The pulp and paper industry produces a large quantity of wastewater containing recalcitrant organic compounds. In this study, a pilot ‐ scale anaerobic–aerobic sequential system was employed to treat four different waste streams produced in a kraft pulp and paper mill. The system consisted of a 2.3 m3 packed ‐ bed anaerobic digester and a completely mixed activated sludge process. Under the applied organic loading rate to the anaerobic digester (0.2 to 4.8 kg ‐ COD m−3 d−1), a COD removal efficiency of 50–65% was achieved. After the anaerobic treatment, the BOD/COD ratio of the effluent was low (0.12 ± 0.03), suggesting that additional pretreatment is necessary for the digester effluent to be further polished aerobically. Combined with the aerobic treatment, the overall COD removal efficiency was up to 70% for the substrates evaluated. Air purging before feeding sulfide ‐ containing substrate was shown to be effective for removing sulfide toxicity in the digester. Kinetic analysis showed that the pseudo ‐ first ‐ order degradation rate constants of the evaluated substrates are 0.28–0.46 d−1 in the anaerobic digester, with a methane production yield of 0.22–0.34 m3 ‐ CH4 kg ‐ COD−1 at standard temperature and pressure (0°C, 1 atm). These values are comparable to those found for other industrial substrates, indicating that an anaerobic process is a sound treatment alternative for the evaluated waste streams. The quality of biogas produced by the substrates was excellent, containing ∼80% of methane. The application of anaerobic treatment has the potential of significantly improving the energy footprint of the pulp and paper industry. © 2013 American Institute of Chemical Engineers Environ Prog, 33: 359–368, 2014
anaerobic digestion; biogas production; activated sludge; biological treatment; pulp and paper wastewater
Pulp and paper industry produces a large quantity of wastewater of high organic strength [
Treatment of bleaching effluents typically incorporates primary clarification followed by a secondary biological treatment [
Anaerobic treatment, although widely used for treating agricultural and municipal wastes [
In this study, the treatability of the liquid wastes from a kraft paper mill was evaluated using a pilot ‐ scale, sequential bioreactor system consisting of an anaerobic and an aerobic process. The liquid wastes included streams produced from chlorine dioxide (CD) bleaching, from alkaline extraction reinforced with oxygen and peroxide (EOP) bleaching, from chemical (sulfate) pulping (so ‐ called foul condensates, FC), and from dewatering operation of plant wasted sludge (screw press liquor, SPL). For improving the digestibility and pH adjustment, a small volume of wasted sugar water (SW) from a food processing plant was blended as a co ‐ digestion substrate. We report the treatment performance, biogas production efficacy of each substrate and system characteristics of the pilot ‐ scale operation.
The schematic of the pilot ‐ scale treatment system is presented in Figure [NaN] . It consists of an equalization tank (2.1 m
The CD/EOP/FC/SPL streams were obtained twice a week from the mill in 0.76 m
The evaluation lasted for 156 days (from October 31, 2011 to April 3, 2012) and was divided into six periods according to different feeds and operating conditions. Initially, the packed bed column was operated as a downflow digester using a flow scheme similar to a trickling filter, with a space loading rate of ∼3 kg ‐ COD d
Pilot ‐ scale feeding activities and operating conditions during the six evaluation periods
Operating periods 1 2 3 4 5 6 Duration (days) 1–36 45–81 82–135 136–142 143–148 149–156 Substrate FC+SW EOP+SW EOP+SW EOP+CD+SW EOP+CD EOP+CD+SPL Flow scheme Downflow Downflow Upflow Upflow Upflow Upflow OLR (kg ‐ COD m−3 d−1) 2.96 ± 0.70 3.02 ± 0.38 2.25 ± 0.81 2.75 ± 0.70 1.59 ± 0.48 1.44 ± 0.48 HRT (d) — — 2.44 ± 0.83 1.72 ± 0.51 2.12 ± 0.91 1.82 ± 0.55 pH in digester 6.92 ± 0.39 7.23 ± 0.11 7.42 ± 0.10 7.60 ± 0.48 7.25 ± 0.02 7.26 ± 0.09 Temperature of effluent (°C) 32.7 ± 2.6 34.3 ± 1.6 31.5 ± 3.1 34.5 ± 1.6 32.2 ± 1.8 33.3 ± 0.9
1 The system was in the recovery mode during Days 37–44 (see Results and Discussion for details).
- 2 *Based on the volume of packing media.
- 3 Based on total volume of the packed ‐ bed digester.
Daily liquid samples were taken from six sampling points (1–6) for chemical analysis, and gas samples were taken from sampling point (
Analytical parameters and frequency for each sampling point in the pilot ‐ scale system
Sampling points Anaerobic digester (1–3) ASP (4–6) Biogas (7) 1 2 3 4 5 6 7 Sampling point Balance tank Predigestion tank Anaerobic digester Aeration tank Recycled sludge line Final effluent Biogas exit Frequency Daily Daily Daily Daily Daily Daily Four times a day Analyzed Parameters pH, T, COD, VFA pH, T, DO, ORP, TN, TP, VFA, BOD5 pH, T, DO, ORP, TN, TP, VFA, ALK, BOD5 pH, T, DO, TS, VS, TSS, VSS, BOD5,COD pH, T, TS, VS, TSS, VSS, COD pH, T, DO, COD, AN, TP, turbidity Volume and composition biogas
- 4 DO, dissolved oxygen; N, ammonium nitrogen; ORP, oxidation–reduction potential; T, temperature; TN, total nitrogen; TP, total phosphorus; TS, total solids; TSS, total suspended solids; VFA, volatile fatty acids; VS, volatile solids; VSS, volatile suspended solids.
- 5 Two samples weekly.
The characteristics of the evaluated waste streams are summarized in Table [NaN] . The COD concentrations range from 2500 to 4800 mg L
Initial characteristics of the evaluated waste streams from the paper mill
Parameter Foul condensate (n = 11) CD filtrate (n = 8) EOP filtrate (n = 4) Screw press liquor (n = 13) COD (mg L−1) 2973 ± 142 2886 ± 381 3901 ± 1940 4498 ± 2020 dCOD (mg L−1) 2740 2445 ± 151 2890 609 ± 189 TS (mg L−1) 406 ± 104 4718 ± 522 4744 ± 532 8768 ± 7957 VS (mg L−1) 210 ± 14 2497 ± 346 1903 ± 136 3742 ± 1666 VS/TS Ratio 0.53 ± 0.1 0.53 ± 0.02 0.4 ± 0.02 0.5 ± 0.1 TSS (mg L−1) 357 ± 577 868 ± 365 388 ± 127 4048 ± 1750 VSS (mg L−1) 339 ± 461 758 ± 339 296 ± 204 1997 ± 875 TSS/VSS Ratio 0.83 ± 0.25 0.86 ± 0.04 0.79 ± 0.23 0.49 ± 0.06 Alkalinity (mg L−1 as CaCO3) 205 ± 50 — 915 ± 263 — pH 9.28 ± 0.18 5.19 ± 1.04 9.29 ± 0.29 8.44 ± 0.83 TN (mg L−1) 52.2 ± 4 4 ± 1.3 27 ± 43.3 2.3 ± 0.1 TP (mg L−1) 0.24 ± 0.09 6.33 ± 0.18 3.98 ± 5.22 0.41 ± 0.04 Conductivity (ms cm−1) 5 ± 5.7 — 14.6 ± 0.4 — Sulfide (mg L−1) 52.2 ± 18.1 <0.5 <0.5 — Sulfate (mg L−1) <40 — 106 ± 23 — Chloride (mg L−1) — — 335 ± 39 —
- 6 n is the number of waste stream samples analyzed.
- 7 dCOD is the dissolved COD concentration, which represents the organic load excluding the contribution from suspended solids.
The operating parameters and performance of the packed bed digester for each of the six periods (Table [NaN] ) are summarized in Table [NaN] . For comparison, the typical values for liquid digesters are also listed. The low DO concentration (near detection limit of the DO probe) and ORP value (<−200 mV) indicate that the system was strictly anaerobic. VFA concentration was lower than 350 mg L
Summary of chemical characteristics in the anaerobic digester and the digestion performance
Operating periods 1 2 3 4 5 6 Typical values DO (mg L−1) 0.10 ± 0.06 0.05 ± 0.0 0.13 ± 0.09 0.16 ± 0.05 0.12 ± 0.07 0.12 ± 0.06 — ORP (mV) 345 ± 13 361 ± 4 282 ± 33 276 ± 39 205 ± 52 272 ± 14 −420 to −200 33 TN (mg L−1) 54.5 ± 12.0 8.9 ± 1.7 12.3 ± 4.7 14.7 ± 2.2 12.9 ± 2.4 14.3 ± 1.5 40–70 34 TP (mg L−1) 2.6 ± 0.9 4.1 ± 0.1 4.1 ± 1.0 6.0 ± 1.3 5.7 ± 0.2 5.6 ± 0.2 8–15 34 Alkalinity (mg L−1 as CaCO3) 484 ± 165 1845 ± 148 2548 ± 160 2456 ± 181 1830 ± 32 1423 ± 55 1500–5000 35 , 36 VFA (mg L−1 as HAc) 291 ± 162 1028 ± 94 350 ± 39 326 ± 49 274 ± 5 221 ± 28 <1800 33 COD removal (%) 58.8 ± 18.6 25.9 ± 9.9 56.2 ± 5.4 57.4 ± 4.5 46.1 ± 8.2 41.0 ± 5.4 — CH4 content (%) 83.4 ± 1.4 81.1 ± 0.7 81.4 ± 1.7 82.2 ± 0.7 78.7 ± 1.3 85.0 ± 2.0 50–75 37 CO2 content (%) 16.4 ± 1.4 18.5 ± 0.1 18.3 ± 1.8 17.5 ± 0.6 20.7 ± 1.9 14.2 ± 1.3 — H2S content (ppm) >5000 3600 ± 430 751 ± 488 671 ± 133 649 ± 498 555 ± 223 — CH4 yield (m3 ‐ CH4 kg ‐ COD−1) 0.283 0.284 0.219 0.296 0.318 0.338 0.25–0.4 37
Figure [NaN] shows the time series plots of substrate COD concentration entering the digester, the biogas production and gas quality (Figure [NaN] a) and COD removal (Figure [NaN] b). The vertical dash lines divide the operational periods as indicated in Table [NaN] . Even with the equalization of the substrate, the organic strength of incoming waste streams still had a moderate variability, with COD concentrations from 3000 to 5000 mg L
From Days 32 to 37 (before switching the substrate to EOP), the air purging was stopped to observe if sulfide stripping played an important role in the treatment of FC. Immediately after stopping the air purging, the H
During the first two periods (Table [NaN] ), FC was more readily treated in the packed bed digester compared to EOP because FC contains low molecular weight organic compounds (lower ‐ carbon fatty acids, methanol, and dimethyl sulfide) [
From Day 45–81, EOP was fed as the primary substrate and the digester was reseeded in the same fashion as the initial seeding (0.19 m
In an attempt to improve the treatment performance, the flow scheme of the digester was modified from the downflow anaerobic trickling filter to upflow flooded bed digester on Day 82 (Table [NaN] ). The change of feed flow scheme greatly improved the biodegradation (Figure [NaN] a). Both the COD removal and biogas production increased continuously over the next 7 days. During Days 82–135, the mean COD removal was 56.2% ± 5.4% (peaked at >70%). The mean biogas production was 1.1 ± 0.35 m
On Day 136, CD was blended as a co ‐ substrate at 50:50 volume ratio (Table [NaN] , the fourth period). Due to the lower pH of the CD (Table [NaN] ), the SW was not supplemented for pH adjustment (Table [NaN] , the fifth period). Finally, SPL was fed with a volume ratio of SPL:EOP:CD at 20:40:40 (Table [NaN] , the sixth period). During these three periods, the incoming COD had a decreasing trend because of the substantially lower dissolved COD (dCOD) of the SPL and CD (Table [NaN] ) and the exclusion of the waste sugar water as the co ‐ substrate. This led to a decrease of gas production rate. Nevertheless, with the decreased COD removal efficiency, the biogas yield was increased (Table [NaN] ) and the biogas quality in terms of CH
Figure [NaN] shows the scattered plot between the COD removal and organic loading rate (OLR). The COD removal efficiency was not significantly affected by varying the OLR, resulting in a linear increase of COD mass removal with respect to the applied OLR (Figure [NaN] ). This suggests that the system should have a greater treatment capacity than the OLR range applied during the evaluation period. There are a few data points that deviated from the main cluster in the scatter plot. The data points represent the period when VFA accumulation and potential H
To estimate the methane production yield of the evaluated substrates, the cumulative CH
Comparison of reported anaerobic degradation rate constants, methane yields, substrate concentrations, and methane contents
Substrates Reactor Substrate utilization rate (d−1) CH4 yield (m3 ‐ CH4 kg ‐ COD−1) Concentration range (mg L−1 COD) CH4 content (%) Ref. FC+SW Downflow PBR — 0.283 2880–5360 83.4 ± 1.4 This study EOP+SW Upflow PBR 0.302 0.219 3850–7060 81.4 ± 1.7 EOP+CD+SW Upflow PBR 0.461 0.296 4100–6140 82.2 ± 0.7 EOP+CD Upflow PBR 0.314 0.318 3230–4220 78.7 ± 1.3 EOP+SPL Upflow PBR 0.279 0.338 2020–2810 85.0 ± 2.0 Kraft evaporator condensate Submerged MBR — 0.35 ± 0.05 — 80–90 43 Peroxide bleached pulping effluent UASB — 0.35–0.4 — — 44 Linerboard mill wastewater UASB — 0.151–0.455 1285–6055 80–85 45 Slaughterhouse wastewater Fluidized bed reactor 1.2 — — — 46 Fruit ‐ processing wastewater Immobilizedcell bioreactor 0.89 0.27 5100 — 47 Palm oil mill effluent Anaerobic pond 0.36 — — — 48 Palm oil mill effluent Upflow sludge fixed film reactor — 0.287–0.348 5260 55 49 Palm oil mill effluent Anaerobic baffled reactor — 0.38 16,000 67–71 50 Soluble fraction in olive mill solid residue CSTR 0.145 — 3200–15,100 — 42
8 The degradation kinetics cannot be assessed using pseudo ‐ first ‐ order kinetics because of the downflow PBR configuration.
Kinetic analysis was performed to estimate the rate of substrate degradation. Given the concentrations measured in this pilot ‐ scale study, a pseudo ‐ first ‐ order kinetic law was applied. Similar approaches were also utilized in earlier studies [
C=C0e(−kθ)
where C
Compared to the methane yields and first ‐ order degradation rate constants reported for other liquid substrates using different reactors (k = 0.15–1.2 d
Starting from the third operating period, the ASP system was initiated for polishing the effluent from the anaerobic digester. The aeration tank was seeded with 0.76 m
The performance of the ASP system is shown in Figure [NaN] . During the third period (before Day 142), the influent to the aeration tank had a BOD concentration of 218 ± 61 mg L
In this study, we evaluated the treatability of the four waste streams from the pulp and paper industry in a pilot plant consisting of a packed bed anaerobic digester and an activated sludge process. It was found that all waste streams are readily treatable. The anaerobic treatment removed 50–65% of substrate COD. Coupled with the aerobic treatment using a completely mixed activated sludge process, the overall COD removal efficiency was 55–70%. Kinetic analysis showed that the pseudo ‐ first ‐ order degradation rate constants of the evaluated substrates in the digester are in the range of 0.28–0.46 d
During the pilot plant study, the packed bed was operated as an anaerobic trickling filter and as an upflow flooded anaerobic digester. For the waste stream produced by the bleaching process (EOP), the upflow configuration yielded a better treatment performance in terms of COD removal. For substrate containing moderately high sulfide concentration (FC), air stripping before feeding the substrate into the liquid digester effectively removed sulfide toxicity in the digester. The biogas quality produced by the substrates was excellent, containing ∼80% methane. After the anaerobic treatment, the BOD/COD ratio of the effluent was low (0.12 ± 0.03). This suggests that additional pretreatment is required for the effluent to be further treated aerobically.
ALK total alkalinity
AN ammonia nitrogen
ASP activated sludge process
BOD 5 5 ‐ day biochemical oxygen demand
CD waste stream from Chlorine Dioxide bleaching process
COD chemical oxygen demand
CSTR continuous stirred tank reactor
EOP waste stream from alkaline Extraction and Oxygen & Peroxide bleaching process
EPA Environmental Protection Agency
FC Foul Condensate, a waste stream from chemical pulping process
HRT hydraulic retention time
OLR organic loading rate
ORP oxidation reduction potential
PBR packed bed reactor
SPL screw press liquor, a waste stream from paper sludge dewatering process
STP standard temperature and pressure (0°C, 1 atmosphere)
SW sugar water, a waste stream from a food processing plant
TKN Total Kjeldahl Nitrogen
TN total nitrogen
TP total phosphorous
TS total solids
TSS total suspended solids
UASB upflow anaerobic sludge blanket reactor
VFA volatile fatty acids
VS volatile solids
VSS volatile suspended solids
This study was supported by MeadWestvaco Evadale TX facility (Project No: MWV0001). The authors would like to thank Dipendra Wagle, Sophia Yang, Yolanda Wang, Brandon Corace, and Erik Corace for their assistance in the field operation and laboratory analysis. The assistance of Gary Colson, Michael Clapper, and Robert Sasser in supporting this work and in obtaining waste streams is greatly appreciated. The administrative assistance of Stewart Cairns, Reid Sweet, and Thomas Sitton are also acknowledged.
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Graph: (a) Schematic diagram of the pilot ‐ scale treatment system. The system is a functional design with transfer pumps for flow transport. Points #1 to #6 are the liquid sampling locations and Point #7 is the gas sampling location. (b) Photo of anaerobic section. (c) Photo of the aerobic section. [Color figure can be viewed in the online issue, which is available at wileyonlinelibrary.com.]
Graph: Biogas production and COD removal of the anaerobic digester: (a) daily biogas production and major gas components (CH 4 and CO 2 ), and (b) feeding COD concentration and COD removal efficiency. Details of the six operational periods are shown in Table . “M” denotes the maintenance and recovery period.
Graph: Results of laboratory air stripping experiments for a foul condensate sample. After 2 h of stripping, the COD concentration decreased by 26%, and sulfide concentration decreased from 75 mg L −1 to 1 mg L −1.
Graph: Scatter plots between organic loading rate and COD mass removal. Data points in the circled area are those recorded when H 2 S toxicity occurred during the period "M" in Figure .
Graph: Cumulative CH 4 production (at standard temperature and pressure) and cumulative COD mass digested during the evaluation period. There are six linear periods (Table ) during which the data were used for calculating the methane yield.
Graph: Performance of the aerobic treatment as a polishing step for the digester effluent. After the treatment, BOD/COD ration was consistently low.
By Che ‐ Jen Lin; Pengchong Zhang; Pruek Pongprueksa; James Liu; Simon A. Evers and Peter Hart