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• Published: 29 August 2024

Challenges and solutions to the scale-up of porous materials

• Marziyeh Nazari   ORCID: orcid.org/0000-0002-6805-4705 1 , 2 ,
• Farnaz Zadehahmadi 3 , 4 ,
• Muhammad Munir Sadiq 4 ,
• Ashley L. Sutton   ORCID: orcid.org/0000-0002-8314-8849 4 ,
• Hamidreza Mahdavi   ORCID: orcid.org/0000-0001-8175-4303 3 , 4 &
• Matthew R. Hill 5  

Communications Materials volume  5 , Article number:  170 ( 2024 ) Cite this article

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• Metal–organic frameworks
• Synthesis and processing

With increasing pace, crystalline open frameworks are moving to larger scale, mature applications that stretch as broadly as catalysis, separation, water purification, adsorption, sensing, biomineralization and energy storage. A particular challenge in this development can be the unexpected variation in material properties from batch to batch, even when a cursory analysis would indicate that no process changes occurred. Our team has lived this journey in many larger projects where pilot scale production of metal-organic frameworks for use in devices has been a key milestone and suffered the difficulties of unexpected performance departures. In this Perspective, we aim to share some of the learning outcomes in the hope that it will further speed development in the field.

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Downsizing metal–organic frameworks by bottom-up and top-down methods

A general large-scale synthesis approach for crystalline porous materials

Flux synthesis of two-dimensional covalent organic frameworks

Introduction.

Porous materials consist of a wide variety of chemistries, which include traditional inorganic zeolites, as well as metal-organic frameworks (MOFs) and composite frameworks 1 , 2 . Their microporous and mesoporous structures have diverse practical applications 3 , 4 , such as gas/vapor storage and separation 5 , 6 , 7 , 8 , 9 , purification, chemical sensing 10 , catalysis 11 , 12 , thermoelectric 13 , nerve degradation 14 , drug delivery 15 , 16 , 17 , fuel cell 18 , and energy storage and production 19 , 20 . These materials possess large surface areas and customized pore structures, which make them extremely adaptable for solving complex problems 21 , 22 . As scientific investigation advances, porous materials offer new opportunities for innovation and technological advances 23 . On the other hand, it is fundamentally implied that repeated experiments under the same conditions would produce the same result if an experimentally derived observation were accepted as factual 24 . In practical terms, developing a new material for a practical application cannot be accomplished unless its properties are routinely repeatable. By way of explanation, achieving reproducibility in the field of porous materials research means being able to duplicate the experimental results or computational outcomes consistently when working with these materials. However, there are a number of factors that contribute to the difficulty of this endeavor. In the first instance, reproducibility can be best explored by repeating experiments systematically, which, unfortunately, requires a substantial amount of resources. Second, due to defects, impurities, and experimental and experimenter inconsistencies, the study results may contradict those of an earlier study, posing additional challenges.

Albeit, several approaches may be able to help improve the situation. Among these are the standardization of measurement methods, the definition of measurement or reporting guidelines, and an increase in collaboration between experimentalists and theorists, as well as different laboratories, in order to help corroborate research results, in addition to the use of various tests and cross-checks to ensure that each set of data on adsorption/desorption is valid. Figure 1 is a schematic illustration describing the fundamentals of porous materials research.

Schematic illustration describing the fundamentals in porous materials’ research.

In the following sections we provide a brief overview of our work on the rapid scaling up of new framework materials from laboratory to commercial scale production and application. As well, they present our perspective on how the community can benefit from the understanding of zeolites for rapid scale up and commercialization of relatively new framework materials such as MOFs, polymer/porous material composites (PPMCs), and porous liquids (PLs).

Rapid scale-up of new framework materials from laboratory to commercial scale

The 1950s heralded a breakthrough for zeolites with respect to their industrial-scale deployment in a wide range of applications such as catalysis, ion exchange, and adsorption-based separation processes 25 . When compared to relatively new porous frameworks/materials with a wide range of applications, zeolites are perhaps the most versatile in terms of synthetic and characterization protocols. Despite their potential, zeolite manufacturing processes are complex and limited by the cost associated with technology development, the energy-intensive production process, and a significant carbon footprint 26 . A success story in the commercial scale production of zeolites is that of the Zeolite Linde Type A (Zeolite LTA or Zeolite A) which is one of the largest zeolites employed by volume and value 27 . Zeolites such as Faujasite and Mordenite (MOR) have also been demonstrated for large scale applications such as O 2 production and CO 2 capture 28 , only possible because of the capacity to manufacture them at kg scale. Commercial-scale autoclaves required for manufacturing zeolites have been reported in the 10–20 m 3 scale 26 , 29 .

To tailor their structures and properties for specific applications, the zeolite community used their understanding of the hydrothermal process 30 , 31 , 32 , and different crystal mechanisms 33 , 34 , 35 , 36 to develop sustainable pathways for large-scale zeolite production by selecting low-cost readily available raw materials 37 ; eliminating the use of organic precursors 38 , 39 , 40 , 41 ; and tuning of operating conditions (mixing rate and intensity) 29 . These early successes provided the platform to explore a wider range of sustainable synthetic pathways that leverage the combination of predictive modeling 42 , 43 , and new chemistries 30 , 44 , 45 , 46 , 47 to develop and produce zeolites at scale for industrial applications. For example, Chen et al. 48 discussed the progress in research on the production of zeolites from coal fly ash, one of the most emitted solid wastes globally 49 , and concluded that only two methods (two-step hydrothermal and alkali melting methods) present the most feasible pathway to commercial production and application. This underscores the need for a holistic approach at the onset of the development phase of new zeolites that not only considers new synthetic pathways, materials, and processes but also incorporates techniques such as life cycle assessment (LCA) to ensure a sustainable and environmentally friendly production process 27 .

The last half century has seen the development of new characterization techniques (e.g., surface area measurements, X-ray diffraction, and electron microscopy) 30 , 44 , 50 , 51 , with advances in material chemistry heralding the growth and deployment of zeolites beyond laboratory-based experiments to active materials used for gas separation, catalysis, water processing, agriculture, and biotechnology to mention but a few. Thus, the porous materials community attempts to develop versatile protocols and pathways towards the scale-up and production of new framework materials, adapting the best practices and methods that have been demonstrated to work so well for zeolites. For example, understanding the impact of stirring rates on the crystallinity of ZSM-22 facilitated its industrial-scale production via a sustainable pathway 29 . Therefore, the community must explore and utilize the knowledge generated in process chemistry to produce zeolites at scale to fast-track translating MOF synthesis from the lab bench to industrial-scale processes for a wide range of MOFs.

Metal-organic frameworks

MOFs are a class of generally porous materials, that have an immense potential for gas storage and separation 52 , 53 , 54 , 55 , as well as drug delivery 56 , 57 , 58 , 59 , and catalysis 60 , 61 , 62 . Over the past decade, it has become apparent that there is a broad reproducibility crisis within the literature including both chemistry and chemical engineering 63 , 64 . We have found that the inability to reproduce MOFs reported in the literature hampers both further research efforts and potential benefits to the wider community.

Notably, there have been few systematic reproducibility studies on MOFs 65 , 66 , 67 . Boström and co-workers highlighted some of the reproducibility issues in 2023 65 when they had ten laboratories prepare two closely related MOFs (PCN-222 and PCN-224). Synthetic details were prescribed and included solvent, modulator, temperature, reaction time, and reagent concentration. Despite this, only one of the ten groups produced a phase pure sample of PCN-222 and three groups were able to prepare a phase pure sample of PCN-224. However, it is evident, based on the procedures that individual groups reported, that other factors beyond the ones described above are at play when attempting to reproduce a phase pure sample of PCN-222 or PCN-224. It is not unreasonable to suggest this is likely the case for the synthetic production of many other MOFs at both small and large scales. We take the same stance as Boström and co-workers in that it is important to include as much detail as possible in describing the synthesis of porous materials, including MOFs at all magnitudes of scale-up. An example of detailed procedures is that for articles published in Nature Protocols.

Over the years, MOFs have been synthesized using various methods, including ambient pressure, solvothermal, mechanochemical, microwave-assisted, electrochemical, and flow-based production 68 . Each method has advantages and challenges in reproducibility (see Table  1 ), primarily arising from an inability to precisely control reaction parameters like time, temperature, pressure, reactant concentrations, flow rates, and surface area-to-volume ratios. Adequate control of these parameters ensures reproducibility across the various synthetic techniques. Our group has succeeded at scaling from tens of milligrams to hundreds of kilograms, through careful control of synthetic variables. Generally, intermediate steps (e.g., 1 kg → 10 kg → 100 kg) and optimization at each stage are required for scale-up 69 .

Tens of thousands of MOFs are known, but very few are industrially produced in part due to complex syntheses. Currently there are no standardized procedures for the scale-up of commercially viable MOFs. However, this situation is likely changing. A number of MOF systems are being pursued for scale-up and commercialization including amine-grafted MOFs for CO 2 capture 70 , MIL-160 for water harvesting 71 , CAU-10-H for water harvesting 72 , and CALF-20 also for flue gas CO 2 capture 73 , with BASF producing tons using green chemistry 74 . Scaling up MOF synthesis can impact reproducibility, as changes in conditions affect crystal size, purity, and morphology. For more detail on large-scale MOF production, highlighting synthetic challenges, we refer the reader to the recent article by Chakraborthy et al. 75 .

Further areas worth specifically mentioning are defects and activation processes. Defects are common in MOFs and can have a significant impact on application-specific performance. Despite this, they are often not well characterized. When scaling up, varying levels of defects can have a tremendous impact. An illustrative example of this could be the impact resulting from the variability of defects in MOFs leading to the presence of open metal sites for catalysis 76 . If the material has a variable loading of open metal sites due to defects, it stands to reason that the material's performance will be variable. As part of standard characterization approaches required for MOFs, defects, both of linker and metal type, should be quantified and reported at both laboratory and scale-up stages, especially where such defects are likely to have a considerable impact on application outcomes. We note, however, that this is often not a simple and straightforward process. Fortunately, there have been some characterization successes with standard techniques including thermal gravimetric analysis (TGA) and nuclear magnetic resonance (NMR) 77 , 78 .

Activation is a crucial step in MOF preparation and can be challenging to conduct especially at scale. Over several years, within our group, we have identified a couple of ways to activate materials when transitioning from laboratory scale to pilot scale. These are the use of carrier gas to remove volatile species within the framework 79 and the recognition that MOFs are quite thermally insulative. We have found that if He flows through the MOF-based material whilst heating, we end up with an activated product that has better performance than just heating under a vacuum. We have found this approach to be successful with a varied set of porous materials and consider this to be a valid approach to activate such materials including MOFs. We do, however, note the use of N2, which has both a lower thermal conductivity and specific heat capacity, does not have a similar enhancement. Further, if a large batch of porous material is heated in an oven as a clump, only the outer layer is suitably activated. A simple approach for overcoming this is the use of multiple sparsely layered trays with the MOF material.

For gas-based applications, shaping and pelletization of MOFs are crucial to facilitate efficient mass transport in scaled-up systems. We will focus on pelletization with a polymeric binder, one of the more common methods to produce MOF pellets. An almost universal problem is the partial pore blocking of the MOF with the polymeric binder—this reduces the MOF surface area and performance (e.g., total uptake). However, there is a delicate balance between the performance loss from pore blocking and the gains from the increased mass transport at scale. Efforts are ongoing to address these binder interactions and microstructure, which requires a multidisciplinary approach 80 , 81 .

Composite frameworks

A multitude of applications can be derived from composite materials due to their ability to combine distinct constituents with distinguishing characteristics, thus providing customized properties that exceed those of the constituents individually. It is, however, essential that reproducibility be achieved in order to utilize these benefits 82 , 83 . Cost management, synthesis conditions, maintaining consistency in material ratios, employing reliable characterization techniques, conducting quality control testing, and overseeing intermediate-scale assessments are among the factors to be considered 68 , 84 . Wherefore, as presented in Fig.  2 , it has been Hill’s team’s objective to achieve synthesis replication, which has resulted in significant progress in the production of a variety of composite frameworks that have been produced efficiently, including porous material pellets (PMPs), magnetic framework composites (MFCs), PPMCs, and type II and III PLs, which are porous framework-solvent composites with exceptional reproducibility.

Key composite frameworks development history of Hill’s team (Reproduced with permission from ref. 98 . Copyright 2014, Wiley-VCH 85 ; Copyright 2018, American Chemical Society 89 ; Copyright 2019, Wiley-VCH 102 ; Copyright 2019, Elsevier 88 ; Copyright 2019, American Chemical Society 87 ; Copyright 2019, Royal Society of Chemistry 103 ; Copyright 2020, American Chemical Society 110 ; Copyright 2022, Tsinghua University Press 112 ; Copyright 2023, Royal Society of Chemistry).

Examining PMPs requires an in-depth assessment of their robustness, reliability, and operability. To accomplish this, various factors must be examined in depth, including the type of binders used and the quantity of them, as well as the shaping technique used, such as pelletization under pressure, foaming, extrusion, granulation, and cake crushing extrusion. PMP advancement is a significant step toward its commercial viability. In spite of this, the process of creating scalable PMPs is complex and requires tailoring for each specific porous material 68 , 85 .

In the area of MFCs, evaluating the long-term functioning/stability, effectiveness of the composite material, and dependability of magnetic characteristics 86 , 87 , 88 involves cyclic performance tests (e.g., static and dynamic sorption and desorption experiments) as well as regeneration experiments using induction heating systems, also referred to as triggered release 89 , 90 , 91 . Even so, it is important to note that the development of scalable MFCs that have enhanced sorption and regeneration capabilities requires not only pellet formation and long-term stability but also high productivity and energy efficiency, as well as the ability to work at low regeneration temperatures while minimizing energy consumption 85 , 92 .

For instance, during the film casting process of PPMCs, the rate at which the solvent evaporates, the precise timing needed to form a porous framework dispersion within a polymer dope solution to ensure consistent agglomeration across batches, and colloidal stability of the resulting casting solution all play a key role 93 , 94 , 95 , 96 , 97 . In addition, to ensure a high level of consistency and reliability, several samples are generated and comparison studies are conducted. Also, in order to detect any changes in characteristics that have occurred over an extended period of time, long-term examinations are crucial 98 , 99 , 100 . Meanwhile, achieving scalable production of PPMCs requires a number of factors, including simple processing steps, a dual-layer structure, strong bonding between the polymer and porous framework, uniform particle distribution with minimal aggregation, and the absence of defects in active and substrate layers 101 , 102 , 103 , 104 . Yet, economically acceptable selectivity, enhanced performance, and reduced material expenditures can only be achieved by ensuring a high particle loading, uniformity in the thickness of both the active and substrate layers, and the use of low-cost polymers exhibiting a strong interlayer adhesion property 105 , 106 , 107 .

The transition from the laboratory to the practical application of type II and III PLs in a variety of industries requires an integrated strategy including synthesis, stability, repeatability, appropriate viscosity criteria for porous frameworks and solvent composites, recovery of porous frameworks following the synthesis of the PLs, applications, and economic viability. For instance, several factors contribute to repeatability, including buoyancy, gravity, and interactions between the porous framework and the solvent of the component materials. In order to ensure a functionally appropriate amount of open porosity for functional purposes, it is imperative to prevent the penetration of solvent into the pores of the porous framework 108 , 109 . In addition, the recovery of the material allows for its continuous use, thus reducing the need to synthesize new materials 110 , 111 . In order to achieve maximum performance, substantial consideration should be given to the energy consumption associated with the regeneration of the adsorbent and absorbent constituents of PLs 112 , 113 .

Characterization considerations in porous materials research

At first glance, characterizing porous materials may appear straightforward, however it is often fraught with difficulties 114 . However, by recognizing these traps, awkward mistakes can be avoided, and the data will be able to withstand critical scrutiny.

The BET method, developed in the 1930s for open surfaces and widely used for micro- and mesoporous materials, faces challenges in reproducibility. Researchers should be mindful of BET theory limitations, especially for microporous adsorbents. During a study in which Hill’s team participated, 18 raw adsorption isotherms were provided to sixty-one labs for calculation of the corresponding BET areas 115 . The results of this study showed clear reporting of the pressure range and data points is crucial for BET surface areas. Transparent presentation of isotherms, including a semi-log representation for low-pressure regions, is recommended. Emphasis should be placed on scrutinizing the adsorption isotherm rather than solely relying on the derived BET area. Additionally, using modern computational methods like the BET surface identification (BETSI) algorithm, based on the criteria suggested by Rouquerol et al., for selecting a suitable p/p˳ range, can be very useful for enhancing the transparency of data reported 115 , 116 , 117 , 118 .

While physisorption isotherms are generally reliable for rigid adsorbents, flexibility in materials can lead to variability. A study by Kaskel et al. 119 , analyzed 50 nitrogen physisorption isotherms at 77 K, correlating them with the synthetic and outgassing conditions of DUT-8(Ni), a “gate opening” MOF. The research highlights the importance of accurately documenting experimental details for the reproducibility of scientific results.

Despite the widespread interest in CO 2 adsorption in porous materials, there are only a small number of MOFs for which firm conclusions can be drawn about the reproducibility of these measurements. The study by Sholl et al. 120 , reveals that approximately 20% of reported adsorption isotherms for alcohols in nanoporous materials are considered outliers, cautioning against the indiscriminate use of individual isotherms, an observation that is similar to earlier analyses of CO 2 adsorption experiments 66 . The extended study by this group on the adsorption of alkanes in nanoporous materials shows that 15% of the replicate alkane isotherms are inconsistent with other replicate measurements.

The occurrence of outliers is attributed to variations in material properties stemming from synthesis and sample preparation, including but not limited to sample activation under vacuum or elevated temperature, which may have a marked impact on measured adsorption properties, especially for materials that strongly adsorb water when exposed to ambient conditions. Adsorption in structurally sensitive materials may also be affected by the history of the sample being used or degradation. Taking CuBTC as an example used in different projects in Hill’s team, it has aged over time if not stored under the proper conditions and the isotherms are not reproducible.

The current need to establish a universal format for archiving adsorption data is crucial. There are some studies like the one reported by Evans et al. 121 , who introduced a standard file, AIF, based on the self-defining text archive and retrieval (STAR) procedure, which is an easily extended free-format archive file that is both human and machine-readable. IUPAC has approved the AIF format, and we encourage authors to provide their isotherm data in the AIF development format, as part of their paper supporting information.

Additionally, studies like the one by Smit et al. 122 , 123 , in making connections between databases of gas adsorption experiments and databases of the atomic crystal structure of the corresponding materials can be helpful.

Despite certain research on this topic 66 , 67 , 115 , 119 , 124 , 125 , 126 , 127 , 128 , 129 , there is still a crucial demand for a more extensive investigation like a comprehensive study by Hirscher et al. 130 , on improving reproducibility in hydrogen storage material research to thoroughly assess the reproducibility of different characterization techniques.

As a general conclusion, to assess the properties of a given porous material comprehensively, it is recommended to use a combination of characterization methods such as X-ray diffraction, electron microscopy, and adsorption/desorption isotherms rather than focusing on a single method.

Forward-looking outlook

Overall, there is a lack of standardized protocols for both synthesis and characterization of porous materials. Without standardized methods, comparing results from different studies and reproducing experiments becomes difficult. It is imperative that the community uses the array of tools and techniques currently available to narrow the development period by rapidly translating ideas to products so that it is able to develop new framework materials from lab to industrial scale production with uniform protocols resulting in reproducible structures and materials.

However, having an extensive collection of materials 131 , 132 opens up a number of exciting possibilities, but also presents some challenges; our data and structures are simply too numerous. Considering the large number of structures, there are many issues to be addressed, including how to manage so much data and how to use the data for the discovery of new science. To exploit the unreasonable effectiveness of data, materials scientists should collaborate with data scientists to apply the tools of big data science. To achieve this, it is evident that a clear protocol, open data sharing, and transparency in research practices can significantly increase the reproducibility of studies involving porous materials. As long as all experimental data is transparently shared, libraries/databases of combined experimental efforts involving predicted or hypothetical porous materials generated through density functional theory (DFT) calculations and molecular simulations can be developed 133 , 134 . This is a powerful technique for studying these materials and discovering complex correlations using big-data methods. A machine learning (ML) algorithm is then employed to screen these libraries/databases to identify the most promising materials for a particular application 135 , 136 . Nevertheless, for these challenges to be overcome, researchers, standardization organizations, and funding agencies must work together.

As seen in Fig.  3 , key recommendations to research teams working at scale who are looking to improve reproducibility include:

Employing identical raw materials is of utmost importance. The influence of raw materials on reproducibility is often overlooked. It’s known that the purity and particle size of raw solids can vary between suppliers, potentially affecting crystallization outcomes.

Maintaining the same production size, reactor type, stirring system, recirculation, and other relevant aspects to achieve consistency in particle size and distribution. Particle size and distribution play a critical role, and they can vary significantly with any changes.

Using the same production equipment with documented clean-in-place (CIP) procedures. As MOFs are formed by a nucleation process, the surface of the reactor plays a huge role. It must be kept as consistent as possible. For this same reason, it is important to keep to a previously validated scale for all batch production processes.

Being mindful of drying and activation procedures. At scale, the highly thermally insulating nature of these materials means that desolvation is not facile. Care must be taken to conduct heat to all of the material.

Keeping detailed records of all parameters for each batch. Many of the variations in materials quality, e.g., defects, surface morphology, and surface charge, may not be immediately obvious in characterization processes but drastically change performance outcomes. MOFs and related materials have a ‘memory’ of their production and handling inbuilt; this should be carefully documented.

Carrying out comprehensive crystallization investigations on important porous materials, specifically within the domain of MOFs. This is because the formation mechanisms of most benchmark MOFs are not still well understood. These investigations could assist researchers in more accurately evaluating the robustness of MOF reproducibility at different scales.

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Nazari, M., Zadehahmadi, F., Sadiq, M.M. et al. Challenges and solutions to the scale-up of porous materials. Commun Mater 5 , 170 (2024). https://doi.org/10.1038/s43246-024-00608-y

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Environmental impact of waste treatment and synchronous hydrogen production: based on life cycle assessment method.

1. Introduction

2. materials and methods, 2.1. the principles of the life cycle methods, 2.2. the fundamental analytical framework of the life cycle approach, 2.3. data sources, 3. results and discussion, 3.1. the basic framework of the lca model for synchronous hydrogen production and environmental waste treatment.

3.2. Analysis of the Potential Environmental Impact

3.3. result analysis and improvement measures, 4. conclusions, author contributions, institutional review board statement, informed consent statement, data availability statement, conflicts of interest.

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Luo, Y.; Su, R. Environmental Impact of Waste Treatment and Synchronous Hydrogen Production: Based on Life Cycle Assessment Method. Toxics 2024 , 12 , 652. https://doi.org/10.3390/toxics12090652

Luo Y, Su R. Environmental Impact of Waste Treatment and Synchronous Hydrogen Production: Based on Life Cycle Assessment Method. Toxics . 2024; 12(9):652. https://doi.org/10.3390/toxics12090652

Luo, Yiting, and Rongkui Su. 2024. "Environmental Impact of Waste Treatment and Synchronous Hydrogen Production: Based on Life Cycle Assessment Method" Toxics 12, no. 9: 652. https://doi.org/10.3390/toxics12090652

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