Production of high purity silica by microfluidic-inclusion fracture using microwave pre-treatment

© 2018 Demand for high purity silica used in component manufacture is set to outstrip current supply in the near future. As such, alternative processing routes to feed-stock materials suitable for use in lighting and solar cell fabrication are required, without having to rely on reject material from semi-conductor manufacture. In this work, we report a facile, environmentally friendly method of producing quartz powder with a total residual impurity level of 30 ± 3 ppm from whole pebbles having an initial impurity level of 158 ± 22 ppm. This has been achieved using a metallurgical upgrading process incorporating microwave pre-treatment, crushing and milling, High Intensity Wet Magnetic Separation (HIWMS) and acid leaching. This process yielded a quartz powder having an 80% reduction in residual impurities compared to the untreated quartz pebbles. Pre-treatment of whole quartz pebbles in a multimode microwave cavity for 10 min yielded a reduction of the residual elemental impurity content associated with micro-fluidic inclusion sites containing calcium, potassium and sodium of 84, 78, and 50% respectively. Statistically significant reduction in residual aluminium phases was also observed (83%) compared to the as received material to below the IOTA® specification for Ultra High Pure Quartz produced by Sibleco. Mechanistically, this has been achieved by selectively heating impurity containing micro-fluidic inclusion sites. Resulting in their explosive decrepitation and enabling removal of the impurities in subsequent processing steps. It has been concluded that natural quartz pebbles can be upgraded through a combination of microwave treatment, magnetic and chemical refinement to produce a viable feedstock for the subsequent production of solar grade silicon

The role of ettringite in the deterioration of artificial lime stabilised soils: a microstructural study

The formation of ettringite has been defined as a major failure mechanism of lime stabilised cohesive soils. It can result in both disruptive volumetric changes and loss of mechanical strength. The mechanisms of its formation and the role it plays in deleterious processes are complex. This paper reports the dimensional and strength changes of a range of artificial lime stabilised cohesive soils subject to two swell test procedures: the UK linear CBR swell test (BS1924-2, BSI 1990) and the European accelerated swell test (EN13286-49, CEN 2007). The resulting microstructural composition was analysed using a combination of Scanning Electron Microscopy and Electron Dispersive X-ray Spectroscopy (SEM-EDX). The results are explained in terms of established theories of crystal formation and subsequent expansion mechanisms

Microwave assisted hydro-distillation of essential oils from fresh ginger root (Zingiber officinale Roscoe)

A solvent free in situ microwave hydro-distillation method for extraction of essential oil from fresh ginger root it presented. Extraction was conducted in a TE10n single-mode microwave cavity and variable power 2 kW generator operating at 2.45GHz. The main extracted components identified by gas chromatography (GC) were Zingiberene, α-Curcumene, β-Sesquiphellandrene and α-Selinene. At energy inputs of 0.40 kWh/kg higher powers and shorter exposure times, crucially did not degrade the highly volatile components (α-Pinene and Camphene) despite providing the highest essential oil yields. Optimum processing conditions were found to be 1000W (0.40kWh/kg) for 5 min, for whole ginger root, where 0.35g oil/100g plant was obtained. This was compared to a yield of 0.2g/100g plant in 150 min in using conventional hydro-distillation and 0.3g/100g plant in 90 min using a multi-mode microwave cavity-based hydro-distillation

Understanding the scabbling of concrete using microwave energy

This paper reports on the use of microwave energy to scabble concrete. While the technique is not new, little information exists relating to the controllability of the process, the effect of different types of concrete and the performance and durability of the scabbled concrete post treatment. Concrete blocks supplied by the UK Sellafield nuclear site were treated with microwave energy using a 15kW system, operating at 2.45GHz. The effect of aggregate type (Whinstone, Gravel and Limestone); standoff distance; and effect of surface coating were studied to determine their influence on the systems performance, in terms of mass and area removal rates. Complimentary modelling studies were undertaken relating the power density of the microwave energy to observed scabbling profile. Mass and area removal rates averaged 11.3gs-1 and 3cms-1 respectively on treating large areas to a depth of 25mm. The process was shown to not adversely affect structural properties of the specimens after treatment

Towards large scale microwave treatment of ores: Part 2 - Metallurgical testing

A pilot scale microwave treatment system capable of treating 10-150t/h of material at 10-200kW was designed, constructed and commissioned in order to understand the engineering challenges of microwave-induced fracture of ores at scale and generate large metallurgical test samples of material treated at approximately 0.3-3kWh/t. It was demonstrated that exposing more of the ore to a region of high power density by improving treatment homogeneity with two single mode applicators in series yielded equivalent or better metallurgical performance with up to half the power and one third the energy requirement of that used with a single applicator. Comminution testing indicated that A*b values may be reduced by up to 7-14% and that the Bond Ball Mill Work Index may be reduced by up to 3-9% depending on the ore type under investigation. Liberation analysis of the microwave-treated ore indicated that equivalent liberation may be achievable for a grind size approximately 40-70µm coarser than untreated ore, which is in agreement with laboratory scale investigations reported in the literature at similar or higher doses. Flow sheet simulations further indicated that reduced ore competency following microwave treatment could potentially yield up to a 9% reduction in specific comminution energy (ECS) at a nominal plant grind of P₈₀190µm, or up to 24% reduction at a grind of P₈₀290µm, for a microwave energy input of 0.7-1.3kWh/t. Throughput could also be increased by up to approximately 30% depending on grind size, ore type and equipment constraints. To date, approximately 900t of material has been processed through the pilot plant, approximately 300t of which was under microwave power. Metallurgical testing has demonstrated that comminution and liberation benefits are achievable at doses lower than that previously reported in the literature, which allow high throughputs to be sustained with low installed power requirements providing a pathway to further scale-up of microwave treatment of ores

Design and optimisation of a microwave reactor for kilo-scale polymer synthesis

Current industrial production of polymer resins is generally undertaken in large multi-tonne stirred tank reactors. These are characterised by relatively slow heating and cooling cycles, resulting in long vessel cycle times and extended production campaigns. In this work we present a design for a hybrid microwave/oil jacket proof of concept system capable of producing up to 4.1?kg of polymer resin per batch. By exploiting rapid volumetric heating effects of microwave energy at 2.45?GHz, we have optimised the synthetic regime, such that a 3.7?kg batch of polyester resin pre-polymer can be made in only 8?h 20?min, with higher molecular weight (Mn 2100) compared to the conventional process taking 22?h 15?min (Mn 1200), yielding an increase in synthesis rate of at least 265%. The increase in polymer molecular weight also suggests a higher conversion was achieved over a shorter time scale

Towards large scale microwave treatment of ores: Part 1 – Basis of design, construction and commissioning

Despite over thirty years of work, microwave pre-treatment processes for beneficiation of ores have not progressed much further than laboratory testing. In this paper we present a scaleable pilot-scale system for the microwave treatment of ores capable of operating at throughputs of up to 150tph. This has been achieved by confining the electric field produced from two 100kW generators operating at 896MHz in a gravity fed vertical flow system using circular choking structures yielding power densities of at least 6x108 W/m3 in the heated mineral phases. Measured S11 scattering parameters for a quartzite ore (-3.69±0.4dB) in the as-built applicator correlated well with the simulation (-3.25dB), thereby validating our design approach. We then show that by fully integrating the applicator with a materials handling system based on the concept of mass flow, we achieve a reliable, continuous process. The system was used to treat a range of porphyry copper ores

Design and Optimisation of a Microwave Reactor for Kilo-Scale Polymer Synthesis

Current industrial production of polymer resins is generally undertaken in large multi-tonne stirred tank reactors. These are characterised by relatively slow heating and cooling cycles, resulting in long vessel cycle times and extended production campaigns. In this work we present a design for a hybrid microwave/oil jacket proof of concept system capable of producing up to 4.1 kg of polymer resin per batch. By exploiting rapid volumetric heating effects of microwave energy at 2.45GHz, we have optimised the synthetic regime, such that a 3.7 kg batch of polyester resin pre-polymer can be made in only 8 hours 20 minutes, with higher molecular weight (Mn 2,100) compared to the conventional process taking 22 hours 15 minutes (Mn 1,200), yielding an increase in synthesis rate of at least 265. The increase in polymer molecular weight also suggests a higher conversion was achieved over a shorter time scale

Development and evaluation of a continuous microwave processing system for hydrocarbon removal from solids

A continuous conveyor-belt processing concept using microwave heating was developed and evaluated. Four hydrocarbon-contaminated soils were used as model feedstocks, and the degree of organic removal was assessed against the power and energy input to the process. The findings of this study at scale (150kg/h) are in direct agreement with data obtained in batch laboratory scale experiments, and show that microwave heating processes are fundamentally scalable. It is shown that there is a trade-off between the efficiency of organic removal and the power distribution, and applying the power in a single stage was found to be 20-30% more energy efficient but the overall degree of organic removal is limited to 60%. 75% removal was possible using two processing steps in series, but the organic removal is ultimately limited by the amount of power that can be safely and reliably delivered to the process material. The concept presented in this work is feasible when 75% organic removal is sufficient, and could form a viable industrial-scale process based on the findings of this study

A novel formulation of inhaled sodium cromoglicate (PA101) in idiopathic pulmonary fibrosis and chronic cough: a randomised, double-blind, proof-of-concept, phase 2 trial

Background Cough can be a debilitating symptom of idiopathic pulmonary fibrosis (IPF) and is difficult to treat. PA101 is a novel formulation of sodium cromoglicate delivered via a high-efficiency eFlow nebuliser that achieves significantly higher drug deposition in the lung compared with the existing formulations. We aimed to test the efficacy and safety of inhaled PA101 in patients with IPF and chronic cough and, to explore the antitussive mechanism of PA101, patients with chronic idiopathic cough (CIC) were also studied. Methods This pilot, proof-of-concept study consisted of a randomised, double-blind, placebo-controlled trial in patients with IPF and chronic cough and a parallel study of similar design in patients with CIC. Participants with IPF and chronic cough recruited from seven centres in the UK and the Netherlands were randomly assigned (1:1, using a computer-generated randomisation schedule) by site staff to receive PA101 (40 mg) or matching placebo three times a day via oral inhalation for 2 weeks, followed by a 2 week washout, and then crossed over to the other arm. Study participants, investigators, study staff, and the sponsor were masked to group assignment until all participants had completed the study. The primary efficacy endpoint was change from baseline in objective daytime cough frequency (from 24 h acoustic recording, Leicester Cough Monitor). The primary efficacy analysis included all participants who received at least one dose of study drug and had at least one post-baseline efficacy measurement. Safety analysis included all those who took at least one dose of study drug. In the second cohort, participants with CIC were randomly assigned in a study across four centres with similar design and endpoints. The study was registered with ClinicalTrials.gov (NCT02412020) and the EU Clinical Trials Register (EudraCT Number 2014-004025-40) and both cohorts are closed to new participants. Findings Between Feb 13, 2015, and Feb 2, 2016, 24 participants with IPF were randomly assigned to treatment groups. 28 participants with CIC were enrolled during the same period and 27 received study treatment. In patients with IPF, PA101 reduced daytime cough frequency by 31·1% at day 14 compared with placebo; daytime cough frequency decreased from a mean 55 (SD 55) coughs per h at baseline to 39 (29) coughs per h at day 14 following treatment with PA101, versus 51 (37) coughs per h at baseline to 52 (40) cough per h following placebo treatment (ratio of least-squares [LS] means 0·67, 95% CI 0·48–0·94, p=0·0241). By contrast, no treatment benefit for PA101 was observed in the CIC cohort; mean reduction of daytime cough frequency at day 14 for PA101 adjusted for placebo was 6·2% (ratio of LS means 1·27, 0·78–2·06, p=0·31). PA101 was well tolerated in both cohorts. The incidence of adverse events was similar between PA101 and placebo treatments, most adverse events were mild in severity, and no severe adverse events or serious adverse events were reported. Interpretation This study suggests that the mechanism of cough in IPF might be disease specific. Inhaled PA101 could be a treatment option for chronic cough in patients with IPF and warrants further investigation