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

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

Abstract

Abstract:

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.

Key words: Microwave synthesis, Metal?organic framework material, Surfactant, Photocatalytic

摘要：

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。

关键词: 微波合成, 金属有机骨架材料, 表面活性剂, 光催化

CLC Number:

TQ034

Yongjuan Qi, Xiaojie Gong, Dan Zhang, Xian Wu, Lihua Li. Preparation and Photocatalytic Performance of MIL⁃53 (Fe) by Single⁃Mode Focused Microwave[J]. Journal of Petrochemical Universities, 2021, 34(5): 24-29.

齐永娟, 宫晓杰, 张丹, 吴限, 李丽华. 单模聚焦微波法制备MIL⁃53(Fe)及其光催化性能研究[J]. 石油化工高等学校学报, 2021, 34(5): 24-29.

Figures/Tables 11

Fig.1 XRD spectra of samples

Fig.2 FTIR spectra of samples

Fig.3 UV?vis spectra of samples

Fig.4 SEM images of samples

Fig.5 Effect of microwave reaction power on photocatalytic activity of MIL?53 (Fe)/CTAB

Fig.6 Effect of microwave reaction temperature on photocatalytic activity of MIL?53 (Fe)/CTAB

Fig.7 Effect of microwave reaction time on photocatalytic activity of MIL?53 (Fe)/CTAB

Fig.8 Effect of CTAB addition on photocatalytic activity of MIL?53 (Fe)/CTAB

Fig.9 Effect of different catalyst dosages on degradation of Rhodamine B

Fig.10 Effect of microwave method and solvothermal method on degradation of Rhodamine B

Fig.11 Free radical capture experiment

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