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dc.contributor.authorCrawford, Deborah E.
dc.contributor.authorCasaban, J.
dc.contributor.authorHaydon, R.
dc.contributor.authorGiri, N.
dc.contributor.authorMcNally, T.
dc.contributor.authorJames, S.L.
dc.date.accessioned2020-01-31T11:01:35Z
dc.date.accessioned2020-02-17T12:08:56Z
dc.date.available2020-01-31T11:01:35Z
dc.date.available2020-02-17T12:08:56Z
dc.date.issued2015-03
dc.identifier.citationCrawford D, Casaban J, Haydon R et al (2015) Synthesis by extrusion: continuous, large-scale preparation of MOFs using little or no solvent. Chemical Science. 6(3): 1645-1649.en_US
dc.identifier.urihttp://hdl.handle.net/10454/17639
dc.descriptionYesen_US
dc.description.abstractGrinding solid reagents under solvent-free or low-solvent conditions (mechanochemistry) is emerging as a general synthetic technique which is an alternative to conventional solvent-intensive methods. However, it is essential to find ways to scale-up this type of synthesis if its promise of cleaner manufacturing is to be realised. Here, we demonstrate the use of twin screw and single screw extruders for the continuous synthesis of various metal complexes, including Ni(salen), Ni(NCS)2(PPh3)2 as well as the commercially important metal organic frameworks (MOFs) Cu3(BTC)2 (HKUST-1), Zn(2-methylimidazolate)2 (ZIF-8, MAF-4) and Al(fumarate)(OH). Notably, Al(fumarate)(OH) has not previously been synthesised mechanochemically. Quantitative conversions occur to give products at kg h−1 rates which, after activation, exhibit surface areas and pore volumes equivalent to those of materials produced by conventional solvent-based methods. Some reactions can be performed either under completely solvent-free conditions whereas others require the addition of small amounts of solvent (typically 3–4 mol equivalents). Continuous neat melt phase synthesis is also successfully demonstrated by both twin screw and single screw extrusion for ZIF-8. The latter technique provided ZIF-8 at 4 kg h−1. The space time yields (STYs) for these methods of up to 144 × 103 kg per m3 per day are orders of magnitude greater than STYs for other methods of making MOFs. Extrusion methods clearly enable scaling of mechanochemical and melt phase synthesis under solvent-free or low-solvent conditions, and may also be applied in synthesis more generally.en_US
dc.description.sponsorshipEPSRC (EP/L019655/1)en_US
dc.language.isoenen_US
dc.relation.isreferencedbyhttps://doi.org/10.1039/C4SC03217Aen_US
dc.rightsOpen Access Article. This article is licensed under a Creative Commons Attribution 3.0 Unported Licence.en_US
dc.subjectMetal organic frameworks (MOFs)en_US
dc.subjectMechanochemistryen_US
dc.subjectTwin screw and single screw extrusionen_US
dc.subjectSynthesisen_US
dc.titleSynthesis by extrusion: continuous, large-scale preparation of MOFs using little or no solventen_US
dc.status.refereedYesen_US
dc.date.Accepted2015-01-07
dc.date.application2015-01-08
dc.typeArticleen_US
dc.type.versionPublished versionen_US
dc.date.updated2020-01-31T11:01:48Z
refterms.dateFOA2020-02-17T12:10:48Z


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