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Superhydrophobic poly(vinylidene fluoride) (PVDF) membranes were obtained by a surface treatment consisting of oxygen plasma activation followed by functionalisation with a mixture of silica precursor (SiP) (tetraethyl-orthosilicate [TEOS] or 3-(triethoxysilyl)-propylamine [APTES]) and a fluoroalkylsilane (1H,1H,2H,2H-perfluorooctyltriethoxysilane), and were benchmarked with coated membranes without plasma activation. The modifications acted mainly on the surface, and the bulk properties remained stable. From a statistical design of experiments on surface hydrophobicity, the type of SiP was the most relevant factor, achieving the highest water contact angles (WCA) with the use of APTES, with a maximum WCA higher than 155° for membranes activated at a plasma power discharge of 15 W during 15 min, without membrane degradation. Morphological changes were observed on the membrane surfaces treated under these plasma conditions, showing a pillar-like structure with higher surface porosity. In long-term stability tests under moderate water flux conditions, the WCA of coated membranes which were not activated by oxygen plasma decreased to approximately 120° after the first 24 h (similar to the pristine membrane), whilst the WCA of plasma-treated membranes was maintained around 130° after 160 h. Thus, plasma pre-treatment led to membranes with a superhydrophobic performance and kept a higher hydrophobicity after long-term operations.

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Characterisation of the fouling attached to PVDF membranes treating an anaerobic effluent for dissolved CH4 recovery was carried out. A commercial flat-sheet PVDF membrane and a PVDF functionalised by grafting of organofluorosilanes (mPVDF) that increased its hydrophobicity were subjected to a continuous flux of an anaerobic reactor effluent in long-term operation tests (> 800 h). The fouling cakes were studied by the membrane autopsy after these tests, combining a staining technique, FTIR, and FESEM-EDX, and the fouling extraction with water and NaOH solutions. Both organic and inorganic fouling were observed, and the main foulants were proteins, polysaccharides, and different calcium and phosphate salts. Also, a significant amount of live cells was detected on the fouling cake (especially on the non-modified PVDF). Although the fouling cake composition was quite heterogeneous, a stratification was observed, with the inorganic fouling mainly in the bulk centre of the cake and the organic fouling mainly located in the lower and upper surfaces of the cake. The mPVDF suffered a more severe fouling, likely owing to a stronger hydrophobic-hydrophobic interaction with the foulants. Irreversible fouling remained on both membranes after the extraction, although a higher irreversible fouling was detected in the mPVDF; however, a complete polysaccharide removal was observed. Regarding the operation performance, PVDF showed a lower stability and suffered a severe degradation, resulting in a lower thickness and perforations. Finally, the decrease in the methane recovery performance of both membranes was associated with the fouling depositions.

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A three-step surface modification consisting of activation with NaOH, functionalisation with a silica precursor and organofluorosilane mixture (FSiT), and curing was applied to a poly(vinylidene fluoride) (PVDF) membrane for the recovery of dissolved methane (D-CH4) from aqueous streams. Based on the results of a statistical experimental design, the main variables affecting the water contact angle (WCA) were the NaOH concentration and the FSiT ratio and concentration used. The maximum WCA of the modified PVDF (mPVDFmax) was >140° at a NaOH concentration of 5%, an FSiT ratio of 0.55 and an FSiT concentration of 7.2%. The presence of clusters and a lower surface porosity of mPVDF was detected by FESEM analysis. In long-term stability tests with deionised water at 21 L h−1, the WCA of the mPVDF decreased rapidly to around 105°, similar to that of pristine nmPVDF. In contrast, the WCA of the mPVDF was always higher than that of nmPVDF in long-term operation with an anaerobic effluent at 3.5 L h−1 and showed greater mechanical stability, since water breakthrough was detected only with the nmPVDF membrane. D-CH4 degassing tests showed that the increase in hydrophobicity induced by the modification procedure increased the D-CH4 removal efficiency but seemed to promote fouling.

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A full-scale biotrickling filter (BTF) treating acetone air emissions of wood-coating activities showed difficulties to achieve outlet concentrations lower than 125 mg C m-3, especially for high inlet concentrations and oscillating emissions. To solve this problem, a laboratory investigation on acetone removal was carried out simulating typical industrial conditions: discontinuous and variable inlet concentrations and intermittent spraying. The results were evaluated in terms of removal efficiency and outlet gas emission pattern. Industrial emissions and operational protocols were simulated: inlet load up to 70 g C m-3 h-1 during 2 cycles of 4 h per day and intermittent trickling of 15 min per hour. The outlet gas stream of the pollutant was affected by intermittent spraying, causing a fugitive emission of pollutant. Complete removal efficiency was obtained during non-spraying. Average removal efficiencies higher than 85% were obtained, showing the feasibility of BTF to treat acetone. The outlet gas stream showed a clear dependence on the pH of the trickling liquid, decreasing the removal at pH < 5.5. Thus, a proper control of alkalinity, with regular NaHCO3 addition, was required for successful operation. The laboratory findings were fruitfully transferred to the industry, and the removal of acetone by full-scale BTF was improved.

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A three-phase dynamic mathematical model based on mass balances describing the main processes in biotrickling filtration: convection, mass transfer, diffusion, and biodegradation was calibrated and validated for the simulation of an industrial styrene-degrading biotrickling filter. The model considered the key features of the industrial operation of biotrickling filters: variable conditions of loading and intermittent irrigation. These features were included in the model switching from the mathematical description of periods with and without irrigation. Model equations were based on the mass balances describing the main processes in biotrickling filtration: convection, mass transfer, diffusion, and biodegradation. The model was calibrated with steady-state data from a laboratory biotrickling filter treating inlet loads at 13-74 g C m-3 h-1 and at empty bed residence time of 30-15 s. The model predicted the dynamic emission in the outlet of the biotrickling filter, simulating the small peaks of concentration occurring during irrigation. The validation of the model was performed using data from a pilot on-site biotrickling filter treating styrene installed in a fiber-reinforced facility. The model predicted the performance of the biotrickling filter working under high-oscillating emissions at an inlet load in a range of 5-23 g C m-3 h-1 and at an empty bed residence time of 31 s for more than 50 days, with a goodness of fit of 0.84.

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The removal of styrene-polluted air emissions by biotrickling filtration was performed to evaluate the influence of using nitrate and urea as a nitrogen source in the nutrient solution supplied to two bioreactors run in parallel under the same operational conditions for 3 months. The use of urea resulted in less biomass content along the packed bed and better performance of the process, with a maximum elimination capacity (EC) of 57.6 g C m(-3 )h(-1) (removal efficiency (RE) of 88.3% and empty bed residence time (EBRT) of 60 s), which was around 54% higher than when using nitrate. EBRTs of 60, 30 and 15 s were evaluated with a urea-based nutrient supply. By decreasing the EBRT from 60 to 30 s the styrene concentration that could be treated with REs above 80% was almost the half, from 1,100 to 600 mg C m(-3), resulting in ECs of 52.8 g C m(-3) h(-1). Working at 15 s was not possible to obtain REs higher than 40% with a maximum EC of 28.5 g C m(-3) h(-1).

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A 0.75-m3 pilot-scale biotrickling filter was run for over 1 yr in a Spanish furniture company to evaluate its performance in the removal of volatile organic compounds (VOCs) contained in the emission of two different paint spray booths. The first one was an open front booth used to manually paint furniture, and the second focus was an automatically operated closed booth operated to paint pieces of furniture. In both cases, the VOC emissions were very irregular, with rapid and extreme fluctuations. The pilot plant was operated at an empty bed residence time (EBRT) ranging from 10 to 40 sec, and good removal efficiencies of VOCs were usually obtained. When a buffering activated carbon prefilter was installed, the system performance was improved considerably, so a much better compliance with legal constraints was reached. After different shutdowns in the factory, the period to recover the previous performance of the biotrickling reactor was minimal. A weekend dehydration strategy was developed and implemented to control the pressure drop associated with excessive biomass accumulation.

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Laboratory scale-studies on the biodegradation of a 1:1:1 weight mixture of three oxygenated volatile organic compounds (VOCs), ethanol, ethyl acetate, and methyl-ethyl ketone (MEK) in a biotrickling filter (BTF) were carried out using two identically sized columns, filled with different polypropylene rings. The performance of the BTFs was examined for a period of 10 months applying several operational strategies. Similar performance was obtained for both supports. Intermittent flow rate of trickling liquid was shown beneficial to improve the removal efficiency (RE). Continuous feeding of VOC resulted in an excessive accumulation of biomass so high pressure drop was developed in less than 20-30 d of operation. Intermittent VOC loading with night and weekend feed cut-off periods passing dry air, but without addition of water, was shown as a successful operational mode to control the thickness of the biofilm. In this case, operation at high inlet loads (ILs) was extended for more than 75 d maintaining high REs and low pressure drops. Outlet emission concentrations lower than 100 mg Cm(-3) were obtained for ILs up to 100 g Cm(-3)h(-1) working at 15s of empty bed residence time. The most easily biodegradable compounds ethanol and ethyl acetate were used primarily than MEK. After a 3-wk-starvation period, the system performance was almost restored since the first d of operation, being the removal of the less biodegradable compound, MEK, partially deteriorated.

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An upflow packed bed reactor at laboratory scale has been operated for a continuous period of 5 months to investigate the technical feasibility of biological nitrate removal applied to the effluent of the coagulation-sedimentation wastewater of a metal-finishing industry. The reactor was fed with industrial wastewater in a five-fold dilution to reproduce the global spill in the factory (20/80, industrial wastewater/domestic wastewater) with a concentration of nitrate between 141 and 210 gNO(3)-N/m(3). Methanol was added as a carbon source for denitrification. Inlet flow rate was progressively increased from 9 to 40 L/day (nitrogen input load from 45 to 250 gNO(3)-N/(m(3)h)). The highest observed denitrification rate was 135 gNO(3)-N/(m(3)h) at a nitrate load of 250 gNO(3)-N/(m(3)h), and removal efficiencies higher than 90% were obtained for loads up to 100 gNO(3)-N/(m(3)h). A mass relation between COD consumed and NO(3)-N removed around 3.31 was observed. Better results were achieved in a previous stage using tap water with nitrate added as a sole pollutant as a synthetic feed (critical load of 130 gNO(3)-N/(m(3)h) and denitrification rate of 200 gNO(3)-N/(m(3)h) at a nitrate load of 250 gNO(3)-N/(m(3)h)). This fact could indicate that the chemical composition of the industrial source hinders to some extent the performance of the biological process. Whatever case, results demonstrated the viability of the denitrification process for the global industrial wastewater. A simple model based on Monod kinetics for substrate consumption, and constant biomass concentration was applied to model the industrial wastewater treatment, and a reasonably good fitting was obtained.

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Three laboratory-scale peat biofilters were operated at 90 s empty bed residence time (EBRT) for over a year. Biodegradation of ethyl acetate, toluene, or a 1:1 mixture were investigated. In first stage, inlet concentration was progressively increased from 0.4 to 4.5 g/m(3). The maximum elimination capacity (EC) found for ethyl acetate was 190 gC/m(3).h, and it was not affected by toluene. The maximum EC found for toluene as a sole contaminant was 150 gC/m(3).h, but the presence of ethyl acetate decreased the toluene maximum EC to 80 gC/m(3).h. From respirometry monitoring, values of 3.19 g CO(2)/gC and 3.06 g CO(2)/gC for pure ethyl acetate and pure toluene, respectively, were found, with overall yield coefficients of 0.13 g dry biomass produced per gram ethyl acetate consumed and 0.28 g dry biomass produced per gram toluene consumed. CO(2) production in the 1:1 mixture was successfully simulated. Dynamics of living and dead cells were monitored in four sections of the biofilters. Concentrations ranged between 2.6 x 10(9) and 3.0 x 10(10) cells per gram-dry peat for total bacteria, and 2.4 x 10(9)-1.9 x 10(10) cells per gram-dry peat for living bacteria. At high loads loss of bacterial density in the inlet zones, and increase in the dead cells percentages up to 60% was observed. In second stage, long-term performance at an inlet concentration of 1.5 g/m(3) was evaluated to show the process feasibility. Good agreement with previous data was obtained in terms of EC and CO(2) production. Restoration of living cells proportion was also observed.

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