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Peterson et al. 47 performed another study on HKUST-1 to examine the evolution of its physical and chemical properties. Thus, the authors applied pressures of 1000 psi (∼7 MPa) and 10 000 psi (∼69 MPa). While the crystal structure was globally preserved, compressed HKUST-1 exhibited broader reflections as well as high signal-to-noise ratios on the XRD patterns. This suggests partial framework damage. Consequently, there was a certain decrease in BET surface area, from 1698 m 2 g −1 for the powder to 892 m 2 g −1 for the pellets made at ∼69 MPa. These values are somewhat different from the ones reported by Kim et al., 48 who stated that above 10 MPa the HKUST-1 framework underwent structural degradation. At the same time, Dhainaut et al. 49 reported a low (15%) loss in BET surface area for HKUST-1, reaching 1091 m 2 g −1 upon densification at 121 MPa. Besides, they showed that addition of 2 wt% of a binder (graphite) slightly improved the mechanical stability of HKUST-1 pellets without significant loss of BET surface area. They explained this relatively small loss as due to the presence of the remaining solvent within the framework, acting as a scaffold during compression, as well as the slow compression speed applied to the powder bed. S)-2-(2′-(bis (4-(trifluoromethyl)phenyl) phosphino)biphenyl-2-yl)-4-phenyl-4,5-dihydrooxazole MOF Description For MOFs, the primary goal of using binders is to enhance the mechanical stability of the granules. For this purpose, compounds capable of creating decently strong bonds with the surfaces of MOFs are preferred as binders. As an example, this implies cohesion of MOF particles via hydrogen bonding, and therefore, compounds possessing multiple functional groups (mainly –OH) are beneficial. This includes alcohols (polyvinyl), sugars (sucrose, cellulose), esters (hydroxypropyl cellulose) and others. However, upon shaping they cannot be removed due to the limited thermal stability of MOFs. S)-2-(2′-(diphenylphosphanyl)-[1, 1′-biphenyl]-2-yl)-4-isopropyl-4,5-dihydrooxazole MOF Description

A mixture of PVA and PVB was used as a binder in the study by Chanut et al. 71 The authors first mixed 5 g of MOF powder with a 3 wt% polymer blend, followed by periodical spraying of ethanol for a total of 50 mL to cause primary particle agglomeration. Upon sieving, a fraction with sizes between 1.3 and 1.7 mm ( Fig. 5h) was rounded using a rolling device to achieve the final shape. Eventually, the spheres were dried at 110 °C for 12 h to remove the residual ethanol. Less than 10,000 people have ever won the right to call themselves one of the Best Craftsmen in France. MOF winners retain their title for life. Many choose to join the National Society of Meilleur Ouvrier de France, a sort of alumni society for winners. The title is taken so seriously that sporting such a collar fraudulently is a crime punishable by prison-time. Introduction Metal–Organic Frameworks (MOFs; also called Porous Coordination Polymers, PCPs) have attracted a great deal of attention since they were first described in 1995 and developed in the early 2000s. 1,2 They represent a new class of hybrid crystalline microporous materials as they are composed of metal nodes (ions or clusters) bound together by multitopic organic linkers. Such coordination allows for an eventual 1-, 2- or 3-dimensional framework. In most cases, the metal core is formed from transition metals, while the linker is often comprised of cyclic organic compounds presenting carboxylate groups or N-donors. Over the past decades, researchers from all over the world have probed a significant number of different combinations of metal precursors, organic linkers, and synthesis conditions, leading to the discovery of many new MOF structures. Nowadays, this denomination includes several thousand structures including the famous HKUST-1, 3 UiO-66, 4 ZIF-8 5 and MIL-101. 6a Attrition tests were performed by rotating a cylinder containing a baffle and the shaped UiO-66-COOH at 60 rpm for 30 min. The percentage corresponds to the total mass of the fine particles – less than 425 μm – after sieving. Under the same conditions, the UiO-66 framework proved to be more stable toward high pressures. 47 Upon compression up to 69 MPa, the BET surface area of the pellet reached 1080 m 2 g −1, which is identical to that of the parent powder. Therefore, when tested for octane adsorption, the UiO-66 pellet compressed at ∼69 MPa demonstrated a saturation loading comparable to its powder counterpart (2.1 vs. 2.5 mmol g −1, respectively).

Interestingly, they also prepared MIL-100 pellets following the pelletization method and compared the thus formed bodies with the granules in terms of NH 3 adsorption. The latter exhibited higher adsorption capacity at 25 °C (4.4 vs. 3.6 mmol g −1), suggesting that upon pelletization, the parent powder underwent more drastic structural and textural changes as compared to granulation. This was supported by XRD and N 2 physisorption measurements. Finally, other less-popular techniques have been successfully applied for shaping MOFs, among which have been reviewed the so-called molecular gastronomy, ice-templating (also called freeze-casting), and phase separation (also called spinodal decomposition). These three techniques presented very low impact on the physicochemical properties of the MOFs applied and are therefore worth investigating more in detail. It should be noted, however, that ice-templating and phase separation both involve the creation of a second level of porosity macrosized (>50 nm) following the replication of ice crystals and polymers, respectively. Following spinodal decomposition, which is also a phase separation method, Hara et al. 155 prepared UiO-66_NH 2-based monolithic materials with a trimodal pore structure. For that, all MOF precursors were dissolved into DMF along with poly(propylene glycol) (PPG) at 60 °C, and the clear solution was sealed in a hydrophobic glass tube kept at 80 °C. After 12 hours, hydrophilic UiO-66_NH 2 MOF mismatched growth occurred, as well as phase separation with the hydrophobic PPG. After washing with solvent, PPG was evacuated from the monolithic solid, leading to the formation of macropores whose diameter, between 0.9 and 1.8 μm, can be controlled by the amount of PPG. The XRD patterns displayed a few broad reflections, with 2 θ positions comparable to those of the simulated UiO-66. The structural properties of the MOF were proven by FT-IR spectroscopy, yielding a spectrum comparable to that of standard UiO-66_NH 2 powder. All samples presented specific surface areas between 712 and 749 m 2 g −1, further underlining the presence of a microporous network, while interparticular mesoporosity could also be deduced from N 2 sorption isotherms at higher relative pressure. Indeed, the TEM images showed particles with sizes below 50 nm. Uniaxial compression tests demonstrated that these monoliths presented a maximal compressive strength of 2.5 MPa. Interestingly, the authors showed that addition of acetic acid, a known modulator accelerating the crystallization, allowed obtaining larger mesopores. Alternatively, a post-shaping solvothermal treatment also allowed controlling the final size of the mesopores following the secondary growth of the MOF crystals. In 2014, Grande et al. 82 performed a study on the manual extrusion of Co-based UTSA-16 with emphasis on the paste composition. To form the paste, they combined polyvinyl alcohol as the binder and a water/propanol (1/1) mixture as the plasticizer. The paste was further extruded into strips using a syringe of a chosen diameter. The thus-shaped MOFs were then dried at 80 °C for 12 h. When varying the binder content, no significant loss in specific surface area with 2 wt% binder was observed. A further increase to 3 wt% PVA led to a 5% loss of SSA. Notably, the authors stated that an activation temperature lower than 120 °C was insufficient to remove the water/propanol mixture. At the same time, 2 wt% binder was found to be adequate to provide a decent crushing strength of around 20 N upon conventional compression tests, comparable to commercial zeolite 4A extrudates (12 N). For comparison, the absence of a binder resulted in a lower mechanical strength of around 7 N.V. Finsy, L. Ma, L. Alaerts, D. E. De Vos, G. V. Baron and J. F. M. Denayer, Separation of CO 2 / CH 4 mixtures with the MIL-53 (Al) metal–organic framework, Microporous Mesoporous Mater., 2009, 120, 221–227, DOI: 10.1016/j.micromeso.2008.11.007. G. Férey, C. Mellot-Draznieks, C. Serre, F. Millange, J. Dutour, S. Surblé and I. Margiolaki, A Chromium Terephthalate-Based Solid with Unusually Large Pore Volumes and Surface Area, Science, 2005, 309, 2040–2042, DOI: 10.1126/science.1116275.

The thus-shaped objects were found to exhibit XRD patterns similar to a MOF-5 degraded by humidity. This was attributed to the formulation procedure prior to printing rather than to the printing procedure itself. Nevertheless, these 3D printed objects were shown to have the ability to adsorb H 2 despite the complex polymer environment.An aqueous spray-drying synthesis of the Zn-imidazole ZIF-8 was done by Tanaka et al. 134 In a typical synthesis, an aqueous suspension containing Zn-acetate and 2-methylimidazole was spray-dried at T in = 150 °C and a feed rate of 5 mL min −1. These conditions yielded dense spherical particles with an average size of 3.9 μm as confirmed by SEM and TEM. However, the XRD results suggested the formation of an unknown phase different from that of the original ZIF-8. Moreover, the product poorly adsorbed nitrogen as revealed by N 2 sorption measurements. Notably, the authors observed the coordination of dissolved species and therefore the solution turning into a suspension right before spraying. The authors explained this phenomenon as due to the hindrance of crystallization created by acetic acid, a by-product originating from the Zn-precursor. The presence of the acid in the as-synthesized product was demonstrated by means of FTIR spectroscopy and TGA. Accordingly, during the spray-drying process, the as-released acetic acid caused a rearrangement of Zn-(2-methylimidazole) bonds, leading to the amorphization of the final product due to the incomplete coordination of the ligands around the metal. Interestingly, the presence of non-coordinated ligands was similarly evidenced by TGA. However, redispersing the spray-dried particles in an alcohol enabled the recrystallization and thus the formation of the targeted ZIF-8 framework. Interestingly, the size of the alcohol molecule influenced the size of the nanocrystals: specifically, the longer the carbon chain the larger the nanocrystals. However, the microbead size remained in the same range. Upon recrystallization, the product yielded an XRD pattern characteristic of ZIF-8 with a S BET of 1440 m 2 g −1, which is consistent with the results published elsewhere. 135 Surprisingly, once these ZIF-8 microbeads were redispersed in an alcoholic solution, they undergo a transition from dense to hollow superstructures. Hence, the recrystallization process is fed by gradually dissolving the amorphous by-product from the surface to the core of the microbeads.

For instance, the authors used copper hydroxide and trimesic acid mixed with methanol as a feed material to produce HKUST-1. Upon extrusion at room temperature, the product was washed with ethanol and dried to yield HKUST-1 extrudates with a specific surface area of 1738 m 2 g −1 and a crystal structure expected for this MOF. Furthermore, the authors showed that ZIF-8 extrudates can be made by both single and twin screw extrusion processes. For this, they used a blend of zinc carbonate and 2-methylimidazole with no solvent added and extruded it at 200 °C. In both cases, the processes yielded a crystalline product with the ZIF-8 topology and high surface areas: 1604 m 2 g −1 (twin screw) and 1750 m 2 g −1 (single screw). Lastly, the authors produced a highly crystalline Al-fumarate with a BET surface area of 1010 m 2 g −1 by extruding a mixture of Al-sulfate, fumaric acid and sodium hydroxide at 150 °C. It is worth noting that this approach enables the production of MOFs with decent space-time yields (STY) as single and twin screw extrusions are continuous processes. Avci-Camur et al. 141 continued exploiting the spray-drying technique for the synthesis of MOFs, targeting the UiO-66 family and more specifically UiO-66-NH 2 by the combined continuous-flow spray-drying method under aqueous conditions. For this purpose, the authors used water-soluble ZrOCl 2·8H 2O and 2-aminoterephthalic acid as the metal-precursor and the ligand, respectively. In this work specific stress was given to the use of a modulator, the acetic acid. Generally, the application of monotopic acids such as hydrochloric, formic and acetic acids facilitates the formation/crystallization of the UiO-family of MOFs. 142 Accordingly, it was shown that an increase in the acid concentration caused significant changes in textural properties. Thus, the UiO-66-NH 2 prepared with 14% acetic acid in the feed solution yielded microbeads with a S BET of 840 m 2 g −1 when spray-dried at T coil = 90 °C, T in = 150 °C, flow rate = 336 mL min −1 and feed rate = 2.4 mL min −1. However, at elevated (56%) concentrations of the acid, the S BET significantly increased up to 1036 m 2 g −1 under the same operating conditions. It should be noted that a further increase (70%) in the acid content led to a partial loss in crystallinity viewed as a decrease in reflection intensities in the XRD pattern as well as a loss in S BET down to 655 m 2 g −1. This suggests a competition between the modulator and the ligand for coordination with the metal clusters and therefore subsequent structural collapse upon exceeding occupation of the clusters by the modulator. The optimal acid concentration was found to be 30%. At this value, the spray-dried UiO-66-NH 2 yielded microbeads with a size distribution of 4–10 μm ( Fig. 16e) and exhibiting the UiO-66 structure according to XRD results. Besides, the S BET value, 1261 m 2 g −1, lies in the range of non-functionalized UiO-66 made via the solvothermal route with DMF, and is much higher than that of the spray-dried UiO-66-NH 2 prepared by Garzon-Tovar et al. ( S BET = 752 m 2 g −1). 138 Finally, the same protocol was applied to the Zr-fumarate MOF. The corresponding information is given in Table 14. Further reports on shaping ZIF-8 via DIW include the work by Lefevere et al., 112 who managed to formulate the MOF with a blend of inorganic and organic binders. The former was added to improve the mechanical stability of the shaped objects, and the latter to enhance the rheological properties of the paste. Typically, the parent ZIF-8 powder (66.7 wt%) was mixed with bentonite (16.7 wt%) and methylcellulose (16.7 wt%) with a subsequent addition of water and mixing to form a homogeneous printable paste. Once homogenized, it was further loaded into a 50 mL syringe and extruded through 250 and 600 μm diameter nozzles in a layer-by-layer fashion at room temperature ( Fig. 11g and h). R. R. Salunkhe, Y. V. Kaneti and Y. Yamauchi, Metal−Organic Framework-Derived Nanoporous Metal Oxides toward Supercapacitor Applications: Progress and Prospects, ACS Nano, 2017, 11, 5293–5308, DOI: 10.1021/acsnano.7b02796.The craftsmanship exhibition has been held every three to four years and showcases different professions including florists, carpenters, butchers, jewelry makers, and of course pastry chefs, to name just a few. Along with the title, winners receive a medal and state diploma. The MOF competition and its preparation are definitely in my top lifetime memories. The hours of preparation, the stress of the competition, the recognition for all the work and commitment, have alla All has changed me forever. I have pushed myself beyond what I imagined possible and it certainly contributed in making me a better professional.” continues Meilleur Ouvrier de France Chef Thomas Marie The culinary connection