Synthesis of a Metal–Organic Framework Material, Iron Terephthalate, by Ultrasound, Microwave, and Conventional Electric Heating: A Kinetic Study

Abstract

A metal-organic framework material named MIL-53(Fe), iron terephthalate, has been synthesized sovothermally at a relatively low temperature by not only conventional electric (CE) heating, but also by irradiation under ultrasound (US) and microwave (MW) conditions to gain an understanding of the accelerated syntheses induced by US and MW. The kinetics for nucleation and crystal growth were analyzed by measuring the crystallinity of MIL-53(Fe) under various conditions. The nucleation and crystal growth rates were estimated from crystallization curves of the change in crystallinity with reaction time. The activation energies and pre-exponential factors were calculated from Arrhenius plots. It was confirmed that the rate of crystallization (both nucleation and crystal growth) decreases in the order US>MW>>CE, and that the accelerated syntheses under US and MW conditions are due to increased pre-exponential factors rather than decreased activation energies. It is suggested that physical effects such as hot spots are more important than chemical effects in the accelerated syntheses induced by US and MW irradiation. The syntheses were also conducted in two steps to understand quantitatively the acceleration induced by MW and it was found that the acceleration in crystal growth is more important than the acceleration in nucleation, even though both processes are accelerated by MW irradiation.

MIL-53(Fe) MOF-mediated catalytic chemiluminescence for sensitive detection of glucose

“…1a, MIL-53(Fe) exhibits a sphere-like shape with an average size of about 600 nm. Also, it can be observed that these MIL-53(Fe) particles have good uniformity, which is consistent with previous reports [33]. The XRD pattern of the prepared MIL-53(Fe) in Fig.…”

“…The XRD pattern of the prepared MIL-53(Fe) in Fig. 1b was consistent with previous reports [32,33]. It is noted that the XRD pattern of MIL-53(Fe) after CL reaction was almost the same as that of the original MIL-53(Fe) (Fig.…”

A novel combined manufacturing technique for rapid production of IRMOF-1 using ultrasound and microwave energies

“…Potentially, MOF materials can be applied in numerous industrial applications including gas separation, adsorption and storage processes [15,16], heterogeneous catalysis [7], pharmaceutical manufacturing processes and drug delivery [10]. Carbon dioxide (CO 2 ) is one of the main green house gases, which is known for its harmful effect on global warming and climate change.…”

Liquid-phase dehydration of sorbitol under microwave irradiation in the presence of acidic resin catalysts

“…However, accelerated MW-syntheses of Cu 2 O [16], molecular sieves like AlPO-11 and SAPO-11 [17] and metal-organic frameworks (MOFs) such as ironbenzenedicarboxylate [18] and copper-benzenetricarboxylate [19] are mainly due to a very large increase in pre-exponential factors (even with increased E a ). Very recently, Ahnfeldt et al [20] have shown the accelerated synthesis of a MOF (CAU-1-(OH) 2 ) with MWs is due to an increase of pre-exponential factor.…”