Photoreactor

摘要:

摘要：以顺丁烯二酸酐（MA）为原料，乙酸乙酯做溶剂，在连续流光反应器中紫外光照射下连续高效的制备环丁烷四羧酸二酐（CBDA）。考察了溶液在管路中的停留时间、管路的尺寸、反应温度、反应物浓度等因素对产品收率及单位时间产量的影响，对比了连续流光反应器和间歇光反应器对产品收率的影响。实验结果表明：长的停留时间、小的管路内径、低浓度的反应物溶液对提高产品的收率有利，当停留时间80min，管路内径2.00mm，反应温度5℃，反应物浓度0.15g/mL时，产品的收率为51.57%，单位时间产量4.64g/h。与间歇光反应器工艺比较，连续流光反应器具有光子利用率高，光传播过程光子损失量小，紫外光透光率高、照射面积更加充足均匀等优点，产品的收率可提高33%以上，且产品纯度更高。

Abstract:

Abstract：Cyclobutane-1,2,3,4-tetracarboxylic dianhydride（CBDA）was continuously and efficiently synthesized by photodimerization of maleic anhydride（MA）in microreactor under UV irradiation. The influences of residence time of solution in reactor tube, tube size, reaction temperature and reactant concentration on product yield were studied, which showed that longer residence time, smaller inner diameter of the tube and lower reactant concentration were found to result in higher product yield. The yield and the unit time output of product could reach as high as 51.75% and 4.64g/h under reactant concentration of 0.15g/mL, reaction temperature of 5℃ and residence time of 80 min in the reactor tube with 2.00mm inner diameter. The photoreactor has better photon utilization efficiency, uniformity of irradiation, mixability and heat transfer performance compared to traditional batch photoreactor.