The production of MOFs at large scale in a sustainable way is key if these materials are to be exploited for their promised widespread application. Much of the published literature has focused on demonstrations of preparation routes using difficult or expensive methodologies to scale. One such MOF is nano-zeolitic imidazolate framework-8 (ZIF-8) – a material of interest for a range of possible applications. Work presented here shows how the synthesis of ZIF-8 can be tracked by a range of methods including X-ray diffraction, thermo gravimetric analysis and inelastic neutron scattering – which offer the prospect of in-line monitoring of the synthesis reaction. Herein we disclose how the production of nano-ZIF-8 can be conducted at scale using the intermediate phase ZIF-L. By understanding the economics and demonstrating the production of 1 kg of nano-ZIF-8 at pilot scale we have shown how this once difficult to make material can be produced to specification in a scalable and cost-efficient fashion.

The complex cation [Pt(1)₂]²⁺[(1)= 1,4,7-trithiacyclononane] shows a quasi square based pyramidal structure with one non-bonding sulphur donor atom; electrochemical oxidation at +0.5 V. vs. Fc⁰/Fc⁺(Fc = ferrocene) at 20 °C in MeCN affords a paramagnetic platinum(III) species.

Oxidation of the green [Pd(1)₂]²⁺ cation [(1)= 1,4,7-trithiacyclononane] in 70% aqueous HClO₄ affords the red [Pd(1)₂]³⁺ cation, the single crystal X-ray structure of which shows a tetragonally distorted geometry about the Pd^III centre with Pd–S(1) 2.5448(15), Pd–S(4) 2.3558(14), and Pd–S(7) 2.3692(15)Å.

The PdO–Pd phase transformation in a 4 wt% Pd/Al₂O₃ catalyst has been investigated using in situ X-ray absorption spectroscopy (XAS) and in situ X-ray total scattering (also known as high-energy X-ray diffraction) techniques. Both the partial and total pair distribution functions (PDF) from these respective techniques have been analysed in depth. New information from PDF analysis of total scattering data has been garnered using the differential PDF (d-PDF) approach where only correlations orginating from PdO and metallic Pd are extracted. This method circumvents problems encountered in characerising the catalytically active components due to the diffuse scattering from the disordered γ-Al₂O₃ support phase. Quantitative analysis of the palladium components within the catalyst allowed for the phase composition to be established at various temperatures. Above 850 °C it was found that PdO had converted to metallic Pd, however, the extent of reduction was of the order ca. 70% Pd metal and 30% PdO. Complementary in situ XANES and EXAFS were performed, with heating to high temperature and subsequent cooling in air, and the results of the analyses support the observations, that residual PdO is detected at elevated temperatures. Hysteresis in the transformation upon cooling is confirmed from XAS studies where reoxidation occurs below 680 °C.