Autotrophic denitrification and chemical phosphate removal of agro-industrial wastewater by filtration with granular medium

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1 Bioresource Technology 98 (27) Autotrophic denitrification and chemical phosphate removal of agro-industrial wastewater by filtration with granular medium Yasuo Tanaka a, *, Atsushi Yatagai b, Hiroshi Masujima c, Miyoko Waki a, Hiroshi Yokoyama a a Waste Recycling Laboratory, National Institute of Livestock and Grassland Science, Ikenodai 2, Tsukuba-shi, Ibaraki 35-91, Japan b Nitchitsu Co. Ltd., Arakawakamitano, Chichibu-shi, Saitama , Japan c Tokyo University of Agricultural, Setagaya-ku, Tokyo , Japan Received 6 June 25; received in revised form 2 March 26; accepted 26 March 26 Available online 16 May 26 Abstract A novel granular medium consisting (1.5 5 mm in diameter) of inert perlite particles as nuclei and an effective surface layer containing sulfur, CaCO 3 and Mg(OH) 2 was developed for advanced treatment of agro-industrial wastewater. The performance of the medium was examined with a laboratory-scale down-flow fixed-bed column reactor using piggery wastewater, which had been treated by an upflow anaerobic sludge blanket reactor and a trickling filter. The removal efficiency of NO x N was more than 7% with a NO x N loading rate of less than approximately.3 kg N m 3 d 1 ; the removal efficiency dropped due to the accumulation of nitrite when the loading rate exceeded that value. A significant drop of phosphate and Mg 2+ concentrations occurred when the effluent ph exceeded 7.9. Ammonium was removed with an average removal efficiency of 12.%. These results indicated that the crystalline reaction of PO 3,Mg2+ and NH þ (MAP reaction) under alkaline conditions contributed to the removal of phosphate. This medium could be useful for the simultaneous reduction of nitrogenous and phosphorus compounds in biologically treated agro-industrial wastewater. Ó 26 Elsevier Ltd. All rights reserved. Keywords: Autotrophic denitrification; Sulfur oxidizing bacteria; Phosphate removal; MAP reaction; Swine wastewater 1. Introduction The sulfur and limestone (CaCO 3 ) autotrophic denitrification (SLAD) process has increasingly been studied due to its high nitrate removal efficiency and cost-effectiveness (Flere and Zhang, 1999). Notwithstanding these advantages, the unbalanced consumption of sulfur and CaCO 3 remains a problem that needs to be worked out of this process before it is ready for industrial use. A granulated sulfur CaCO 3 mixture material, named SC11, made from sulfur and CaCO 3 of equal quantities by weight, was developed by Kawaharazuka et al. (21) to overcome this defect. This material was promising from the point of view of balancing the consumption of sulfur and CaCO 3, because CaCO 3 particles were homogeneously embedded * Corresponding author. Tel.: ; fax: address: osuya@affrc.go.jp (Y. Tanaka). in the sulfur matrix. However, efficient backwashing of the medium bed was difficult due to the large diameter (5 2 mm) of the granulated medium. Flere and Zhang (1999) have pointed out that sufficient backwashing was indispensable to the SLAD process. The objective of this study was to develop a novel medium with both balanced consumption of constituents and an appropriate diameter for the backwashing process. The study also aimed at providing phosphorus removal activity to the medium. 2. Methods 2.1. Granular medium The granular medium was prepared as follows. First, limestone powder (>98% CaCO 3 content; 3 mesh pass) /$ - see front matter Ó 26 Elsevier Ltd. All rights reserved. doi:1.116/j.biortech

2 788 Y. Tanaka et al. / Bioresource Technology 98 (27) and Mg(OH) 2 powder (1 lm diameter) were mixed with melted sulfur (12 C) (weight ratio of CaCO 3, Mg(OH) 2 and S was 1:.9:1). Perlite particles (1 3 mm diameter) were added to the melted mixture as nuclei and the melted mixture was coated on the particles with a granulating machine that maintained the temperature at 12 C. The coated particles (1.5 5 mm diameter) were cooled and used for the experiment. The final composition of the medium by weight was 25.6% sulfur, 25.6% CaCO 3, 23% Mg(OH) 2, and 25.8% perlite. Mixing of the CaCO 3 was important to successful granulation of the medium. The density of the medium determined with the pycnometer method was Reactor and experimental procedure Discharge water from the swine wastewater treatment plant at the Japanese National Institute of Livestock and Grassland Science was used as the influent for experiments. The plant consists of an anaerobic treatment reactor (UASB reactor) and an aerobic treatment reactor (trickling filter) for post-treatment. Fig. 1 shows a schematic representation of the experimental apparatus. The reactor was column-shaped (7.8 cm diameter and 65 cm height). A plastic punched-plate was attached at 2 cm above the reactor bottom to support the medium. The granular medium of.9 kg was put into the reactor (medium bed depth was 1 cm). The influent was stored in a 6-L plastic tank maintained at about 1 C. Newly collected influent (6-L) was supplied to the tank every two weeks. The influent water quality fluctuated throughout the experimental period due to the difference in the water quality of the collected discharge water and successive autochthonous change in the water quality due to biological and chemical reactions during storage. The influent was fed into the reactor by a diaphragm pump at a flow rate of L d 1, and the effluent was discharged from the bottom of the reactor. The hydraulic retention time (HRT) corresponding to the nominal bed volume (.8 L) was 2.9 h. The initial water depth on the medium bed layer was 25 cm. Backwashing was carried out when the water depth exceeded 35 cm. The procedure for backwashing was as follows. Three seconds of aeration with a compressor was carried out 2 times with a 2-s pause between aerations, then water in the reactor was drained completely through two drain valves. The experiments were carried out at 2 C in the dark Analytical methods The ph was determined using a glass electrode. The concentrations of NO 2 N, NO 3 N, PO3 P and SO2 S were determined by ion chromatography using a Yokogawa IC 7 Series II analyzer (Yokogawa Analytical Systems), attached to an Excelpak ICS A23 column. The ammonium, Mg 2+, and Ca 2+ concentrations were deter- Fig. 1. Reactor for denitrification and phosphate removal using the granular medium.

3 Y. Tanaka et al. / Bioresource Technology 98 (27) mined by ion chromatography using a Dionex DX 12 analyzer attached to an IonPac CS12A column. Total phosphorus (TP) was measured using a flow injection analyzer (Sanuki Engineering Co., Ltd.). In this system, phosphorus compounds were oxidized to phosphate by heating at 12 C for 3 min after adding potassium-persulfate solution. Ammonium molybdate, potassium antimonyl tartrate acidic solution and ascorbic acid solution were then added in succession, and absorbancy at 88 nm was measured. 3. Results and discussion The novel medium developed in this study consisted of porous perlite particles as inert nuclei and a sulfur matrix outer layer in which powdered CaCO 3 and Mg(OH) 2 were embedded. The purpose of adding Mg(OH) 2 in addition to CaCO 3 was to add phosphorus removal ability to the medium. It was hypothesized that this medium would have the following advantages: (1) since CaCO 3 and Mg(OH) 2 were homogeneously dispersed in the sulfur matrix, their dissociation would proceed simultaneously with sulfur oxidation; (2) the spherical shape of the medium would be an advantageous characteristic for filtration processes since it might homogenize flow-velocity distribution in the medium bed and minimize headloss; (3) expansion and fluidization of the medium bed would be easy during backwashing due to the lower density and smaller diameter (1.5 5 mm) of the medium; and () Mg(OH) 2 may contribute to PO 3 P removal by establishing a weak alkaline condition that would enhance the crystalline reaction of phosphate with calcium and/or magnesium. Table 1 shows the water quality (ph, BOD, TN, NH þ, TP, Mg 2+,Ca 2+ and SO 2 ) of the influent and effluent. The ranges of ph values were and for the influent and effluent, respectively. In conventional SLAD systems, in which CaCO 3 was the sole neutralization agent, effluent ph generally declined due to the generation of sulfate (Flere and Zhang, 1999; Kawaharazuka et al., 21). The dissociation of Mg(OH) 2 in addition to CaCO 3 may contributed to the increase of effluent ph in the present experiment. The total nitrogen decreased from mg/l in the influent to mg/l in the effluent Table 1 Water qualities of the influent and effluent ave. (MIN. MAX., SD) ave. (MIN. MAX., SD) ph BOD (mg/l) 59.1 ( , 86.5) 5.5 ( , 58.7) NH þ N (mg/l) 59.6 ( , 29.3) 52.2 ( , 27.3) TN (mg/l) ( ,.9) 1. ( , 35.1) TP (mg/l) 32.3 (1. 9.1, 1.7) 22.2 ( , 12.) Ma 2+ (mg/l) 7. ( , 16.8) 18. ( , 33.6) Ca 2+ (mg/l) 63.7 ( , 15.5) 59.9 ( , 15.5) S (mg/l) 17.8 ( , 3.) 93.6 ( , 53.7) SO 2 (Table 1). Ammonium also decreased 12.% by the treatment (Table 1). Fig. 2 shows the changes in the concentrations of NO 3 N and NO 2 N. The removal of NO 3 N was efficient throughout the experimental period. On the other hand, NO 2 N increased by treatment during days 1 and 12, probably due to the incomplete reduction of nitrate. Fig. 3a shows the relationship between the loading rate of NO x N and the removal efficiency of NO x N. High removal efficiency exceeding 7% could be obtained when the loading rate was less than approximately.3 kg N m 3 d 1, while the efficiency dropped when the loading rate exceeded this value. As shown in Fig. 3b, the accumulation of NO 2 N became prominent at a NO x N loading rate of more than approximately.35 kg N m 3 d 1 (.3 g N kg 1 d 1 ). This indicates that NO 2 N accumulation was the cause of the drop in the NO x N removal efficiency at higher NO x N loading rates. Kawaharazuka et al. (21) also reported that NO 2 N accumulation occurred when the NO 3 N loading rate exceeded.2 g kg 1 d 1. According to van der Hoek et al. (1992a,b), the maximum NO 3 N loading rate should be.217 kg NO 3 Nm 3 d 1 to achieve the highest removal efficiency. Flere and Zhang (1999) pointed out that the maximum removal efficiency of nitrate was achieved at a loading rate of kg NO 3 Nm 3 d 1 for the treatment of groundwater by granular elemental sulfur and limestone ( mm diameter). Similar nitrate loading rates, kg NO 3 Nm 3 d 1, were also - - NO 3 N (mg/l) (a) NO 2 N (mg/l) Time (days) Fig. 2. Changes in NO 3 N and NO 2 N of the influent and effluent during the experimental period.

4 - 79 Y. Tanaka et al. / Bioresource Technology 98 (27) N removal efficiency (%) NO x - (a) ΔNO 2 -N (kg.m -3.d -1 ) kgno x -N-m -3.d -1 Fig. 3. Influence of NO x N loading rate on NO x N removal and NO 2 N accumulation. adopted in autotrophic denitrification using hydrogen sulfide as the electron donor (Vaiopoulou et al., 25), while Kleerebezem and Mendez (21) have reported higher volumetric treatment capacities (less than 1 kg NO 3 Nm 3 d 1 ) using hydrogen sulfide. These reports and the present results suggest that approximately.2.3 kg NO 3 Nm 3 d 1 is an optimum loading rate for denitrification by the sulfur oxidizing bacteria. A stable SO 2 S concentration of about 2 3 mg/l was observed for the influent (Table 1). In contrast, the effluent SO 2 S concentration changed considerably with the influent nitrate concentration. As shown in Fig., good correlation was observed between the decrease in NO x N (DNO x N) and the increase in SO2 S(DSO2 S). This correlation indicates that the sulfur consumption for denitrification was about 2.5 kg sulfur per 1 kg denitrified nitrogen. This means 7.5 kg SO 2 was produced by 1 kg NO 3 N denitrification. This SO 2 production value is close to the theoretical value of 7.53 calculated by the equation of Zhang and Lampe (1999), and to experimental values of 7.89 (Koenig and Liu, 1996) and 7.6 (Flere and Zhang, 1999). The average concentration of TP decreased from 32.3 to 22.2 mg/l by the treatment (Table 1), though the effluent TP fluctuated considerably, probably due to temporary leaks of accumulated insoluble phosphorus from the medium bed. As shown in Fig. 5, the concentrations of PO 3 P decreased significantly by treatment until about day 2, while the removal activity almost disappeared thereafter. Slightly soluble Mg(OH) 2 powder (1 lm in diameter) that was of the same quality as that used for the preparation of the medium was added to the medium bed seven times during days 68 8 (total weight of 3 g) to evaluate the contribution of Mg(OH) 2 to PO 3 P removal. The removal activity increased significantly after about day 7. This would suggest the important contribution of Mg(OH) 2 to phosphate removal. Raising the Mg(OH) 2 content in the medium would be effective for maintaining phosphate removal activity beyond about 2 days. Fig. 6a shows the relationship between effluent ph and the PO 3 P removal rate. The removal rate increased when the effluent ph exceeded 7.9. The Mg 2+ concentrations in the effluent also dropped significantly when the effluent ph exceeded 7.9 (Fig. 6b). As shown in Fig. 7, positive correlation was observed between the removal rates of NH þ and PO 3, though plots varied widely. The crystalline reactions of PO 3,Mg2+ and NH þ with a molar ratio of about 1:1:1 (MAP reaction) would have occurred under alkaline conditions. During the treatment with the reactor, the headloss of the medium bed increased gradually, probably due to the accumulation of microbes, suspended solids, and formed crystalline materials. Backwashing was carried out on days 17, 25, 52, 61, 16 and 221. The headloss was restored to the original value after each backwashing. Periodic backwashing is indispensable for maintaining the treatment performance of this process. It may also be effective for the ΔSO -S (mg/l) y = 2.536x R 2 = Fig.. Relationship between NO x - ΔNO x -N (mg/l) N decrease and SO2 S increase. PO 3- -P (mg/l) Time (days) Fig. 5. Changes in PO 3 P in the influent and effluent during the experimental period.

5 Y. Tanaka et al. / Bioresource Technology 98 (27) Concentration in effluent (mg/l) PO -P removal rate (kg.m -3.d -1 ).2.1 (a) Mg 2+ Ca ph Fig. 6. Influence of effluent ph on the PO 3 P removal rate and on the effluent Mg 2+ and Ca 2+ concentrations. Mole NH -N.m -3.d Mole PO 3- -P.m -3.day -1 Fig. 7. Relationship between the PO 3 P and NHþ N removal rates. release of trapped nitrogen bubbles formed within the medium bed, which cause short-circuiting and a decrease in nitrate removal efficiency. The necessity for periodical backwashing in conventional SLAD systems has been emphasized by Flere and Zhang (1999). The coated matrix layer of the medium might worn out during prolonged use. The remaining perlite particles could be removed from the reactor selectively by the backwashing process, due to their smaller particle diameter and lower density compared to the coated medium. Perlite removed from the reactor could be reused as a material for maintaining moisture content in crop land soil, or as a bulking agent for the composting of livestock wastes.. Conclusions The present study demonstrated that a medium consisting of perlite, sulfur, CaCO 3 and Mg(OH) 2 was useful for the removal of both nitrate and phosphate. The loading rate of nitrate should not exceed.3 kg NO 3 Nm 3 d 1 to ensure high nitrate removal efficiency. The effluent ph should be above 7.9 to remove phosphate. Evidently Mg(OH) 2 contributed strongly to the phosphate removal, and that raising the Mg(OH) 2 content in the medium effectively extended the life of the medium for phosphate removal. Acknowledgement We wish to thank Ms. Keiko Sumiya, for her skillful technical assistance. References Flere, J.M., Zhang, T.C., Nitrate removal with sulfur limestone autotrophic denitrification processes. Journal of Environmental Engineering 125, Kawaharazuka, T., Yatagai, A., Masujima, H., 21. Denitrification of underdrainage by granulated sulfur limestone mixture. Journal of Agricultural Science, Tokyo Nogyo Daigaku 6 (1), 7 12 (in Japanese). Kleerebezem, R., Mendez, R., 21. Autotrophic denitrification for combined hydrogen sulfide removal from biogas and post-denitrification. In: Ninth World Congress Anaerobic Digestion Proceedings Part 1, Antwerpen-Belgium, September 2 6, Koenig, A., Liu, L.H., Autotrophic denitrification of landfill leachate using elemental sulfur. Water Science and Technology 3 (5 6), Vaiopoulou, E., Melidis, P., Aivasidis, A., 25. Sulfide removal in wastewater from petrochemical industries by autotrophic denitrification. Water Research 39, van der Hoek, J.P., Hijnen, W.A.M., van Bennekom, C.A., Mijnarends, B.J., 1992a. Optimization of the sulphur limestone filtration process for nitrate removal from groundwater. Journal of Water SRT-Aqua 1, van der Hoek, J.P., Kappelhof, J.W.N.M., Hijnen, W.A.M., 1992b. Biological nitrate removal from ground water by sulphur/limestone denitrification. Journal of Chemical Technology and Biotechnology 5, Zhang, T.C., Lampe, D.G., Sulfur:limestone autotrophic denitrification processes for treatment of nitrate-contaminated water: Batch experiments. Water Research 33,

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