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Moreira et al. 52 demonstrated the reverse selectivity of UiO-66 towards liquid-phase separation of xylene isomers. Indeed, the obtained results suggested o-xylene selectivities of 1.8 and 2.4 with respect to m- and p-xylene, at 40 °C with n-heptane as the eluent. Besides, the authors showed that the selectivities were retained upon compression, meaning that no major modification of the pore network took place upon compression. Interestingly, the authors stated that at low concentrations the selectivity values of UiO-66 were comparable to the ones previously reported for MIL-53. However, the latter failed to separate m- and p-isomers unlike UiO-66. Z. Jia, H. Li, Z. Yu, P. Wang and X. Fan, Densification of MOF-5 synthesized at ambient temperature for methane adsorption, Mater. Lett., 2011, 65, 2445–2447, DOI: 10.1016/j.matlet.2011.04.099. Jérémy Dhainaut received his PhD in Chemistry of Materials from the University of Upper Alsace (Mulhouse) in 2012. He further developed an expertise in the fields of porous materials and their shaping through postdoc positions at the Ceramic Synthesis and Functionalisation Laboratory (Cavaillon), the Institute of Research on Catalysis and the Environment (Lyon), the Laboratory of Catalysis and Solid-State Chemistry (Villeneuve d’Ascq), and the Institute for Integrated Cell-Material Sciences (Kyoto). In 2019, he was appointed as a CNRS Researcher at UCCS. His work focuses on studying the effect of shaping methods on the physico-chemical properties of porous materials including MOFs. The MOF title is really unique. It carries an important historical legacy and recognizes work approaching perfection. It is a true honor to receive recognition for one'speers and country. Today, I proudly represent and further with my best abilities the values of professional excellence, innovation and transmission.” explains Meilleur Ouvrier de France ChefChristian Segui What is the competition about? Therefore, each of the shaping techniques provides unique features to the final objects in terms of size and appearance for a defined application. This review will focus on conventional shaping techniques such as granulation, pelletization, extrusion, and spray-drying and challenges associated upon formulation of MOF powders. This will also include the 3D printing method as it can be referred to as a type of extrusion with controlled deposition of the forming paste in three dimensions in space. Therefore, 3D printing allows shaping powders with desired shapes and dimensions for a wide variety of applications. They will be as well discussed in the corresponding section along with the challenges related to the formulation of MOF powders. Besides, a separate section will be dedicated to the so-called non-conventional techniques which include freeze granulation, ice templating and biopolymer precipitation. Membranes and coatings, and sol–gel-based monoliths have been excluded from this review on purpose as they have been recently reviewed. 19

X. Fang, B. Zong and S. Mao, Metal–Organic Framework-Based Sensors for Environmental Contaminant Sensing, Nano-Micro Lett., 2018, 10, 64, DOI: 10.1007/s40820-018-0218-0. 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. A. Dhakshinamoorthy, Z. Li and H. Garcia, Catalysis and photocatalysis by metal organic frameworks, Chem. Soc. Rev., 2018, 47, 8134–8172, 10.1039/C8CS00256H. V. Finsy, H. Verelst, L. Alaerts, D. E. De Vos, P. A. Jacobs, G. V. Baron and J. F. M. Denayer, Pore-Filling-Dependent Selectivity Effects in the Vapor-Phase Separation of Xylene Isomers on the Metal−Organic Framework MIL-47, J. Am. Chem. Soc., 2008, 130, 7110–7118, DOI: 10.1021/ja800686c. As is evident from Table 13, both extrusion and DIW can yield shaped objects while preserving the textural properties of pristine MOFs. The loss in surface area in the case of the 3D printed objects is somewhat higher than the binder content which is due to the presence of the plasticizer. The final printed objects have a developed network of millimeter-sized channels thanks to the layer-by-layer deposition upon printing. This can significantly improve the diffusion of gas or liquid within the shaped objects. Spray-drying The spray-drying technique has been known for over a century. As the name suggests, it is used to dry powder-like materials in a continuous fashion. Compared with ovens and conveyor belts, spray-dryers allow treating several tons per hour of wet product. Over the past few decades, the application potential of spray-drying has considerably expanded and now includes the food industry, 125 the pharmaceutical industry, 126 and many others. 127Fig. 6 Schematic representation of the extrusion process on a piston-type extruder (a) and on a single screw-type extruder (b). Being a MOF undeniably implies responsibility and one of my favorite may well be passing on the passion and art to the next generation. My role at EHL plays an important part in this and I am thrilled every time I see students’ eyes light up when accomplishing something they never thought they were capable of.”concludesMeilleur Ouvrier de France Chef Fabien Pairon 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. 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.

Generally, extruders are divided into screw and piston types. The former allows continuous processing and might consist of one (single screw), two (twin screw) or multiple screws which operate in simultaneous and parallel rotations. On the other hand, piston extruders operate in batch mode; however, they enable the extrusion of pastes with high viscosity and compaction. Ligand codes: BTC – benzene-1,3,5-tricarboxylic acid; BDC – benzene-1,4-dicarboxylic acid; BPTC – biphenyl-3,3′,5,5′-tetracarboxylic acid; BTB – 1,3,5-tris(4-carboxyphenyl)benzene; DHBDC – 2,5-dihydroxy-1,4-benzenedicarboxylic acid; FA – fumaric acid; MIM – 2-methyl imidazole; IP – isophthalate; BPY – 4,4′-bipyridine; NDC – naphthalenedicarboxylic acid; and L – 1 H-pyrazole-4-carboxylic acid. Spray-dryer codes: B-290 – B-290 Mini Spray Dryer (Büchi Labortechnik); SD-1000 – SD-1000 Spray Dryer (Tokyo Rikakikai); and AF-88 – AF-88 Laboratory Spray Dryer (AFIND Scientific Instrument Co. Ltd). “—” not specified. The MOF competition is a fierce one, requiring many months, sometimes years, of intense preparation. It aims to evaluate the dexterity, knowledge of modern and traditional techniques, know-how and creativity of candidates representing over 200 different professions, with artisans representing 16 industries as far-flung and diverse as hospitality, textiles, floral design, leatherworking, and ceramics. Within each category there are several smaller groups representing different specialties.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. A. Dailly an Granulation is the last industrially-mature technology reviewed herein, and allows producing millimeter-sized grains. Two types of granulation techniques are typically discussed: wet granulation, when powders are aggregated in a high-shear rate mixer in the presence of a solvent; and dry granulation, when grains are obtained from a previously shaped object either mildly crushed and sieved, or spheronized. Due to higher stresses applied, the dry granulation implies more severe losses in the initial physicochemical properties of the MOFs, while the wet granulation has a less pronounced effect and therefore might be more adequate. Especially, replacing water with another solvent with a lower surface tension is highly beneficial.