单模聚焦微波法制备MIL⁃53(Fe)及其光催化性能研究

Preparation and Photocatalytic Performance of MIL⁃53 (Fe) by Single⁃Mode Focused Microwave

齐永娟 宫晓杰 张丹 吴限 李丽华

Yongjuan Qi Xiaojie Gong Dan Zhang Xian Wu Lihua Li

辽宁石油化工大学 石油化工学院，辽宁 抚顺 113001 东北大学 材料与冶金学院，辽宁 沈阳 110004

School of Petrochemical Engineering，Liaoning Petrochemical University，Fushun Liaoning 113001，China School of Materials & Metallurgy，Northeastem University，Shenyang Liaoning 110004，China

采用单模聚焦微波合成系统快速合成金属有机骨架光催化剂MIL?53(Fe)。选用十六烷基三甲基溴化铵(CTAB)作为添加剂，考察了CTAB的添加对MIL?53(Fe)晶相结构、形貌尺寸的影响，以及微波合成条件对MIL?53(Fe)催化性能的影响。以10 mg/L的罗丹明B为模拟降解物，比较了CTAB添加量对光催化效果的影响。结果表明，CTAB的添加使得MIL?53(Fe)晶体颗粒尺寸缩小，形态更加规整，且当微波反应功率为75 W，温度为100 ℃，反应时间为1 h，n(FeCl3·6H2O)/n(CTAB)=1∶0.5，催化剂质量浓度为0.2 g/L，在300 W钨灯照射100 min时对罗丹明B的降解率可达90%以上。通过自由基捕获实验可知，空穴和·OH是光催化过程中的主要贡献者。

A single?mode focused microwave synthesis system was used to rapidly synthesize MIL?53(Fe).The effect of reaction additive hexadecyl trimethyl ammonium bromide(CTAB) on the crystal structure, morphology, and particle size of MIL?53(Fe), as well as the microwave synthesis conditions on catalytic performance of MIL?53(Fe) were investigated using 10 mg/L Rhodamine B as a target contaminant. The results show that the addition of CTAB reduces the size of MIL?53(Fe) and makes the shape more regular. When the microwave power is 75 W,the temperature is 100 ℃,the synthesis time is 1 h,n(FeCl3·6H2O)/n (CTAB)=1∶0.5,the catalyst dosage is 0.2 g/L,the degradation rate of Rhodamine B can be more than 90% in 100 minutes under the radiation of 300 W tungsten lamp. It was known from free radical capture experiments that holes and ·OH were the main active species in the photocatalytic process.

辽宁省教育厅高校科研基金(L2020039)

10.3969/j.issn.1006-396X.2021.05.004