Instant MOFs: continuous synthesis of metal–organic frameworks by rapid solvent mixing

Gimeno-Fabra, Miquel; Munn, Alexis S.; Stevens, Lee A.; Drage, Trevor C.; Grant, David M.; Kashtiban, Reza J.; Sloan, Jeremy; Lester, Edward; Walton, Richard I.

doi:10.1039/c2cc34493a

Cited by 110 publications

(85 citation statements)

References 23 publications

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“…HKUST-1 has been synthesised previously in continuous flow, 28,29,43 and using ethanol in batch. 44 The process reported here combines the use of the green solvent ethanol and a continuous process, and PXRD of the isolated materials from this process confirms the formation of HKUST-1 ( Figure 7).…”

Section: Resultsmentioning

confidence: 99%

“…26,27 Continuous flow synthesis of MOFs has been demonstrated previously in elegant studies using interfacial synthesis to produce hollow MOF capsules on a small scale, 28 and utilising rapid solvent mixing. 29,30 Significantly, however, these methods still make use of organic solvents such as 1-octanol, 28 DMF 29 and EtOH. 30 One of our objectives is to completely eliminate the use of toxic/organic solvents by using high temperature water (HTW).…”

Section: Introductionmentioning

confidence: 99%

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Synthesis of metal–organic frameworks by continuous flow

et al. 2014

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A continuous flow process for the synthesis of a metal-organic framework using only water as the reaction medium and requiring only short residence times is described. This affords a new route to scale-up of materials incorporating many of the principles of green chemistry.The process is demonstrated by the synthesis MIL-53(Al) via continuous flow reaction requiring only 5-6 minutes with a space time yield of 1300 kg m -3 d -1 . We have demonstrated the synthesis of 500 g of MIL-53(Al) using this process, which can be scaled-up further by simply feeding further solutions of metal salt and ligand through the reactor. The product has a higher surface area and a better colour than a commercially produced sample of this MOF.In addition, a new and effective method for the extraction of terephthalic acid from within the pores of MIL-53(Al) using supercritical ethanol has been developed, representing a new methodology for activation and removal of substrates from porous hosts.___________________________________________________________________________

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Synthesis of metal–organic frameworks by continuous flow

et al. 2014

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“…Current MOF synthesis typically involves solvothermal batch processing, [56] with large amounts of solvent and potentially also heat being required. ZIF-8 and HKUST-1, two archetypal and potentially commercially important MOFs, can be prepared electrochemically [57] or in a continuous flow reactor as reported by Lester et al [58] However, synthesis by TSE has been shown to allow for the continuous manufacturing of three MOFs (ZIF-8, HKUST-1, and Al(fumarate)(OH)) in multi-kg h −1 quantities, with little or no solvent being required.…”

Section: Mechanosynthesis Of Mofs and Discrete Metal Complexesmentioning

confidence: 99%

Recent Developments in Mechanochemical Materials Synthesis by Extrusion

Crawford¹,

Casabán

2016

Advanced Materials

113

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Mechanochemical synthesis, i.e., reactions conducted by grinding solid reactants together with no or minimal solvent, has been demonstrated as an excellent technique for the formation of both organic and inorganic compounds. Mechanochemistry is viewed as an alternative approach to chemical synthesis and is not always considered when developing manufacturing processes of fine chemicals. Here, recent advances are highlighted regarding mechanochemical synthesis, by utilizing a well-developed continuous technique - extrusion, and the advantages it offers to further support its use in the manufacturing of these chemicals. To put this work into context, it is shown how extrusion plays a vital role for manufacturing in the food, polymer, and pharmaceutical industries, and how the research carried out by these respective industrialists provides great insight and understanding of the technique, with the results being applicable in the chemical industry. The synthesis of metal-organic frameworks (MOFs) is highlighted herein as an excellent example showcasing the advantages that extrusion provides to the manufacture of these materials, one advantage being the exceptional space time yields (STYs) reported for these processes, at three orders of magnitude greater than conventional (solvothermal) synthesis.

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“…However, over the last 10 years, researchers have had considerable success synthesizing a wider range of materials, including metals [14], spinel materials [15], sulfides [16,17], hydroxides [18,19], phosphates [20], nitrides [21], and more complex materials such as metal organic frameworks [22]. Figure 1 shows a range of particles from metals to oxides to sulfides that were synthesized during the SHYMAN project, which funded this research work.…”

Section: Introductionmentioning

confidence: 99%

Understanding bottom-up continuous hydrothermal synthesis of nanoparticles using empirical measurement and computational simulation

et al. 2016

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(2016) Understanding bottom-up continuous hydrothermal synthesis of nanoparticles using empirical measurement and computational simulation. Nano Research, 9 (11). pp. 3377-3387. ISSN 1998-0000 Access from the University of Nottingham repository: http://eprints.nottingham.ac.uk/41016/1/1215_proof.pdf Copyright and reuse:The Nottingham ePrints service makes this work by researchers of the University of Nottingham available open access under the following conditions. This article is made available under the University of Nottingham End User licence and may be reused according to the conditions of the licence. For more details see: http://eprints.nottingham.ac.uk/end_user_agreement.pdf A note on versions:The version presented here may differ from the published version or from the version of record. If you wish to cite this item you are advised to consult the publisher's version. Please see the repository url above for details on accessing the published version and note that access may require a subscription. ABSTRACTContinuous hydrothermal synthesis was highlighted in a recent review as an enabling technology for the production of nanoparticles. In recent years, it has been shown to be a suitable reaction medium for the synthesis of a wide range of nanomaterials. Many single and complex nanomaterials such as metals, metal oxides, doped oxides, carbonates, sulfides, hydroxides, phosphates, and metal organic frameworks can be formed using continuous hydrothermal synthesis techniques. This work presents a methodology to characterize continuous hydrothermal flow systems both experimentally and numerically, and to determine the scalability of a counter current supercritical water reactor for the large scale production (>1,000 T•year -1 ) of nanomaterials. Experiments were performed using a purpose-built continuous flow rig, featuring an injection loop on a metal salt feed line, which allowed the injection of a chromophoric tracer. At the system outlet, the tracer was detected using UV/Vis absorption, which could be used to measure the residence time distribution within the reactor volume. Computational fluid dynamics (CFD) calculations were also conducted using a modeled geometry to represent the experimental apparatus. The performance of the CFD model was tested against experimental data, verifying that the CFD model accurately predicted the nucleation and growth of the nanomaterials inside the reactor.

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Instant MOFs: continuous synthesis of metal–organic frameworks by rapid solvent mixing

Cited by 110 publications

References 23 publications

Synthesis of metal–organic frameworks by continuous flow

Synthesis of metal–organic frameworks by continuous flow

Recent Developments in Mechanochemical Materials Synthesis by Extrusion

Understanding bottom-up continuous hydrothermal synthesis of nanoparticles using empirical measurement and computational simulation

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