Ball-milling for the green synthesis of metal-organic frameworks: a design-of-experiment approach Qian Yu 1 , Huan Doan 2 , Yongde Xia 1 , Xiayi Hu 3 , Alex John 1 , Yanqiu Zhu 1 and Mi Tian 1* 1 College of Engineering, Mathematics and Physical Sciences, University of Exeter, UK, 2 School of Chemistry, University of Bristol, UK, 3 College of Chemical Engineering, Xiangtan University, China The development of solvent-minimised synthesis is crucial to decreasing dependence on traditional hazardous routes of metal-organic frameworks (MOFs)[1]. This work explored the green synthesis of a copper trimethyl 1,3,5-benzenetricarboxylate (CuBTC or HKUST-1) MOF using mechanochemical synthesis by ball milling. Here, we employed a design-of-experiment (DoE) approach to explore the reaction mechanism and optimise the MOF formation. In this study, the mechanochemical-driven MOF samples were fully characterised by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), scanning electron microscope (SEM) and gas adsorption. The XRD and FT-IR results demonstrate the successful synthesis of CuBTC. SEM images indicate that the particle size of the synthesised MOF samples is between 0.6 µm and 0.9 µm. Interestingly, the mechanochemical synthesis reached a higher yield of 24% than 4% yield from the solvothermal counterpart although the crystal size was slightly smaller. This study is a good showcase for the advantages of mechanochemical synthesis in the rapid preparation of CuBTC, suggesting the development of the green and upscalable synthesis with potential industrialisation promising.
Figure 1. XRD patterns of MS-ball mill (a), FTIR pattern of solvothermal and MS (b), and the SEM images of the MS-hand mill (c) and MS-ball mill synthesised CuBTC (d). References 1. Kumar, S., et al., Green synthesis of metal–organic frameworks: A state-of-the-art review of potential environmental and medical applications. Coordination Chemistry Reviews, 2020. 420 : p. 213407.
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