Journal of Membrane Science 254 (2005) 129137

Wastewater treatment of a vegetable oil factory by a hybrid ultraltration-activated carbon process

Toraj Mohammadi , Ashkan Esmaeelifar
Research Lab for Separation Processes, Faculty of Chemical Engineering, Iran University of Science and Technology, Narmak, Tehran, Iran Received 2 March 2004; received in revised form 13 December 2004; accepted 13 December 2004 Available online 16 February 2005

Abstract In this paper, experimental investigation of wastewater treatment by ultraltration (UF) is introduced. In the experiments, a UF membrane (UFPHT20-6338) and samples of Behshahr Ind. Co. wastewater as feed were used. Effect of operating conditions such as pressure difference, cross ow velocity, shear stress, temperature, concentration of organic compounds and pH on permeation ux, ux decline and fouling resistance were studied. Results show that a pressure difference more than 3 105 Pa (3 bar), a high cross ow velocity (depending on economic considerations), a temperature of 30 C and a pH of 9 are the best operating conditions. Fouling of the membrane completely follows Hermias model (cake ltration mechanism). Analysis of the wastewater treated by UF represents 91, 87, 100, 85 and 40% reduction in COD, TOC, TSS, [PO4 3 ] and [Cl ], respectively. Also, treatment of the wastewater by UF-powdered activated carbon (PAC) was studied. According to results, using PAC in feed circulation loop of UF system with a concentration of about 0.1% (W) not only improves water quality but also increases permeation ux. A shear stress induced by PAC on the membrane surface decreases cake layer thickness and as a result increases permeation ux. Analysis of the wastewater treated by UF-PAC represents 94, 93, 100, 99 and 43% reduction in COD, TOC, TSS, [PO4 3 ] and [Cl ], respectively. Reduction of the phosphate concentration by UF-PAC is very considerable. A comparison between the results shows that UF is better than conventional biological method and UF-PAC is better than UF. 2005 Elsevier B.V. All rights reserved.
Keywords: Ultraltration; Fouling; Wastewater treatment; Powdered activated carbon

1. Introduction Conventional water and wastewater treatment processes were long established in removing many chemical and microbial contaminants of concern to public health and the environment. However, effectiveness of these processes has become limited over the last two decades because of three new challenges. First, increased knowledge about consequences from water pollution and public desire for better quality water promoted implementation of much stricter regulations by expanding scope of regulated contaminants and lowering their maximum contaminant levels (MCLs). In water treatment, the most important development is establishment of

Corresponding author. Tel.: +98 21 7896621; fax: +98 21 7896620. E-mail address: torajmohammadi@iust.ac.ir (T. Mohammadi).

possible link between halogenerated disinfection by-products (DBPs) and cancers. Similarly, stricter regulations were set over a much broader range of contaminants for wastewater discharges. Among them, the most signicant are perhaps new requirements to remove nutrients (nitrogen and phosphorus) and synthetic organic compounds (SOCs) because of their signicant impacts on public health and the environment. Second, water resources are diminishing and population is rapidly growing. Reuse of municipal and industrial wastewaters and recovery of potential pollutants used in industrial processes become more critical. This is especially true in arid or semiarid areas where potable water and irrigation water must be imported expensively. Advanced treatment technologies were demonstrated to remove various potentially harmful compounds that could not be effectively removed by conventional treatment processes.

0376-7388/$ see front matter 2005 Elsevier B.V. All rights reserved. doi:10.1016/j.memsci.2004.12.037

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Last, advances in manufacturing industries and growing markets associated with advanced treatment processes resulted in substantial improvements to versatility of these processes at commercial scale. Using life-cycle analysis, it was concluded that costs of new pressure-driven membrane ltration plants are expected to be comparable with or even less than those of conventional treatment processes for capacities up to 20,000 m3 per day [1]. To resolve these new challenges and better use economical resources, various advanced treatment technologies were proposed, tested and applied to meet both current and anticipated treatment requirements. Among them, membrane ltration, advanced oxidation processes (AOPs) and UV irradiation were proven to successfully remove a wide range of contaminants and hold great promise in water and wastewater treatment. Ultraltration (UF) is very effective for wastewater treatment and can operate at very low pressure. Several recent developments were reported to combine these membrane processes with other conventional treatment processes so that various dissolved species could also be removed. Among them, UF-powdered activated carbon (PAC) and membrane bioreactor showed great promise in water and wastewater treatment. At present, these hybrid processes are mainly used for (i) high-strength wastewaters, (ii) strict disinfection requirements for treated water and (iii) trace xenobiotic contaminant and nitrate removal. In UF-PAC, PAC is added to recirculation loop of UF [2,3]. Dissolved organic matters such as SOCs and DBPs are adsorbed on activated carbon particles, which are then separated from wastewater by UF. At present, UF-PAC is mainly used for removing microbial contaminants, turbidity and dissolved organic matters altogether in water treatment. Use of membrane processes alone or combined with conventional treatment processes demonstrates that membrane processes may offer a number of advantages over conventional treatment processes including (i) high-quality efuent over a wide range of raw water sources, (ii) no chemical addition except when organic removal is practiced, (iii) a small amount of solids requires disposal, (iv) very compact installations, (v) simpler automation and control and (vi) reduced operation and maintenance requirements [1]. As a result, this paper focuses on treatment of wastewater of a vegetable oil factory by UF and UF-PAC with emphasis on process fundamentals and operating conditions.

ux decreases as time goes on. Especially in microltration (MF) and UF, ux decline is very severe and ux is often less than 5% of pure water ux. In contrast, this is less severe in gas separation (GS) and pervaporation (PV). Flux decline can be enhanced by several factors, such as concentration polarization, adsorption, cake (gel) layer formation and pore plugging. All these factors induce additional resistances on feed side. Extent of these phenomena and mechanism of fouling are strongly dependent on membrane and feed. The most famous mathematical fouling model, which can be used in most of practical cases, is Hermias model that predicts four different fouling behaviors. UF usually works in cross ow form. In this method, feed ows on membrane surface in parallel direction. Thus, only small part of feed is processed by membrane, and in all cases of practical UF applications, all or part of unprocessed feed is recycled. Generally, the most important advantage of this form is to diminish concentration polarization and membrane fouling. Permeation ux through cake layer and membrane is calculated according to Darcys Law [4].

3. Materials 3.1. Membrane UFPHT membrane produced by DOW Company, Denmark (UFPHT20-6338) was employed for all experiments because of its stability under different operating conditions. It is a polymeric membrane and is made from polysulfone with a MWCO = 30 kDa. 3.2. Feed Outow of equalization tank of Behshahr Ind. Co. wastewater unit was employed as feed. Contaminants of the feed can be categorized into two parts: (1) Organic components such as vegetable fats and oils; fatty acids; glycerine; soap; colored components; gums and detergents. (2) Mineral components such as sodium polyphosphate; sodium silicate and sulphonate; calcium, magnesium and sodium carbonates and chlorides. Approximate analysis of the feed is shown in
Table 1 Analysis of wastewater and treated wastewaters by different methods Feed Permeate (ppm) Biological (ppm) Reduction (%) UF (ppm) Reduction (%) UF-PAC (ppm) Reduction (%) COD 550 90 84 50 91 35 94 TOC 300 130 57 40 87 20 93 TSS 120 50 58 0 100 0 100 PO4 3 20 25 3 85 0.2 99 Cl 350 400 210 40 200 43

2. Theory In UF, driving force of mass transfer is pressure difference, which is within 25 105 Pa (25 bar) and usually forced to system by a pump. Under these conditions, solvent and small solute molecules pass through UF membrane whereas big molecules and colloids remain behind it. During an actual separation in a pressure-driven process, membrane performance (or system performance) changes very much with time and often a typical uxtime behavior is observed: membrane

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Fig. 1. UF experimental set up.

Table 1. The feed was collected daily and used immediately. Its pH was 10.5. 3.3. Adsorbent PAC produced in Merck Company, Germany (Catalog no. = 102514) was used in all UF-PAC experiments.

4.2. Wastewater analysis methods Water generally contains some amount of carbon in form of organic compounds (TOC) and inorganic compounds (TIC) and dissolved dioxides. These may exist as solids, suspensions, dissolved particulates or volatile organic compounds (VOC). Total carbon (TC) can be a useful measurement in certain applications. In the strictest denition, TOC is comprised of all organic carbon including both purgeable components (POC) and nonpurgeable components (NPOC). TOC gained acceptance as the premier water monitoring technique. For most efuents, TOC had some correlation to Oxygen Demand Load. Chemical Oxygen Demand (COD) is dened as quantity of a specied oxidant that reacts with a sample under controlled conditions. Quantity of oxidant consumed is expressed in terms of its oxygen equivalence. COD is expressed in mg/L and often measured as a rapid indicator of organic pollutant in water. It is normally measured in both municipal and industrial wastewater treatment plants and gives an indication of treatment process efciency. COD is measured on both inuent and efuent water. The treatment process efciency is, normally expressed as COD removal, measured as a percentage of organic matter puried during the process. Total suspended solid (TSS) is a measure of both dissolved and suspended solids in a liquid media. It is measured in mg/L and used to express concentration of suspended impurities in a sample. During any treatment process, TOC, COD and TSS should be reduced to an acceptable limit. In all experiments, COD was measured using 5220 C. Closed Reux, Titrimetric Method. TOC was measured using 5310 B. Combustion-Infrared Method. Concentration of Chloride was measured using 4500-Cl C. Mercuric Nitrate Method. Concentration of Phosphate was measured using 4500-P C. Vanadomolybdophosphoric Acid Calorimetric Method. pH was measured using 4500-H+ B. Electrometric Method and TSS was measured using 2540 D. Total suspended solids dried at 103105 C [5].

4. Method 4.1. Experimental method Fig. 1 shows experimental set up used in all experiments. UF cell was made of two apart pieces of stainless steel (Fig. 2). These two parts were sealed by an O-ring and the membrane (28.64 cm2 ) was placed between them. It must be mentioned that for each experiment a new piece of membrane was employed. Since membranes were not completely homogenous, each piece of membrane was initially evaluated by pure water. During the experiments, exact supervision was done to control ow rate, pressure and temperature. Using permeated volume for 10 min and membrane area, permeation ux was calculated and reported according to its conventional unit (L/(m2 h)). In UF-PAC experiments, PAC was added to feed tank at different concentrations, and it consequently entered in feed circulation loop. All of the adjustments and measurements for UF and UF-PAC experiments were the same.

Fig. 2. UF cell.

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Fig. 5. Effect of temperature on equilibrium permeation ux and fouling resistance. Fig. 3. Effect of pressure on equilibrium permeation ux and fouling resistance.

5. Results and discussion 5.1. Effect of operating conditions on permeation ux, fouling and fouling resistance 5.1.1. Effect of pressure Increasing pressure increases permeation ux, but higher pressures cause the cake layer formed on membrane surface to compress. This accelerates membrane fouling [68]. Thus, at optimum pressure, permeation ux is high and tendency to cake layer formation is low. Fig. 3 shows the equilibrium permeation ux as a function of pressure. According to Darcys Law, as pressure increases, while other operating parameters remain constant, permeation ux increases. Fouling experiments were carried out at different pressures. The results are shown in Fig. 4. Investigations of permeation ux as a function of time at different pressures show that trend of variations at all pressures is almost the same. In all cases, after a denite time, permeation ux reaches to a constant value depending on operating pressure. Using Fig. 4, ux decline at different pressures can be compared. The results show that, at higher pressures, ux decline is greater. According to the results, at each pressure after about 60 min, ux reaches to a constant value. It is because, after

this time, the cake layer reaches to equilibrium and its growth ceases. So, the cake layer resistance and subsequently permeation ux remain constant [9,10]. As shown in Fig. 3, membrane resistance (Rm ) does not change with pressure whereas fouling resistance (Rf ) increases as pressure increases. Until a pressure of 3 105 Pa (3 bar), Rf increases but after that it does not change considerably and remains nearly constant. Thus, a pressure of 3 105 Pa (3 bar) is the least operating pressure. Because at higher pressures, permeation ux increases as pressure increases but Rf does not change any more. 5.1.2. Effect of temperature Temperature has also a serious effect on permeation ux and this can be represented by Arenius equation [4,11]. Also, according to Darcys Law, increasing temperature increases permeation ux and experimental data conrm this expectation (Fig. 5). It is because viscosity decreases and diffusivity increases at elevated temperatures [12]. From another point of view, increasing temperature increases osmotic pressure and increasing osmotic pressure decreases permeation ux. Therefore, because of bilateral effect of temperature, an optimum temperature must be specied. Fouling experiments were carried out at different temperatures. The results are shown in Fig. 6. As mentioned before, permeation ux reduces with time but generally after 60 min

Fig. 4. Effect of pressure on fouling.

Fig. 6. Effect of temperature on fouling.

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Fig. 8. Effect of concentration on fouling.

Fig. 7. Effect of concentration on equilibrium permeation ux and fouling resistance.

using the original feed (TOC = 300 ppm) and proportional amount of distilled water (e.g., mixing 1 part of the feed with 3 parts of distilled water gives a new feed (TOC = 75 ppm)). 5.1.4. Effect of velocity As shown in Fig. 9, increasing velocity increases Reynolds number from 1302 to 4808 and this enhances turbulency and as a result permeation ux increases. The main reason is reduction of concentration polarization effect. Turbulency and shear stress on membrane surface increase by increasing velocity. Therefore, the accumulated compounds on membrane surface return in to the bulk of uid and concentration polarization effect diminishes. This, thus, causes osmotic pressure to decrease and permeation ux to increase [13,14]. Increasing velocity increases permeation ux linearly but for all velocities employed, there is a ux decline (Fig. 10). Such as other results, permeation ux reaches to a constant value after 60 min depending on operating velocity. At higher velocities, some parts of the cake layer are removed from membrane surface by hydrodynamical forces and returned in to the bulk of uid. Thus, at higher velocities, the cake layer is thinner and permeation ux is higher [9,10]. The results shown in Fig. 9 conrm the pervious results. From the results, it can be concluded that, at higher velocities, fouling resistance is lower and subsequently permeation ux is higher. It should also be noticed that increasing velocity, in-

reaches to a constant value depending on operating temperature. At higher temperatures, since viscosity decreases and diffusivity increases, permeation ux is higher [12]. However, specic properties of some solutions such as dissolved matters, their interaction, etc. limit this effect. As shown in Fig. 5, increasing temperature to about 30 C decreases Rf very considerably, but as temperature increases more Rf remains almost constant. This can be attributed to the properties of solution and is being under investigation. Also, as mentioned before, increasing temperature increases osmotic pressure. Thus, effective pressure difference decreases and this partly neutralizes effect of increasing diffusivity. Therefore, the best operating temperature is about 30 C. 5.1.3. Effect of concentration As shown in Fig. 7, increasing concentration decreases permeation ux. It is because higher concentrations have higher osmotic pressures. Thus, increasing concentration decreases effective pressure difference and subsequently permeation ux. Also, increasing concentration causes the cake layer formed on membrane surface to thicken. As shown, at higher concentrations, equilibrium permeation uxes approach to almost the same value. It is due to the fact that for each feed (depending on dissolved matters and its osmotic pressure) there is a certain concentration and higher concentrations do not affect the cake layer formation on membrane surface [9]. Fouling experiments were carried out at different concentrations. The results are shown in Fig. 8. As shown, permeation ux decreases quickly at the beginning of ltration for all concentrations. Also, at each time interval, permeation uxes are less at higher concentrations. It is because of higher growth rate of the cake layer and thicker layers at higher concentrations [7,9]. As shown in Fig. 7, as concentration increases, deposition of the organic compounds on membrane surface, and as a result Rf , increases. As a result, it can be said that, at lower concentrations, treatment process can be better carried out. In the experiments, feed preparation at different concentrations was performed

Fig. 9. Effect of velocity on equilibrium permeation ux and fouling resistance.

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Fig. 10. Effect of velocity on fouling. Fig. 12. Effect of pH on fouling.

creases energy consumption. In this study, experiments were carried out with a maximum velocity of 0.52 m/s, however, results of other researchers show that at a denite threshold, increasing velocity does not affect permeation ux [13,14]. 5.1.5. Effect of pH Fig. 11 shows effect of pH on permeation ux. As shown, increasing pH increases permeation ux considerably. It is because of better dissociation of fatty acids at alkali solutions. Fatty acids are weak acids and their dissociations are equilibrium reactions. Thus, increasing pH pushes the equilibrium to product side. Therefore, fatty acid molecules are converted into ions and their accumulation on the membrane surface reduces. As a result, permeation ux increases [15]. Concentration of fatty acids in the feed (wastewater, on the basis of oleic acid) was 150200 ppm. It was determined by extraction of fatty acids from the feed (with hexane) and using AOCS ofcial method Ca 5a-40 [5]. The results show that as pH increases to about 9, permeation ux increases very considerably but at higher pH this positive effect is not signicant. It is because, most of fatty acid molecules dissociate until a pH of 9. Thus, concentration of undissociated fatty acid molecules is low and increasing pH does not have any considerable effect. Fouling experiments were carried out at different pHs. The results are shown in Fig. 12. As shown, permeation ux in-

creases as pH increases but for all pHs, it reaches to a constant value that is higher at higher pH. As mentioned, the main reason is better dissociation of fatty acids at alkali solutions and subsequently removing the molecules from the membrane surface. So, at higher pHs, the cake layer is thinner and permeation ux is higher [15]. As fatty acid concentration increases, effect of pH on permeation ux becomes more considerable. Fig. 11 shows effect of pH on Rf . As pH increases to a value of 9, Rf decreases severely. As can be observed, reduction of Rf is sharp until a pH of 9 and after that Rf does not change signicantly. 5.2. Modeling of ux decline After comparison of the experimental data with Hermia s model, which predicts four different fouling behaviors, it was observed that fouling of the membrane completely follows cake ltration mechanism. Fig. 13 shows agreement of the experimental data with these mechanisms. Deviation of the experimental data from cake ltration mechanism is less than 3%. According to the cake ltration mechanism, permeation ux decreases with increasing resistance in the proximity of membrane surface (where solutes accumulate) [9,16]. 5.3. Effect of pressure on COD To evaluate performance of the membrane, COD of the permeate was measured at each pressure. The results are presented in Fig. 14. As shown, increasing pressure difference increases COD of the permeate. It is due to the fact that, at higher pressures, effect of pressure predominates over effect of pore size, and as a result, more organic compounds pass through the membrane [6]. It must be mentioned that COD reduction is signicant at all pressures (COD of the feed was 550 ppm). 5.4. Investigation of UF-PAC In UF-PAC experiments, PAC was added to the feed circulation loop. Effect of PAC on UF was studied at different PAC concentrations (Fig. 15) and equilibrium permeation ux was measured.

Fig. 11. Effect of pH on equilibrium permeation ux and fouling resistance.

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Fig. 13. Comparison of the experimental data with Hermias model.

Organic compounds (such as SOCs) are adsorbed by PAC particles and subsequently these particles are retained by the membrane [1,1720]. As shown, increasing PAC concentration to 0.1% increases permeation ux. Shear stress induced by PAC particles on the membrane surface decreases the cake layer thickness [1]. However, increasing PAC concen-

tration to higher than 0.1% decreases permeation ux. It can be due to the fact that, at concentrations higher than 0.1%, PAC particles cause the cake layer on membrane surface to thicken.

Fig. 14. Effect of pressure on COD of the permeate.

Fig. 15. Effect of PAC concentration on equilibrium permeation ux and COD.

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Effect of PAC concentration on COD of the permeate is shown in Fig. 15. As seen, increasing PAC concentration decreases COD of the permeate. In other words, increasing PAC concentration in the feed circulation loop increases surface area of PAC particles, and as a result, causes more organic compounds to be adsorbed [1,18,21]. Since COD depends on concentration of dissolved organic materials, reduction of their concentration decreases COD considerably. Analysis of the wastewater treated by UF-PAC shows that during the process, each gram of PAC adsorbs 0.1 g of dissolved organic materials, approximately (0.1 g of organic materials/1 g of PAC). 5.5. Comparison of several treatment methods Table 1 shows the results of three different treatment methods (Biological, UF and UF-PAC). Currently, conventional biological method is being used in Behshahr Ind. Co. for wastewater treatment. As shown, the results of UF for all analysis are better than the results of biological method. This is more considerable for TOC, TSS and [PO4 3 ]. In biological method, concentrations of [Cl ] and [PO4 3 ] in outow stream are more than those in inow stream. It is because fats and other organic compounds decompose during two biological steps and this releases some excess Cl and PO4 3 ions from these materials. The released excess Cl and PO4 3 ions exit from the system via the outow stream and this causes concentrations of these two ions to increase. However, in UF, concentrations of these two ions decrease considerably. In UF-PAC, the achieved results are better than those of both UF and biological method. In this method, because of using PAC in the feed circulation loop, some soluble organic compounds are adsorbed by carbon particles and as a result remain behind the membrane. Therefore, TOC and as a result COD of the permeate when using UF-PAC are less than those when using UF. The main advantage of using PAC is considerable reduction of phosphate concentration. Phosphorus is a nutrient material and unlimited entrance of this material to the environment causes serious problems. By using UF-PAC, phosphate concentration can be signicantly reduced (more than 99%). Separation performance of different methods is also presented in Table 1.

ties do not affect permeate properties seriously. The results show that a pressure difference more than 3 105 Pa (3 bar), high cross ow velocity, a temperature of 30 C and a pH of 9 are the best operating conditions. It was found that using PAC in the feed circulation loop improves separation performance. Also, this is very effective for reduction of phosphate concentration. In UF-PAC, optimum concentration of PAC is about 0.1%. It was found that increasing PAC concentration to more than 0.1% enhances membrane fouling.

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6. Conclusion According to the results, it can be concluded that UF treatment is an advantageous method for treatment of the wastewater. More suitable properties of the permeate, easier operating conditions, more ability to combine with other methods (chemical and biological) and easier control of the system are considerable advantages of UF. In addition, slight dependence of permeate properties on feed properties is another advantage. In other words, nite variations in feed proper-

T. Mohammadi, A. Esmaeelifar / Journal of Membrane Science 254 (2005) 129137 [19] L. Nicolet, U. Rott, Recirculation of powdered activated carbon for the adsorption of dyes in municipal wastewater treatment plants, Water Sci. Technol. 40-1 (1999) 191. [20] C. Bornhardt, J.E. Drewes, M. Jekel, Removal of organic hologens (AOX) from municipal wastewater by powdered activated carbon (PAC)/activated sludge (AS) treatment, Water Sci. Technol. 35-10 (1997) 147.

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