An Oxalate-Bridged Binuclear Iron(III) Ionic Liquid for the Highly Efficient Glycolysis of Polyethylene Terephthalate under Microwave Irradiation.

An oxalate-bridged binuclear iron(III) ionic liquid combined with an imidazolium based cation, (dimim)2 [Fe2 Cl4 (µ-ox)], was synthesized and characterized by a wide range of techniques. This halometallate ionic liquid was active in catalyzing the depolymerization of polyethylene terephthalate (PET) by glycolysis, under conventional and microwave-assisted heating conditions. Both methodologies were very selective towards the production of bis(2-hydroxyethyl)terephthalate (BHET). The employment of microwave heating proved beneficial in terms of time and energy saving when compared to the use of thermal heating. Indeed, dielectric spectroscopy studies revealed that the binuclear iron-containing ionic liquid exhibits an excellent heating response under an electromagnetic field. The catalyst provided quantitative conversions to BHET in the glycolysis of post-consumer PET bottles in only 3 h through microwave heating, as compared to 80 % conversion after 24 h under conventional heating.

Selective molecular annealing: in situ small angle X-ray scattering study of microwave-assisted annealing of block copolymers.

Microwave annealing has emerged as an alternative to traditional thermal annealing approaches for optimising block copolymer self-assembly. A novel sample environment enabling small angle X-ray scattering to be performed in situ during microwave annealing is demonstrated, which has enabled, for the first time, the direct study of the effects of microwave annealing upon the self-assembly behavior of a model, commercial triblock copolymer system [polystyrene-block-poly(ethylene-co-butylene)-block-polystyrene]. Results show that the block copolymer is a poor microwave absorber, resulting in no change in the block copolymer morphology upon application of microwave energy. The block copolymer species may only indirectly interact with the microwave energy when a small molecule microwave-interactive species [diethylene glycol dibenzoate (DEGDB)] is incorporated directly into the polymer matrix. Then significant morphological development is observed at DEGDB loadings ≥6 wt%. Through spatial localisation of the microwave-interactive species, we demonstrate targeted annealing of specific regions of a multi-component system, opening routes for the development of "smart" manufacturing methodologies.