The relationship of dielectric response and water activity in food

This study has deduced a correlation between points of inflection of water activity and loss factor with respect to moisture content. A point of inflection in loss factor with respect to moisture content was found to coincide with the sorption isotherm point of inflection that defines the transition from multilayer to solution in every instance analysed, with an average difference of just 0.01kg.kg-1. Food can support microbial growth and chemical reactions in water activity levels above this critical transition. This correlation was discovered using published dielectric and sorption data for specific foods at similar temperatures. It was found that low sugar foods containing high levels of hydrocolloids generally exhibited different behaviour from fruits. This shows that microwave heating behaviour will be different in fruits compared to low sugar foods with high hydrocolloid content when drying to achieve a certain water activity and therefore shelf life

Characterisation of potato crisp effective porosity using micro-CT

Background The effective porosity is an important quantitative parameter for food products that has a significant effect on taste and quality. It is challenging to quantify the apparent porosity of fried potato crisps as they have a thin irregularly shaped cross section containing oil and water. This study uses a novel micro-CT technique to determine the solid volume fraction and hence the effective porosity of three types of potato crisps: standard continuously fried crisps, microwaved crisps, and continuously fried ‘kettle’ crisps. Results It was found that continuously fried kettle crisps had the lowest effective porosity at 0.54, providing the desired crunchy taste and lower oil contents. Crisps produced using a microwave process designed to mimic the dehydration process of standard continuous fried crisps had an effective porosity of 0.65, which was very similar to the effective porosity of 0.63 for standard continuously fried crisps. The results were supported by the findings of a forced preference consumer test. Conclusion The effective porosity affects the product taste and is therefore a critical parameter. This study shows that micro-CT analysis can be used to characterise the change in effective porosity of a thin irregularly shaped food product, caused by a change of cooking procedure

Enhanced 'In-situ' catalysis via microwave selective heating: catalytic chain transfer polymerisation

An extremely facile, single stage, ‘in-situ’, Catalytic Chain Transfer Polymerisation (CCTP) process has been identified, where the optimal polymerisation process was shown to depend upon a combination of catalyst characteristics (i.e. solubility, sensitivity, activity) and the method of heating applied. In comparison to the current benchmark catalyst, the preparation of which is only about 40 % efficient, this represents a significant increase in waste prevention/atom efficiency and removes the need for organic solvent. It was also shown possible to significantly reduce the overall ‘in-situ’ reaction cycle time by adopting different processing strategies in order to minimise energy use. The application of microwave heating was demonstrated to overcome system diffusion/dilution issues and result in rapid, ‘in-situ’ catalyst formation. This allowed processing times to be minimised by enabling a critical concentration of the species susceptible to microwave selective heating to dominate the heat and mass transfer involved

Methodology for the synthesis of methacrylate monomers using designed single mode microwave applicators

© 2019 The Royal Society of Chemistry. A novel single-well prototype high throughput microwave reactor geometry has been produced and shown to be capable of synthesizing an array of non-commercially available methacrylate monomers. The reactor, which delivers the energy required via a dedicated coaxial line, has been shown experimentally to outperform other conventional/microwave formats. It is demonstrated to achieve significantly higher conversions than the alternative reactor types, whilst requiring (a) low levels of input power, (b) no additional energy for agitation/mass transfer, (c) no solvent and (d) no environmentally impacting thermos-fluids

Realising the environmental benefits of metal–organic frameworks: recent advances in microwave synthesis

Metal–organic frameworks (MOFs) are a broad class of porous crystalline materials that show great potential for a wide-range of applications in areas such as energy and environmental sustainability. MOFscan show significant advantages in gas selectivity and separation over traditional adsorbents such as zeolites and activated carbons since they are tuneable both in terms of porosity and chemical functionality. The ability to control the pore environment of the MOF is one of their remarkable advantages and affords control over the structure and properties required for specific applications. Despite these advantages, the industrial adoption of MOFs is slow owing to the paucity of scalable, environmentally sustainable manufacturing methods and higher costs compared to zeolites. Microwave (MW) technology is an extremely promising method of MOF production owing to significantly reduced reaction times and subsequently lower process energy consumption, control over MOF properties, and the ability to produce MOFs and MOF-hybrids otherwise difficult to isolate or unobtainable through other synthetic routes. However, the ability to produce the multiple kilogram or even tonne quantities of MOFs required by industry using MW technology is yet to be achieved owing to little or no understanding of the interaction(s) of reactants and MOFs with the electric field, and crucially, how this informs the design of the scale up processes. This review aims to bridge this gap in knowledge by (1) highlighting recent advances in understanding of MW–MOF interactions and areas for future focus; (2) providing an up-to-date and comprehensive summary of literature on MW synthesis of MOFs, focusing on examples where MW heating has facilitated novel and unique results in the laboratory; and (3) emphasising the advantages, challenges and current steps and methodologies required towards industrial-scale MW production of MOFs

Combining continuous flow oscillatory baffled reactors and microwave heating: Process intensification and accelerated synthesis of metal-organic frameworks

We have constructed a continuous flow oscillatory baffled reactor (CF-OBR) equipped with a homogeneous and controllable microwave applicator in an entirely novel design. This affords a new route to chemical production incorporating many of the principles of process intensification and allows, for the first time, investigation of the synergistic benefits of microwave heating and CF-OBRs such as; faster and continuous processing; improved product properties and purity; improved control over the processing parameters; and reduced energy consumption. The process is demonstrated by the production of a metal-organic framework (MOF), HKUST-1, a highly porous crystalline material with potential applications in gas storage and separation, catalysis, and sensing. Our reactor enabled the production of HKUST-1 at the 97.42 g/h scale, with a space time yield (STY) of 6.32 × 105 kg/m3/day and surface area production rate (SAPR) of 1.12 × 1012 m2/m3/day. This represents the highest reported STY and fastest reported synthesis (2.2 seconds) for any MOF produced via any method to-date and is an improvement on the current SAPR for HKUST-1 by two orders of magnitude owing to the superior porosity exhibited by HKUST-1 produced using our rig (Langmuir surface area of 1772 compared to 600 m2/g)

Molecular differentiated initiator reactivity in the synthesis of poly(caprolactone)-based hydrophobic homopolymer and amphiphilic core corona star polymers

Macromolecules that possess three-dimensional, branched molecular structures are of great interest because they exhibit significantly differentiated application performance compared to conventional linear (straight chain) polymers. This paper reports the synthesis of 3- and 4-arm star branched polymers via ring opening polymerisation (ROP) utilising multi-functional hydroxyl initiators and Sn(Oct)2 as precatalyst. The structures produced include mono-functional hydrophobic and multi-functional amphiphilic core corona stars. The characteristics of the synthetic process were shown to be principally dependent upon the physical/dielectric properties of the initiators used. ROP’s using initiators that were more available to become directly involved with the Sn(Oct)2 in the “in-situ” formation of the true catalytic species were observed to require shorter reaction times. Use of microwave heating (MWH) in homopolymer star synthesis reduced reaction times compared to conventional heating (CH) equivalents, this was attributed to an increased rate of “in-situ” catalyst formation. However, in amphiphilic core corona star formation, the MWH polymerisations exhibited slower propagation rates than CH equivalents. This was attributed to macro-structuring within the reaction medium, which reduced the potential for reaction. It was concluded that CH experiments were less affected by this macro-structuring because it was disrupted by the thermal currents/gradients caused by the conductive/convective heating mechanisms. These gradients are much reduced/absent with MWH because it selectively heats specific species simultaneously throughout the entire volume of the reaction medium. These partitioning problems were overcome by introducing additional quantities of the species that had been determined to selectively heat

Understanding the acceleration in the ring-opening of lactones delivered by microwave heating

AbstractThis paper reports the first detailed study focussed upon identifying the influence that microwave heating (MWH) has upon the mechanic steps involved in the tin catalysed ring-opening of lactones such as ɛ-caprolactone (CL). Direct comparison of conventional (CH) and microwave (MWH) heated kinetic studies showed that a key factor in the reduction of the polymerisation cycle time with MWH was the elimination of the induction period associated with in situ catalyst manufacture and initiation. NMR studies demonstrated that the most significant mechanistic change contributing to the observed induction time reduction/elimination was faster initiation (i.e., reaction of the initiatior/catalyst complex with the first monomer unit). Consequently, analysis of the dielectric properties of the reaction components predicted that this MWH induced change was related to the selective volumetric heating of both the catalyst and the monomer. Furthermore, this indication of the greater significance of the initiation step in defining the length of the induction period suggests that this is the rate determining step of the process, whether conducted by CH or MWH. Increasing the catalyst concentration was demonstrated to produce significant reductions in reaction heat-up time and to induce a significant (up to 30 °C) overshoot in reaction mixture bulk temperature in with MWH only. Thus supporting the conclusion that selective heating of the organometallic species in the system contributes directly to differences in the reaction conditions and which need to be taken into account when drawing comparisons with CH systems. Consequently, both effects were concluded to be thermally generated from selective volumetric heating

Modern microwave methods in solid state inorganic materials chemistry: from fundamentals to manufacturing

No abstract available