Development of a slurry continuous flow reactor for photocatalytic treatment of industrial waste water

The water treatment capability of a novel photocatalytic slurry reactor was investigated using methylene blue (MB) as a model pollutant in an aqueous suspension. A pellet TiO ₂ catalyst was employed and this freed the system from the need of filtration of catalyst following photocatalysis. This configuration combines the high surface area contact of catalyst with pollutant of the slurry reactor and also offers a high illumination of catalyst by its unique array of weir-like baffles. In this work, the batch adsorption of MB from aqueous solution (10μM) onto the TiO ₂ catalyst was studied, adsorption isotherms and kinetics were determined from the experimental data. Complete degradation of MB was achieved within 60 min illumination with various loadings of catalyst (30-200 g L ^-1). A modest catalyst loading (30 g L ^-1) achieved 98% degradation within 60 min of irradiation. Experimental results indicate that this novel reactor configuration has a high effective mass transfer rate and UV light penetration characteristics. 

A continuous flow packed bed photocatalytic reactor for the destruction of 2-methylisoborneol and geosmin utilising pelletised TiO2

Taste and odour compounds, especially geosmin (GSM) and 2-methylisoborneol (2-MIB), cause major problems in both drinking water and aquaculture industries world-wide. Aquaculture in particular has experienced significant financial losses due to the accumulation of taint compounds prior to harvest resulting in consumer rejection. UV-TiO2 photocatalysis has been demonstrated to remove GSM and 2-MIB at laboratory scale but the development of a continuous flow reactor suitable for use in water treatment has not been investigated. In this study, a pilot packed bed photocatalytic reactor was developed and evaluated for water treatment with both laboratory and naturally tainted samples. A significant reduction of both 2-MIB and GSM was achieved in both trials using the packed bed reactor unit. With the laboratory spiked water (100ngL-1 of each compound added prior to treatment), detectable levels were reduced by up to 97% after a single pass through the unit. When the reactor was used to treat water in a fish farm where both compounds were being produced in situ (2-MIB: 19ngL-1 and GSM: 14ngL-1) a reduction of almost 90% in taint compounds was achieved. These very encouraging promising results demonstrate the potential of this UV-TiO2 photocatalytic reactor for water treatment in fish rearing systems and other applications.

Efficient and selective hydrogen peroxide-mediated oxidation of sulfides in batch and segmented and continuous flow using a peroxometalate-based polymer immobilised ionic liquid phase catalyst

The peroxometalate-based polymer immobilized ionic liquid phase catalyst [PO4{WO(O-2)(2)}(4)]@PIILP has been prepared by anion exchange of ring opening metathesis-derived pyrrolidinium-decorated norbornene/ cyclooctene copolymer and shown to be a remarkably efficient system for the selective oxidation of sulfides under mild conditions. A cartridge packed with a mixture of [PO4{WO(O-2)(2)}(4)]@PIILP and silica operated as a segmented or continuous flow process and gave good conversions and high selectivity for either sulfoxide (92% in methanol at 96% conversion for a residence time of 4 min) or sulfone (96% in acetonitrile at 96% conversion for a residence time of 15 min). The immobilized catalyst remained active for 8 h under continuous flow operation with a stable activity/selectivity profile that allowed 6.5 g of reactant to be processed (TON = 46 428) while a single catalyst cartridge could be used for the consecutive oxidation of multiple substrates giving activity-selectivity profiles that matched those obtained with fresh catalyst.

Visible-light-mediated synthesis of helicenes in batch and continuous flow systems

Le présent mémoire décrit le développement d’une méthode de synthèse des hélicènes catalysée par la lumière visible. Les conditions pour la formation de [5]hélicène ont été établies par une optimisation du photocatalyseur, du solvant, du système d’oxydation et du temps réactionnel. Suite aux études mécanistiques préliminaires, un mécanisme oxydatif est proposé. Les conditions optimisées ont été appliquées à la synthèse de [6]hélicènes pour laquelle la régiosélectivité a été améliorée en ajoutant des substituants sur la colonne hélicale. La synthèse de thiohélicènes a aussi été testée en utilisant les mêmes conditions sous irradiation par la lumière visible. La méthode a été inefficace pour la formation de benzodithiophènes et de naphtothiophènes, par contre elle permet la formation du phenanthro[3,4-b]thiophène avec un rendement acceptable. En prolongeant la surface-π de la colonne hélicale, le pyrène a été fusionné aux motifs de [4]- et [5]hélicène. Trois dérivés de pyrène-hélicène ont été synthétisés en utilisant les conditions optimisées pour la photocyclisation et leurs caractéristiques physiques ont été étudiées. La méthode de cyclisation sous l’action de la lumière visible a aussi été étudiée en flux continu. Une optimisation du montage expérimental ainsi que de la source lumineuse a été effectuée et les meilleures conditions ont été appliquées à la formation de [5]hélicène et des trois dérivés du pyrène-hélicène. Une amélioration ou conservation des rendements a été observée pour la plupart des produits formés en flux continu comparativement à la synthèse en batch. La concentration de la réaction a aussi été conservée et le temps réactionnel a été réduit par un facteur de dix toujours en comparaison avec la synthèse en batch.

Continuous-flow processing of gaseous ammonia using a Teflon AF-2400 tube-in-tube reactor: synthesis of thioureas and in-line titrations

A simple tube-in-tube reactor based on the gas-permeable membrane Teflon AF-2400 was used in the continuous flow reaction of gaseous ammonia with isothiocyanates and one isocyanate. A colourimetric in-line titration technique is also reported as a simple method to quantify the amount of ammonia taken up by the solvent in the system.

A modular flow reactor for performing Curtius rearrangements as a continuous flow process

The use of a mesofluidic flow reactor is described for performing Curtius rearrangement reactions of carboxylic acids in the presence of diphenylphosphoryl azide and trapping of the intermediate isocyanates with various nucleophiles.

Development of a stable continuous flow immobilized enzyme reactor for the hydrolysis of inulin

A 23.5-fold purified exoinulinase with a specific activity of 413 IU/mg and covalently immobilized on Duolite A568 has been used for the development of a continuous flow immobilized enzyme reactor for the hydrolysis of inulin. In a packed bed reactor containing 72 IU of exoinulinase from Kluyveromyces marxianus YS-1, inulin solution (5%, pH 5.5) with a flow rate of 4 mL/h was completely hydrolyzed at 55 °C. The reactor was run continuously for 75 days and its experimental half-life was 72 days under the optimized operational conditions. The volumetric productivity and fructose yield of the reactor were 44.5 g reducing sugars/L/h and 53.3 g/L, respectively. The hydrolyzed product was a mixture of fructose (95.8%) and glucose (4.2%) having an average fructose/glucose ratio of 24. An attempt has also been made to substitute pure inulin with raw Asparagus racemosus inulin to determine the operational stability of the developed reactor. The system remained operational only for 11 days, where 85.9% hydrolysis of raw inulin was achieved.

Computational thermal analysis of a continuous flow micro Polymerase Chain Reaction (PCR) chip

The first continuous flow micro PCR introduced in 1998 has attracted considerable attention for the past several years because of its ability to amplify DNA at much faster rate than the conventional PCR and micro chamber PCR method. The amplification is obtained by moving the sample through 3 different fixed temperature zones. In this paper, the thermal behavior of a continuous flow PCR chip is studied using commercially available finite element software. We study the temperature uniformity and temperature gradient on the chip’s top surface, the cover plate and the interface of the two layers. The material for the chip body and cover plate is glass. The duration for the PCR chip to achieve equilibrium temperature is also studied.

Milk lactate determination with a rotating bioreactor based on an electron transfer mediated by osmium complexes incorporating a continuous-flow/stopped-flow system

The high sensitivity that can be attained using a bienzymatic system and mediated by the redox polymer [Os(bpy)₂ClPyCH₂NHpoly(allylamine)] (Os-PAA), has been verified by on-line interfacing of a rotating bioreactor and continuous-flow/stopped-flow/continuous-flow processing. When the hydrogen peroxide formed by LO_x layer reaches the inner layer, the electronic flow between the immobilized peroxidase and the electrode surface produces a current, proportional to lactate concentration. The determination of lactate was possible with a limit of detection of 5 nmol l⁻¹ in the processing of as many as 30 samples per hour. This arrangement allows working in undiluted milk samples with a good stability and reproducibility. Horseradish peroxidase [EC 1.11.1.7] and Os-PAA were covalently immobilized on the glassy carbon electrode surface (upper cell body), lactate oxidase [EC 1.1.3.x] was immobilized on a disk that can be rotated.