Water Air Soil Pollut (2010) 208:323333 DOI 10.

1007/s11270-009-0170-1

Hydrogenated Vegetable Oil Industry Wastewater Treatment using UASB Reactor System with Recourse to Energy Recovery
Sunita Shastry & Tapas Nandy & S. R. Wate & S. N. Kaul

Received: 24 April 2009 / Accepted: 23 July 2009 / Published online: 23 August 2009 # Springer Science + Business Media B.V. 2009

Abstract The investigation was carried out on laboratory scale to assess the feasibility of upflow anaerobic sludge blanket reactor system as a pretreatment for hydrogenated vegetable oil industry wastewater with recourse to energy recovery. The reactor system operated at 35C, resulted in COD removal efficiency in the range 98.980.1% at organic loading varying in the range 1.3310 kgCOD/m3 day. The specific methane yield varied from 0.295 0.345 m3CH4/kgCODr. Hydraulic retention time, substrate concentrations, pH, and temperature were also varied to study the influence of operating parameters on reactor performance. The methane content decreased with increase in substrate loading rate, and varied from 5366.7% under varying operating conditions. Impulse loading studies in terms of hydraulic, organic, and pH though resulted in destabilization of the reactor; however, the reactor rapidly achieved stable performance after steady operation.

Keywords Hydrogenated vegetable oil . Wastewater . Anaerobic . UASB . Startup . Biogas . Methane . Reactor performance . Shock loading

1 Introduction Hydrogenated vegetable oil, a substitute for butter oil, is extensively used in India. It forms a dietary supplement among all categories of population. The vegetable oil industry generally falls under small to medium scale though quite a few large scale industries also exist. However, due to strict legislation for protection of environment, it is imperative to arrive at appropriate treatment technology for the wastewater emanating from this industry. The medium strength wastewater generated from hydrogenated vegetable oil industry is highly alkaline and distinguishes itself because of its high fatty material content. Approach involving aerobic biological process alone or in combination with physicochemical treatment alternatives involves high capital investments, requires skilled manpower in addition to being energy intensive. In comparison, anaerobic treatment system involves low investment, omitting aeration equipment, sludge disposal facility, and recirculation and provides biogas as a fuel substitute (Path et al. 1988; Kaul and Nandy 1993; Mahmoud et al. 2008), and therefore, the system is a more viable alternative as a pretreatment facility.

S. Shastry (*) : T. Nandy : S. R. Wate National Environmental Engineering Research Institute, Nagpur, India e-mail: [email protected] S. N. Kaul MIT College of Engineering, Paud Road, Kothrud, Pune, India

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In line with anaerobic processes, the upflow anaerobic sludge blanket (UASB) reactor system has emerged as a successful low investment technology (Kotsopoulos et al. 2006; Kyazze et al. 2008; Ganesh et al. 2007; Elmitwalli et al. 2007). Researches and full scale application have demonstrated the utility of UASB technology in methane recovery system for varied substrate (Lettinga et al. 1980, 1982, 1984; Pathe et al. 1995; Seghezzo et al. 1998; Uemura and Harada 2000; Ghangrekar et al. 2002; Lew et al. 2004; Show et al. 2004). The treatment technology is a viable option due to biomass retention achieved through granulation process, and inherent simplicity allows economic application as a pretreatment facility (El-Gohary et al 2008). Accordingly, the viability of upflow anaerobic sludge blanket reactor system as a pretreatment facility with recourse to methane recovery from hydrogenated vegetable oil industry wastewater has been investigated on laboratory scale in this study. Impact of hydraulic and organic overloading, shock loadings in terms of pH and starvation on reactor performance have also been investigated and presented.

addition to a scum breaker incorporated within the GSS, was used for breaking the scum. Biogas was collected in aspirated bottle through liquid displacement technique. The treated effluent pipe was connected to inverted siphon to prevent escape of biogas from the liquid by maintaining liquid seal. The temperature probe was inserted at mid-depth of the reactor column. The pH electrodes were fitted inside the feed tank as well as in the effluent line for monitoring. The schematic of the reactor assembly is presented in Fig. 1. 2.2 Hydrogenated Vegetable Oil Industry Details The studies were carried out using hydrogenated oil industry wastewater obtained from a factory located in Central India. The daily production of hydrogenated oil is 2030 tonnes using soyabean, rice bran, cottonseed, and rapeseed oil either alone or in combination. Caustic soda, phosphoric acid, bleaching earth, common salt, citric acid, and nickel catalyst are the other raw materials used in the process. The oil refining process consists of degumming to recover phosphatides (gums) that can be processed to make lecithin since oils contain appreciable quantity of gums or mucilages. The following reactions are involved in degumming and alkali refining: Phosphatides + water hydrated gums Phospholipids + acid/alkali hydrated gums Calcium/magnesium + phosphate insoluble phosphates Free fatty acids + alkali soaps The neutralization treatment to oil consists of addition of alkali (814.6% NaOH) to neutralize free fatty acids in the raw oil and form soaps thereby resulting in amount of free fatty acids of 0.010.03%. Pigment dissolved in the oil is removed by bleaching using bleaching earth. Hydrogenation step involves addition of molecular hydrogen obtained by electrolysis to unsaturated compounds in the presence of nickel catalyst (chemical change of the glyceride molecule causes hardening). Hydrogen addition destroys the odor of natural fat or oil completely and makes the oil whiter. The hardened oil becomes resistant to rancidity. Deodorization is carried out by steam stripping under vacuum, to remove volatile fraction of organics

2 Materials and Methods 2.1 Upflow Anaerobic Sludge Blanket Reactor The laboratory model reactor was fabricated using perplex glass column. The reactor dimensions comprised of 220 mm diameter and 1,300 mm depth with total holding capacity of 0.05 m3. The dimensions of reactor system were chosen considering the amount of wastewater to be treated and the maximum permissible surface load, which roughly dictates the height area ratio of the reactor. The feed inlet system consisted of a perforated base plate provided to ensure uniform feed distribution through the reactor. Deflection plates inclined at 45 were provided to prevent escape of biogas into settling zone. Gas solid liquid separator (GSS) was provided as described elsewhere (Lettinga et al. 1980). The three phase separator was fixed at height of about 800 mm from bottom. The inclination of separator wall was 50 from the horizontal. Outlet weir was provided with Vnotch above the settling zone for effluent collection using perplex glass to ensure uniform outlet flow from the system. A gas recirculation pump, in

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Fig. 1 Experimental set-up of UASB reactor used for the study

causing odor. According to the specification issued by Department of Food, New Delhi, India (CPCB 1994) compulsory incorporation of 700 IU of Vitamin A per ounce is necessary. The hydrogenated oil must conform to the following requirements: & & & & & & & Maximum moisture content fixed at 0.25% Maximum unsaponifiable matter at 1.5% Free fatty acids not to exceed 0.25% Melting point between 31C and 37C with a tolerance of 2C on either side B.R. Reading at 40C, not less than 48 As identifying substances, compulsory addition of 5% of refined or refined hydrogenated sesame oil Boudin test, not less than 3.0 red

&

Fortification with synthetic vitamin A, not less than 25 IU per gram (1 IU of Vitamins A and D corresponds to 0.344 and 0.025m, respectively).

2.3 Wastewater Characteristics Wastewater samples were collected from the collection tank of the industry under study for conducting the experiments. Physico-chemical characteristics of the wastewater used during experimental study are presented in Table 1. The characteristics of wastewater indicate highly alkaline pH (10.811.3). The BOD/COD ratio of 0.410.43 indicates biodegradable nature of wastewa-

326 Table 1 Physico-chemical characteristics of wastewater used for study S.No. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. Parameters Temperature, C pH Alkalinity Suspended solids Total dissolved solids BOD COD Total fatty matter Total kjeldhal nitrogen Phosphates Nickel Zinc Concentration (range) 4148 10.811.3 3,7504,180 1,5001,900 5,8706,310 1,6503,400 3,8508,290 1,3801,650 17.218.8 50.560.8 0.460.52 1.161.20

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All values except pH and temperature are in mg L1

continuous feeding was initiated maintaining organic loading rate (OLR) of 0.5 kgCOD m3 day1. Wastewater was fed to the reactor using Watson Marlo peristaltic pump for flow control. The wastewater was fed after pH adjustment using 1 N dilute sulphuric acid to near neutral. Sufficient upflow velocity was maintained to achieve proper fluidization and mixing of sludge granules inside the reactor. The OLR applied at the end of startup period was 1 kgCOD m3 day1. After development of sludge bed and blanket zone, experimental studies were carried out by varying detention period from 3 to 0.33 days and concentration of substrate from 4,000 to 8,000 mg/l. The OLR was increased to the next level only after pseudo steady state was reached, as indicated by stable gas production rate (10%) and effluent COD concentration (5%). The experiments were carried out at temperature 352C. 2.5 Method of Analysis

ter with concentration of total fatty matter in the range 1,3801,650 mg/L making it amenable to biological treatment. Phosphorous was adequate considering the nutrient requirement of 100:2.5:0.5 for BOD:N:P; however, external addition of nitrogen source was essential. 2.4 Reactor Startup The reactor was seeded with sludge collected from the holding tank provided within the industry premises. In addition, slimy layer of microbial culture attached to soil and acclimatized to the oily wastewater from the vicinity of effluent discharge site of the industry was also added. The characteristics of seed sludge used in the study are given in Table 2. Initially during startup, the reactor was operated on batch mode and the reactor was monitored for gas production. Later

The parameters monitored were inlet and outlet pH, VSS, alkalinity, biogas composition, and COD and flow rate to the reactor system. The inlet and outlet sample was collected hourly and composited for 12 h and analyzed for various parameters. Biomass was periodically collected from the sampling ports along the height of reactor for VSS estimation. All the analyses were performed in accordance with standard methods (APHA 1995). Specific activity of biomass was also measured during startup and after stabilization following the procedure outlined (Sorensen 1993). Gas production was measured using liquid displacement technique and the gas composition was analyzed for methane, carbon dioxide, and hydrogen sulfide by gas chromatography using Porapak column and thermal conductivity detector with hydrogen as carrier gas.

Table 2 Characteristics of seed sludge used in study

1. 2. 3. 4. 5. 6. 7.

Color of sludge mass Sludge occupancy in reactor Total solids Total suspended solids Volatile suspended solids Total kjeldhal nitrogen of solids Sludge activity

Dark gray 0.37 m 28,750 mg L1 27,740 mg L1 18,170 mg L1 4 (as % of VSS) 0.12 kgCH4-COD kgVSS1 day1

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3 Results and Discussion 3.1 Reactor Startup In the present investigation, the reactor was seeded with 18.2 kgVSS/m3, creating a sludge bed of 0.37 m in the reactor. The specific activity of the seed sludge was 0.12 kgCH4-COD/kgVSS day. An initial volumetric loading rate of 0.1 kgCOD/m3 day was employed corresponding to sludge loading rate of 0.0055 kgCOD/kgVSS day. During the initial phase when batch feeding was in progress, the substrate conversion efficiency was stable at a minimum value and started an upward trend. The stabilization rate extended till rate of increase in conversion efficiency was constant by around 30th day of operation. The reactor was then operated on continuous feed mode. After an initial drop in efficiency, the reactor once again achieved an upward trend. The reactor was then operated by gradually increasing loading to 1 kgCOD/ m3 day. During 48th day, the sludge bed expanded from 0.37 to 0.42 m due to hydraulic loading and gas production rate. First sludge granules were detected on day 80 and the sludge bed concentration of 28 kgVSS/m 3 and blanket concentration of 3 kgVSS/m3 was obtained by day85. The sludge retained in the reactor decreased slowly until day100, beyond which slight increase could be noted. The specific activity of the retained sludge increased gradually from 0.12 to 1.8 kgCH4-COD/kgVSS day indicating development of active biomass in the system. This clearly indicates that growth of finely dispersed sludge is reduced and the bacterial growth is delegated to a limited number of growth nuclei that may consists of inert organic and inorganic carrier materials or small bacterial aggregates. The selective washout of dispersed sludge resulted in increased growth of retained heavier sludge which is crucial for granulation process (Hulshoff Pol et al. 2004).

Complete stabilization period for the reactor to be fed with hydrogenated vegetable oil wastewater was approximately 195 days achieving steady state substrate conversion efficiency of around 99%. Further studies were carried out with step increase in loading rate by varying substrate concentration and hydraulic detention period. The performance exhibited during seeding and stabilization period is depicted in Fig. 2. 3.2 Reactor Performance The performance of the reactor system was characterized by varying, substrate concentration from 4,000 to 8,000 mg/l and hydraulic detention period from 0.33 to 3 days. The experimental observation of the reactor system is depicted in Fig. 3. Perusal of the figure indicates that with increase in loading rate (to 2.0 kgCOD/m3 day), reduction in conversion efficiency was observed regaining stability after about 15 days. The corresponding steady state removal efficiency was 97.5%. Similar pattern was observed on further increase in substrate loading but the time required for regaining stability reduced with time span. As can be seen from figure, with high step increase in loading rate, the recovery period to attain steady state removals did vary with corresponding fall in substrate removal rates. At high loading rate of 18.0 kgCOD/m3 day, fall in steady state substrate removal efficiency was as low as 71.2%. However, studies have been carried out up to a maximum loading of 22 kgCOD/m3 day. The corresponding substrate removal efficiency achieved was 56.8%. The steady state substrate removal rate (kgCODr/ m3 day) and substrate (in terms of COD) removal efficiency of the reactor system at various substrate loadings rates are depicted in Fig. 4. Behavioral pattern indicates exponential relation between substrate removal rate and loading rate. At higher loading rates, substrate removal rates tend to decrease as indicated by the relationship, while with increase in

Fig. 2 Startup and acclimatization of the rector system

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Fig. 5 Plot of hydraulic detention period as a function of substrate removal efficiency at varying feed substrate concentration Fig. 3 Reactor performance for step increase in loading rates

loading rates there was decrease in substrate removal efficiency bearing a linear relationship between the two parameters and the rate of decrease in substrate conversion obtained is expressed as: y 2:215x 99:8 1

Impact of variation in hydraulic detention period on substrate conversion efficiency at varying feed substrate concentrations of the reactor system is shown in Fig. 5. Substrate removal performance has been similar at different influent substrate concentration of 4, 5, 6, 7, and 8 kgCOD/m3. The observations from data plot reveal that decrease in conversion efficiency with reduction in hydraulic retention time (HRT) is more at higher substrate concentration as compared to lower substrate concentration indicating the fact that the system becomes more organically stressed at higher organic feed concentration. However, variation in HRT at constant substrate loading by varying feed substrate concentration indicates that performance efficiency varies linearly increasing with increase in

HRT. But the increase in efficiency is marginal, i.e., not more than 10% by varying HRT from 0.33 to 3 days at constant substrate loading rate. Therefore, the system can be operated at the said loading either by increasing influent substrate concentration with high HRT or operating with low HRT and low influent substrate concentration. The experimental evaluation indicates that HRT in the range of 12 days can be identified as critical depending on feed substrate loading rate. The details on performance of the reactor under varying temperature and pH are reported elsewhere (Shastry 2004). 3.3 Biogas Generation The prime factor in anaerobic treatment is methane recovery, which requires a proper balance between rate of acid generation and rate of biogas (methane) production in the system. On the whole, methane production must control the overall rate of reaction necessitating proper environmental conditions to be maintained for effective methane fermentation. The biogas generated during anaerobic treatment was plotted as shown in Fig. 6 depicting total biogas yield and methane yield as a function of substrate loading rate. The graphical presentation reveals that biogas and methane yield (m3/m3 day) increases with increase in mass of substrate removed per unit volume per day of the reactor system. However, the rate of increase in the yield marginally declines at higher loading rates the decline of methane yield being more as compared to biogas yield. The specific methane yield (m3CH4/ kgCODr) and methane content in biogas showed a declining trend with increased substrate loading rate bearing a linear relationship (Fig. 7), indicating the fact that at higher loading rate acid production predominate

Fig. 4 Plot of substrate loading rate as a function of substrate removal rate and substrate conversion efficiency

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Fig. 8 Plot of methane yield as a function of substrate loading rate at varying temperature

variance of pH and temperature is shown in Figs. 8 and 9, respectively. These graphical plots indicate linear relationship between methane yield and substrate loading rate with values of m and C varying with pH and temperature, y mx C
Fig. 6 Plot of total biogas and methane yield as a function of substrate of loading rate

the reaction rate as compared to methane generation which is in agreement with that reported by Atuanya and Aigbirior (2002). The methane yield as a function of substrate loading rate for the reactor system under operational

The expression does help in arriving at the optimum yield based on removal that can be applied to the reactor system. The effect of pH and temperature variation on specific methane yield has been illustrated in Fig. 10 clearly indicating that the specific methane yield m (m3CH4/kgCOD) decreases with increase in pH and increases with temperature up to 40C beyond which the yield decreases. 3.4 Impact of Shock Loadings To assess the process stability of the reactor, shock loading studies were carried out. Since, most of the hydrogenated vegetable oil industries are operated in batches, there is variation in wastewater quality and quantity resulting in wide fluctuations in terms of organic and hydraulic loadings. Since the waste generated is generally alkaline in nature, and the

Fig. 7 Plot of specific methane yield and methane content as a function of substrate loading rate

Fig. 9 Plot of methane yield as a function of substrate loading rate at varying pH

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Fig. 10 Effect of pH and temperature on specific methane yield

problem of fluctuations in pH may also arise due to inadequate neutralization imparted to the wastewater. In view of the unstable wastewater characteristics from the industry, studies were carried out to investigate the process resistibility to the impact of shock loading as follows: Organic shock load by intermittent feeding (Fig. 11) Hydraulic shock load (Fig. 12) Shock load due to pH variation (Fig. 13)

increase in substrate reduction was observed because of the available dilution. Later the removal efficiency decreased slightly till steady state condition was achieved on the fourth day. For 10 days of unfed condition, similar behavior was observed. However, there was marked decrease in substrate reduction after the third day and later achieving steady state condition after eighth day. The system was kept under steady state condition for about 6 days. Fifteen days of feed stoppage resulted in initial increase followed by pronounced decrease in substrate removal efficiency. A period of two and half weeks was required to gain stable steady state conditions and the system was kept under this condition for nearly 8 days. In case of a month-long feed stoppage, minimum substrate removal efficiency of 68% on the 17th day was observed. The system recovered again to steady state levels in about 25 days of operation. The study indicated that the reactor system could be operated without feed to a maximum period of 5 days whereby the system regained stability within 4 days of fresh loading. For starvation period beyond 5 days, the system took a long time to recover to stable conditions. 4.1 Hydraulic Shock Load The impact of hydraulic shock loading was assessed by operating at pH7.0 and temperature 35C with substrate concentration of 5,000 mg/L. Low substrate concentration was chosen as otherwise the indirect impact of organic shock load imparted due to increase in hydraulic flow would be too high as compared to the hydraulic shock loading. Operating at an optimum flow of 0.050 m3/day (HRT1.0 day) the system was

4 Organic Shock Load Perusal of Fig. 11 indicates that at optimum loading, with the discontinued feed to the reactor for 5 days,
Fig. 11 Effect of organic shock loading on reactor performance by stoppage of feeding for different span of time

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Fig. 12 Effect of hydraulic shock loading on reactor performance

subjected to a hydraulic flow of 0.067 m3/day, 0.100 m3/day, and 0.152 m3/day (Fig. 12). With the increase in flow from 0.050 m3/day to 0.067 m3/day, the decrease in performance efficiency was 94.0% to around 70% within 3 days. Steady state performance was regained on sixth day and maintained for some more time. Steady state removal at flow of 0.067 m3/day was however lower than that achieved at a flow of 0.050 m3/day may be mainly due to the system being more organically loaded. Flow after resumed to 0.050 m3/day was again increased to 0.100 m3/day achieving reduction in substrate removal of about 60%. It took about 8 days to attain steady state removal of around 8485%. Once again resuming the normal flow of 0.050 m3/ day, the system flow rate was later maintained at 0.152 m3/day. There was a sharp fall in the performance of the reactor system and took around 15 days to gain stability with conversion levels of 7981%.
Fig. 13 Effect of pH variation on reactor performance

The sudden rise in hydraulic flow must have resulted in wash out of biomass from the reactor thereby affecting the system performance adversely. The system performance indicated that under existing operating condition, hydraulic shock load of twice the optimum flow require approximately 7 days to regain stability. However, hydraulic flow beyond this may result in requirement of longer stability period or failure of the system due to wash out of biomass from the system.

5 pH Shock Load Evaluating the effect of pH shock load, the reactor system was operated at a substrate loading of 5.0 kgCOD/m3 day and temperature of 35C. Hydrogenated vegetable oil wastewater with pH levels of 9.5, 10.0, 10.5, and 11.0 was used as feed to evaluate

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the reactor response to pH variation (Fig. 13). Shock loading studies were carried out after the system attained steady state conditions. Reactor performance to various pH shock dose indicated that with feed pH 9.5, there was a fall in substrate removal efficiency however, resuming normal feed, the system regained steady state removal within 5 days. The feed pH of 10.0 indicated pronounced decreasing trend as compared to the reactor working under normal feed. In this case also normal pH developed which may be due to the internal buffering capacity available within the reactor system. Within 8 days period from the start of normal feed of pH7.0, the system achieved steady state conditions. When feed pH11.5 corrected to 10.5 was fed to the reactor system, slowly the contents of the reactor got adversely affected in 6 days time with steep decline in system performance. Later, the system was energized with fresh feed of pH7.0 requiring 12 days to reach steady state conditions. For feed pH of 11.0, there was steep decrease in substrate removal efficiency. Within a period of 4 days, the complete reactor became alkaline. From the eighth day, normal feeding with pH7.0 was started. Slowly the system improved its efficiency regaining steady state performance after about 15 days from the start of fresh feed of pH7.0. The studies revealed that the system when fed with feed pH above 10.0, reactor content becomes highly alkaline resulting in the failure of the system. However, with shock feed pH of 10.0, the reactor can be operated requiring a recovery period of 78 days to achieve steady state substrate conversion rates.

ed vegetable oil industry wastewater, the optimum operational conditions in reference to system performance evaluated were: pH7.0 Temperature35C Hydraulic detention time1.0 to 2.0 days Optimum loading rate7.0 KgCOD/m3 day Maximum loading rate9.88 KgCOD/m3 day The studies relating to susceptibility of the reactor system to shock loading, namely organic, hydraulic, and pH shock load indicated that: The reactor can be starved (no feeding) for a maximum period of 5 days beyond which the system requires a long time to recover The system can handle hydraulic overloading twice the normal flow without any serious problem At feed pH level above 10.0, the microbes in the system are limited in their growth by the low concentration of unionized fatty acids.

The evaluation of the system performance indicated the potential of upflow anaerobic sludge blanket reactor system for the pretreatment of medium strength hydrogenated vegetable oil industry wastewater with recourse to methane recovery. In addition, reuse of energy efficient biogas produced will offset the financial burdens of such systems. The capacity to handle shock loads is an added advantage for such industrial application where both quantity and quality of the wastewater vary extensively.
Acknowledgement The authors are grateful to the Director, NEERI, Nagpur, India for granting permission to carry out the research work.

6 Conclusions A programmed startup operation was essential for effective commissioning of the upflow anaerobic sludge blanket reactor system. A period of around 200 days was required for complete stabilization of the reactor system to be fed directly with hydrogenated vegetable oil industry wastewater. Results of the experiments conducted at various substrate loading rates are indicative of the fact that as the organic loading rate increases there is a decline in the substrate conversion efficiency bearing a linear relationship. Based on the experimental investigation on upflow anaerobic sludge blanket reactor treating hydrogenat-

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