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Bioelectrochemical Reactor Technology for the Treatment of Alkaline Waste Streams of Alumina Industry

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Bioelectrochemical Reactor Technology for the Treatment of Alkaline Waste Streams of Alumina Industry Department of Civil Engineering Bioelectrochemical Reactor Technology for the Treatment of Alkaline Waste Streams of Alumina Industry Tharanga Nimashanie Weerasinghe Mohottige This thesis is presented for the Degree of Doctor of Philosophy of Curtin University September 2017 Declaration To the best of my knowledge and belief, this thesis contains no material previously published by and other person except where due acknowledgement has been made. This thesis contains no material which has been accepted for the award of any other degree or diploma in any university. Signature: Tharanga Nimashanie Weerasinghe Mohottige Date: 22nd September 2018 i Abstract Aluminium is one of the most commercially utilized metals in the world due to its light weight, high strength and excellent corrosion resistance. Aluminium does not occur in its metallic form and refining is required to produce aluminium from its mineral ore. Bauxite is the most commonly used aluminium ore and it is refined in Bayer process to produce alumina (Al2O3). In brief, the major steps of the Bayer process are (1) the digestion of bauxite in a hot concentrated caustic (NaOH) solution; (2) the recovery of aluminium hydroxide (Al(OH)3) with seeded precipitation at low temperature; and (3) the calcination of aluminium hydroxide to produce alumina. The accumulation of organic impurities into the process liquor is a major challenge in Bayer processing. Bauxite contains a range of organic substances, which are extracted into process liquor during the digestion step. After precipitation of aluminium hydroxide, the liquor part (spent liquor) is recycle back to digestion step for reuse of the remaining caustic. However, this recirculation of the spent liquor increases the organics concentration of the process liquor. Among the organic impurities, sodium oxalate (Na2C2O4) is detrimental, as oxalate co-precipitates with Al(OH)3 and reduces the product quality and process efficiency. In Western Australia typical alumina refinery can produce approximately 40 t/d oxalate, which requires environmentally feasible treatment option. Biological processes have been considered as an environmentally sustainable solution for complete degradation of sodium oxalate. The commercial scale aerobic bioreactors are in operation at some refineries in Western Australia. Although the aerobic biodegradation of oxalate is a proven treatment solution, it does not allow the recovery of caustic soda. Therefore, the main objective of this study was to investigate an alternative technology, as bioelectrochemical systems (BES), to biodegrade oxalate and recover caustic soda from solutions that represent Bayer liquor in its alkalinity, salinity and oxalate concentration. The other objective of this research was to investigate the use of nitrogen fixing bacteria in both aerobic bioreactors and BES reactor to alleviate the need for external nitrogen supplementation for oxalate biodegradation. A series of laboratory scale experiments were carried out to: 1) prove the concept of organics removal in BES using alkaline and saline solution under both N- ii supplemented and N-deficient conditions, 2) investigate and compare the caustic recovery under N-supplemented and N-deficient conditions, 3) enrich a haloalkaliphilic oxalate degrading biofilm in an aerobic reactor under both N- supplemented and N-deficient conditions, 4) optimise the aerobic process under different operational parameters (pH, dissolve oxygen concentration (DO) and oxalate cocnentration) and 5) investigate the oxalate degradation in BES using aerobically acclimatised biofilm. Comparative analysis of N-deficient systems vs. N- supplemented systems was conducted to evaluate whether nitrogen fixing microorganisms provide competitive performance as compared to N-supplemented microbial communities. During the entire study, a synthetic solution that stimulate the Bayer liquor alkalinity, salinity and oxalate content was used as the feed solution. As the proof of concept, the feasibility of using BES to oxidise oxalate in the anodic chamber of BES at alkaline and saline conditions with and without N source (reactor R1 with N source, reactor R2 without N source) was investigated. Two identical duel chamber laboratory scale BES reactors (operated > 300 days) filled with graphite granules as the anode and cathode material were used in this experiment. Activated sludge was used as the inoculum source to establish an electrochemically active haloalkaliphilic biofilms. Even though the biofilms in R1 and R2 were unable to anodically oxidise oxalate under the operating conditions (pH 9.0, NaCl 25 g/L and anode potential +200 mV vs. Ag/AgCl), acetate and formate were readily oxidised in the BES. After adding sodium acetate as a co-substrate, the R1 and R2 biofilms produced maximum currents of 227±6.5 mA (Chemical oxygen demand (COD) removal 31%, organic loading rate (OLR) 15.3 kg COD/m3.d) and 135±4 mA (COD removal 38 %, OLR 5.1 kg COD/m3.d), respectively. However, the oxalate removal efficiency was very low (< 5%) compared to complete acetate removal regardless of N supplementation. Further, the results showed that although the bioanode potentials in both R1 and R2 were mostly maintained at +200 mV vs. Ag/AgCl during the start- up, both biofilms were able to generate maximal anodic current at a much lower anode potentials (-300 mV vs. Ag/AgCl for R1; -200 mV vs Ag/AgCl for R2). The microbial community analysis revealed that the inefficient oxalate removal was likely due to the lack of oxalotrophic strains responsible for catalysing the decarboxylation of oxalate. The same two BES reactors were used to investigate the cathodic caustic production under N-supplemented and N-deficient conditions. The BES anodic compartments iii were fed continuously with oxalate and acetate containing saline and alkaline solution simulating the salinity and alkalinity of Bayer liquor (0.4 M NaCl, pH 10), and the anolyte was actively maintained at pH 9 by dosing NaOH. Cathodes were operated in fed-batch mode with 0.4 M NaCl (2 L) as the catholyte. Na+ transfer % to catholyte was higher in N-deficient BES reactor (95.8%) compared to N-supplemented BES (94.9%). Both reactors were able to produce coulombic efficiency (CE) of >75% for caustic generation. The energy input for the caustic production was lower than reported in previous studies conducted by using BES for caustic recovery. To overcome the difficulty in oxalate oxidation for established biofilm inoculated with activated sludge in BES reactors, two aerobic bioreactors were setup to enrich oxalate degrading biofilms. Two packed bed column reactors filled with graphite granules as biofilm carriers were used as aerobic bioreactors (operated > 265 days) for the experiments. Soil samples collected from coastal sediments and rhizosphere from a nature reserve were used as an inoculum source. The graphite granules (conductive material) were used as the biofilm carriers with the aim to use the granules as anode material for later BES experiments. Comparative analysis was carried out to characterise and optimise different operational parameters with N-supplemented and N-deficient conditions. In one set of experiments, oxalate degradation rates and oxygen uptake rates (OUR) were determined at different bulk water DO set-points. The results revealed that oxalate removal rates (33 – 111 mg/h.g biomass) linearly correlated with OUR (0 – 70 mg O2/h.g biomass) in the N-supplemented reactor. However, in the N-deficient reactor, a linear increase of oxalate removal was recorded only with DO up to ≤ 3 mg/L. Surprisingly, anaerobic oxalate removal was evident even in the presence of up to 8 mg/L DO in both reactors. Further investigation revealed formate, acetate and methane as by-products of anaerobic oxalate removal in both reactors. Although an N-deficient culture appears beneficial (no requirements to supplement N) this culture is yet to be fully characterised and compared against the N-supplemented cultures used by the industry. As Bayer liquor is an alkaline solution, the knowledge about the influence of pH is necessary for the industry to consider and adopt haloalkaliphilic nitrogen fixers as a preferable microbial culture. Hence, the influence of pH on oxalate removal efficiencies of two biofilms enriched under N-deficient and supplemented conditions was comparatively examined. Although, N-deficient biofilm iv was acclimatised at pH 9, the highest oxalate removal rate was over a pH range of 7 to 8 possibly due to the inhibition of nitrogenase activity at pH > 8. In contrast, the N- supplemented reactor showed the highest removal rate at pH 9. Further, the effect of other simple organic compounds (sodium acetate, sodium formate, sodium succinate and sodium malonate) present in Bayer process on aerobic oxalate oxidation was evaluated and the results suggested that no influence from the other organics on oxalate oxidation in aerobic reactor regardless of N availability. Until now, there has been paucity of information available on oxalate degradation kinetics, although it is a key design factor for developing bioreactor processes. In this study, Michaelis-Menten kinetics was used to determine the oxalate degradation kinetics in N-deficient and N-supplemented cultures. The N-deficient reactor had a higher affinity (Km) towards oxalate and showed higher maximum specific oxalate oxidation rates (Vmax) compared to the N-supplemented reactor. The derived kinetic parameters were used to propose a novel two step treatment process to remove oxalate
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