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Pet. Sci. (2017) 14:605–615 DOI 10.1007/s12182-017-0178-x OR IGINAL PAPER Efficient ozonation of reverse osmosis concentrates from petroleum refinery wastewater using composite metal oxide- loaded alumina 1 1 2 3 1 • • • • • Yu Chen Chun-Mao Chen Brandon A. Yoza Qing X. Li Shao-Hui Guo 1 1 1 • • Ping Wang Shi-Jie Dong Qing-Hong Wang Received: 15 December 2016 / Published online: 13 July 2017 The Author(s) 2017. This article is an open access publication Abstract Novel Mn–Fe–Mg- and Mn–Fe–Ce-loaded alu- Keywords Petroleum refinery wastewater Reverse mina (Mn–Fe–Mg/Al O and Mn–Fe–Ce/Al O ) were osmosis concentrate Catalytic ozonation Composite 2 3 2 3 developed to catalytically ozonate reverse osmosis con- metal oxide centrates generated from petroleum refinery wastewaters (PRW-ROC). Highly dispersed 100–300-nm deposits of 2? 3? composite multivalent metal oxides of Mn (Mn ,Mn , 1 Introduction 4? 2? 3? 2? and Mn ), Fe (Fe and Fe ) and Mg (Mg ), or Ce 4? (Ce ) were achieved on Al O supports. The developed The need for freshwater and its conservation are motivating 2 3 Mn–Fe–Mg/Al O and Mn–Fe–Ce/Al O exhibited higher factors for treatment of wastewaters generated by petro- 2 3 2 3 catalytic activity during the ozonation of PRW-ROC than leum refining industries. Reverse osmosis (RO) systems are Mn–Fe/Al O , Mn/Al O , Fe/Al O , and Al O . Chemical widely used during the treatment and reclamation pro- 2 3 2 3 2 3 2 3 oxygen demand removal by Mn–Fe–Mg/Al O - or Mn– cesses for the effluent from petroleum refinery wastewater 2 3 Fe–Ce/Al O -catalyzed ozonation increased by 23.9% and (PRW) plants (Pe ´rez-Gonza ´lez et al. 2012). In China, 70 2 3 23.2%, respectively, in comparison with single ozonation. wt%–80 wt% of the effluent is reclaimed using RO systems Mn–Fe–Mg/Al O and Mn–Fe–Ce/Al O notably pro- and used as the high-quality feed water for steam produc- 2 3 2 3 moted OH generation and OH-mediated oxidation. This tion. The remaining 20 wt%–30 wt% of RO concentrate study demonstrated the potential use of composite metal (ROC) contains petroleum-derived chemicals (Chen et al. oxide-loaded Al O in advanced treatment of bio-recalci- 2016). Direct discharge of the ROC threatens the ecolog- 2 3 trant wastewaters. ical environment and human health. The organics in ROC generated from PRW reclamation (PRW-ROC) need to be reduced to eliminate these negative impacts and to meet increasingly stringent discharge standards (Moreira et al. 2017). Previous work has already investigated the use of Yu Chen and Chun-Mao Chen have contributed equally to this work. physicochemical and biological treatments; however, low concentrations and biologically recalcitrant organic matter & Qing-Hong Wang suggest these methods are unsuitable (Bagastyo et al. wangqhqh@163.com 2013). State Key Laboratory of Petroleum Pollution Control, Beijing Advanced oxidation processes (AOPs) are the preferred Key Laboratory of Oil and Gas Pollution Control, China advanced treatment method during reclamation of various University of Petroleum, Beijing 102249, China municipal and industrial wastewater ROC products (Joo Hawaii Natural Energy Institute, University of Hawaii at and Tansel 2015; Ren et al. 2016). These methods, Manoa, Honolulu, HI 96822, USA including ozonation (Dialynas et al. 2008), Fenton oxida- Department of Molecular Biosciences and Bioengineering, tion (Zhou et al. 2012), photocatalysis (Joo and Tansel University of Hawaii at Manoa, Honolulu, HI 96822, USA 2015), photooxidation (Umar et al. 2016), sonolysis (Pe ´rez- Gonza ´lez et al. 2012), or electrochemical oxidation Edited by Xiu-Qin Zhu 123 606 Pet. Sci. (2017) 14:605–615 (Bagastyo et al. 2011; Van Hege et al. 2002), can provide of BrO formation and high total organic carbon removal efficient removal of low concentration and recalcitrant for a Br-containing raw water (Nie et al. 2014). Numerous organics. Among these, the heterogeneous catalytic studies have revealed that composite metal oxides loaded ozonation processes (COPs) are the most promising, as on Al O supports exhibited high catalytic activity com- 2 3 they are economical, highly efficient, and simple in their pared with single metal oxide loading (Tong et al. 2010). application. The predominant role of catalysts for hetero- Mn–Fe–Cu/Al O enhanced catalytic ozonation of PRW 2 3 geneous COP treatment is decomposing ozone into more compared with single or double metal oxide-loaded Al O , 2 3 active species such as hydroxyl radicals (OH), and/or for a result from interactions between the composite metal the adsorption of specific organics that can react with oxides on the Al O surface (Chen et al. 2015). Magnesium 2 3 dissolved ozone (Chen et al. 2015). A wide variety of oxides, that include MgO nanocrystals and MgO/granular catalysts have been developed for COPs; however, most activated carbon (GAC), have potential for ozonation of synthesized or prepared catalysts are costly, limiting their bio-recalcitrant organics including phenols (Moussavi et al. industrial application. 2014), benzene homologues (Rezaei et al. 2016), and dye Alumina (Al O ) and metal oxide-loaded Al O have pollutants (Moussavi and Mahmoudi 2009). During the 2 3 2 3 been widely applied in COPs. These materials have highly ozonation of catechol that is catalyzed by MgO/GAC, OH active and large surface area, good mechanical properties was responsible for its degradation and mineralization, and and are stable (Einaga and Futamura 2005; Pocostales et al. this reaction rate constant was six times greater than single 2011; Keykavoos et al. 2013; Vittenet et al. 2015). Indus- ozonation (Moussavi et al. 2014). Catalysts containing Ce trial grade c-Al O particles have been used for enhanced have also been studied for the ozonation of p-chloroben- 2 3 ozonation of petrochemical effluents (Vittenet et al. 2015). zoic acid (Bing et al. 2013), bezafibrate (Xu et al. 2016), Ti/Al O (Bing et al. 2017), Ru/Al O (Zhou et al. 2007), dimethyl phthalate (Yan et al. 2013), and tonalide (Santi- 2 3 2 3 and V/Al O (Qi et al. 2009) are efficient catalysts for the ago-Morales et al. 2012). However, their applicability for 2 3 treatment of recalcitrant organics such as dimethyl phtha- wastewater treatment has not yet been reported. late and 1, 2-dichlorobenzene. Mn/Al O is another pow- In this study, novel composite metal oxide-loaded Al O 2 3 2 3 erful catalyst for removal of bio-recalcitrant organics. Mn/ catalysts, including Mn–Fe–Mg/Al O and Mn–Fe–Ce/ 2 3 Al O can significantly produce OH when it reacts with Al O , were prepared and characterized. The potential use 2 3 2 3 ozone, resulting in enhanced catalytic degradation of of these catalysts for the advanced treatment of PRW-ROC atrazine (Rosal et al. 2010a), and fenofibric acid (Rosal using COP was investigated. Insights into these catalytic et al. 2010b). Fe/Al O exhibited both significant inhibition mechanisms are also provided. 2 3 Mn-Fe-Ce/Al O 2 3 Mn-Fe-Mg/Al O 2 3 Mn-Fe/Al O 2 3 Mn/Al2O3 Fe/Al O 2 3 Al O 2 3 012 34567 89 10 Catalysts 20 30 40 50 60 70 80 90 Fig. 1 COD removals for PRW-ROC using single ozonation and 2 , degree θ various COPs (0.5 g catalyst, 5 mg/min ozone, 30 C, and 40 min). 1 single ozonation, 2 Al O -COP, 3 Fe/Al O -COP, 4 Fe/Al O (s)- 2 3 2 3 2 3 COP, 5 Mn/Al O -COP, 6 Mn/Al O (s)-COP, 7 Mn–Fe/Al O -COP, Fig. 2 XRD patterns of Al O and metal oxide-loaded Al O 2 3 2 3 2 3 2 3 2 3 8 Mn–Fe–Mg/Al O -COP, and 9 Mn–Fe-Ce/Al O -COP catalysts 2 3 2 3 COD removals, % Intensity, a.u. Pet. Sci. (2017) 14:605–615 607 (a) (b) (c) (d) (e) (f) Fig. 3 SEM micrographs of Al O (a), and SEM–TEM micrographs of Fe/Al O (b), Mn/Al O (c), Mn–Fe/Al O (d), Mn–Fe–Mg/Al O (e), 2 3 2 3 2 3 2 3 2 3 and Mn–Fe–Ce/Al O (f) catalysts 2 3 (a) (b) 2.0 Al O 2 3 Al O 2 3 Fe/Al O 2 3 Fe/Al O 2 3 Mn/Al O 2 3 1.5 Mn/Al O 2 3 Mn-Fe/Al O 2 3 Mn-Fe/Al O 2 3 Mn-Fe-Mg/Al O 2 3 Mn-Fe-Mg/Al O 2 3 Mn-Fe-Ce/Al O 2 3 Mn-Fe-Ce/Al O 2 3 1.0 0.5 0.0 0.0 0.2 0.4 0.6 0.8 1.0 1 10 100 Relative pressure (P/P ) Pore diameter, nm Fig. 4 Isotherms (a) and pore distribution curves (b)ofAl O and metal oxide-loaded Al O catalysts by N adsorption–desorption 2 3 2 3 2 Quantity adsorbed, cm /g STP BJH adsorption dV/dlog (D) pore volume 608 Pet. Sci. (2017) 14:605–615 Table 1 Surface areas and pore structures of Al O and metal oxide- Impregnation of 60.0 g boehmite with 4.46 or 9.00 g 2 3 loaded Al O catalysts 2 3 Fe(NO ) 9H O yielded Fe/Al O or Fe/Al O (s) cata- 3 3 2 2 3 2 3 2 3 lysts, respectively. The impregnated samples were calcined Catalysts S ,m /g V ,cm /g D ,nm BET P a at 550 C for 4 h in air after drying at 120 C for 12 h. Al O 250 0.38 6.1 2 3 Al O was prepared from pseudoboehemite by calcination 2 3 Fe/Al O 252 0.36 5.7 2 3 at 550 C for 4 h in air. Mn/Al O 258 0.36 5.6 2 3 Mn–Fe/Al O 255 0.37 5.7 2 3 2.2 Characterization of catalysts Mn–Fe–Mg/Al O 230 0.35 6.1 2 3 Mn–Fe–Ce/Al O 242 0.35 5.8 2 3 The crystal forms were observed by X-ray powder diffraction (XRD) using a D8 advance X-ray powder diffractometer (Bruker, Germany) with 40.0 kV working voltage and 40.0 mA current and a copper target X-ray tube. The specific Fe/Al2O3 surface area and pore size distribution were determined using Mn/Al2O3 a Tristar II 3020 surface area and porosity analyzer (Mi- Mn-Fe/Al2O3 cromeritics, USA) with liquid nitrogen cooling at -196 C. Mn-Fe-Mg/Al2O3 The total surface areas (S ) and total pore volume (V )were BET p Mn-Fe-Ce/Al2O3 calculated according to Brunauer–Emmett–Teller (BET) and Barrett–Joyner–Halenda (BJH) methods, respectively. The bulk chemical composition was determined by X-ray fluo- rescence (XRF) analysis with an AX XRF analyzer (Axiosm, Netherlands). The elemental surface distribution was deter- mined by X-ray photoelectron spectroscopy (XPS) analysis with a PHI Quantera SXM X-ray photoelectron spectrometer (ULVAC, USA), where all measured values of the binding energy (BE) were referred to the C line at 284.8 eV. The 1S diffuse reflectance spectra were recorded on a U-4100 UV– Vis spectrophotometer (Hitachi, Japan). The surface mor- 200 300 400 500 600 700 800 phology was observed with a Tecnai G2 F20 transmission Wavelength, nm electron microscope (TEM) and a Quanta 200F scanning electron microscope (SEM) (FEI, USA). The point of zero Fig. 5 UV-Vis patterns of metal oxide-loaded catalysts charge (pH ) was determined according to the pH drift pzc method (Altenor et al. 2009). 2 Experimental 2.3 Ozonation of PRW-ROC 2.1 Preparation of catalysts The PRW-ROC used was collected directly from the RO Commercial pseudoboehemite (65.6 wt% of Al O )was pur- 2 3 unit of a wastewater treatment plant in Liaohe Petrochemical chased from Chalco Shandong Co., Ltd. (China). Fe(NO ) 3 3- Co., China National Petroleum Corp. The ranges of pH 9H O(C98.5 wt%), Mn(NO ) 4H O solution (50 wt%), 2 3 2 2 values, 5-day biochemical oxygen demand (BOD ), chemi- Mg(NO ) 6HO(C99.0 wt%), and Ce(NO ) 6H O 3 2 2 3 3 2 cal oxygen demand (COD), and electric conductivity (C99.0 wt%) were obtained from Beijing Chemical Reagents (25 C) were determined. These were 8.0 to 8.5, 9.2 to 16.3, Co., China. The catalysts were prepared according to the 105.6 to 125.3 mg/L, and 4438 to 5130 lS/cm, respectively. incipient wetness impregnation method. 60.0 g boehmite was The COD concentration of PRW-ROC failed to meet the impregnated with the mixture solution of 4.57 g Mn(NO ) 3 2- current Emission Standard of Pollutants for Petroleum 4H O, 4.57 g Fe(NO ) 9H O and 0.79 g Mg(NO ) 6H O, or 2 3 3 2 3 2 2 Refining Industry of China (GB 31570-2015) in which the 0.35 g Ce(NO ) 6H O(C99.0 wt%) to yield Mn–Fe–Mg/ 3 3 2 allowable COD concentration is lower than 60 mg/L. The Al O or Mn–Fe–Ce/Al O catalysts. 2 3 2 3 BOD /COD ratios of PRW-ROC were ranged from 0.09 to Impregnation of 60.0 g boehmite with a mixture solu- 0.13. Due to low biodegradability, COP was determined as tion of 4.55 g Mn(NO ) 4H O and 4.56 g Fe(NO ) 9H O 3 2 2 3 3 2 an efficient advanced treatment method for PRW-ROC. yielded Mn–Fe/Al O catalyst. Impregnation of 60.0 g 2 3 The experimental system was constructed with an oxy- boehmite with 4.45 or 9.00 g Mn(NO ) 4H O yielded Mn/ 3 2 2 gen tank, RQ-02 ozone generator (Ruiqing, China), Al O or Mn/Al O (s) catalysts, respectively. 2 3 2 3 200-mL quartz column reactor, flow meter, and an exhaust Absorbance, a.u. Pet. Sci. (2017) 14:605–615 609 Mn2p3/2 Fe2p3/2 Mn-Fe-Ce/Al2O3 Mn-Fe-Ce/Al2O3 Mn-Fe-Mg/Al2O3 Mn-Fe-Mg/Al2O3 Mn-Fe/Al O Mn-Fe/Al O 2 3 2 3 Mn/Al O 2 3 Fe/Al2O3 638 640 642 644 646 706 708 710 712 714 716 Binding energy, eV Binding energy, eV Mg1s Ce3d Mn-Fe-Mg/Al O 2 3 Mn-Fe-Ce/Al2O3 870 880 890 900 910 920 1296 1299 1302 1305 1308 1311 Binding energy, eV Binding energy, eV Fig. 6 XPS spectra of Mn2p, Fe2p, Ce3d, and Mg1s of metal oxide-loaded catalysts -1 Counts, s Counts, a.u. -1 Counts, s Counts, a.u. 610 Pet. Sci. (2017) 14:605–615 Table 2 Binding energies and surface atomic ratios of Mn, Fe, Mg, and Ce elements on catalysts Items Fe/Al O Mn/Al O Mn–Fe/Al O Mn–Fe–Mg/Al O Mn–Fe–Ce/Al O 2 3 2 3 2 3 2 3 2 3 Binding energies Mn2p – 641.8 642.2 642.2 642.2 Fe2p 711.1 – 711.9 711.5 711.7 Ce3d – – – – 903.0 Mg1s – – – 1303.2 Metal oxides value state 2? 3? 4? Mn :Mn :Mn – 0.22:0.37:0.41 0.22:0.36:0.42 0.10:0.38:0.53 012:0.39:0.51 2? 3? Fe :Fe 0.31:0.69 – 0.52:0.48 0.50:0.50 0.57:0.43 Surface atomic ratio Mn2p/Al2p – 0.015 0.016 0.014 0.015 Fe2p/Al2p 0.016 – 0.018 0.011 0.013 Mg1s/Al2p – – – 0.010 Ce3d/Al2p – – – 0.004 (Mn2p ? Fe2p ? Mg1s ? Ce3d)/Al2p 0.016 0.015 0.034 0.035 0.032 gas collector. An aliquot of 100 mL of PRW-ROC and 0.5 g catalyzed using Mn–Fe–Mg/Al O (Mn–Fe–Mg/Al O - 2 3 2 3 of catalyst were added in the reactor at 30 C. The gaseous COP) resulted in an increased COD removal (57.3%) ozone was then introduced through a porous diffuser at the compared with the other catalysts, Mn–Fe-Ce/Al O -COP 2 3 bottom of the reactor with a flow rate of 5 mg/min. The (56.6%), Mn–Fe/Al O -COP (55.8%), Fe/Al O -COP 2 3 2 3 experiments were carried out under varying the initial pH (52.0%), Fe/Al O (s)-COP (53.8%), Mn/Al O -COP 2 3 2 3 values (adjusted with 1 N NaOH or HCl) and reaction times. (51.3%), Mn/Al O (s)-COP (53.5%), and Al O -COP 2 3 2 3 After treatment, dried oxygen was blown into the PRW- (45.2%). It was especially significant when compared with ROC at a rate of 3.0 L/min to quench the reaction and single oxide ozonation (33.4%) using a 40-min treatment eliminate the residual ozone. The resulting suspension was (Fig. 1). The surface content of loaded Fe O or MnO was 2 3 filtered (Whatman Qualitative No. 5) to separate catalyst about 4.3 wt% for Fe/Al O (s) and Mn/Al O (s), almost 2 3 2 3 particles prior to further analysis at various intervals. The double compared with Fe/Al O and Mn/Al O (2.1 wt%). 2 3 2 3 OH quenching experiments were performed to determine The increased Fe and Mn oxide contents resulted only in a the oxidation mechanism. The OH scavengers, tert-butanol limited performance improvement for COD removal. In (tBA), and sodium bicarbonate (NaHCO ) were added into comparison, composite metal oxide-loaded Al O was 3 2 3 PRW-ROC (0.5 and 1.0 g/L, respectively) prior to experi- more effective at equivalent loadings (about 4.2 wt%), ments. All the experiments were performed in triplicate. suggesting synergistic effects. For Mn–Fe–Mg/Al O , Mn– 2 3 The pH and conductivity were measured with a MP 220 Fe–Ce/Al O , Mn–Fe/Al O , Fe/Al O , and Mn/Al O 2 3 2 3 2 3 2 3 pH meter (Mettler Toledo, Switzerland) and a CD400 composites, the content of Fe O and MnO was 2.1 wt%, 2 3 conductivity meter (Alalis, China), respectively. The and MgO and CeO were above 0.3 wt% based on XRF leaching of Ce and Mg elements was measured with an analysis. Further investigation focused on utilization of AAnalyst atomic absorption spectrometer (PerkinElmer, Mn–Fe–Ce/Al O , Mn–Fe–Mg/Al O , Mn–Fe/Al O , Mn/ 2 3 2 3 2 3 USA) using a nitrous oxide/oxygen–acetylene flame. The Al O , Fe/Al O , and Al O catalysts. 2 3 2 3 2 3 BOD was tested on a BODTrak II BOD meter (HACH, USA). The COD was measured with a CTL-12 COD meter 3.2 Characteristics of catalysts (HATO, China). The COD removal was calculated using the following equation: The metal oxide-loaded Al O showed typical c-Al O 2 3 2 3 COD removal = ½ COD ½ COD =½ COD ð1Þ 0 1 0 diffraction peaks (Fig. 2). Obvious XRD diffraction peaks from the metal oxides were not observed, due to the low 3 Results and discussion loading or amorphous status. Using TEM, it was deter- mined that the deposited metal oxides formed micro-ag- 3.1 Catalytic performances of catalysts glomerates in irregular shapes and sizes on the surface of Al O (Fig. 3), and that based on SEM, the surface mor- The COD removal from PRW-ROC using COPs increased 2 3 using Al O and metal oxide-loaded Al O . Ozonation phology of Al O itself was little changed. 2 3 2 3 2 3 123 Pet. Sci. (2017) 14:605–615 611 Adsorption–desorption isotherms and pore distributions 8 (a) varied among Al O and metal oxide-loaded Al O catalysts 2 3 2 3 (Fig. 4a, b). According to IUPAC classification, the isotherms of these catalysts suggest a typical type IV mesopore structure (Xu and Pang 2004). A hysteresis loop attributed to type H was observed for Al O ,Fe/Al O ,Mn/Al O ,Fe–Mn/Al O , 2 3 2 3 2 3 2 3 Al O 2 3 and Mn–Fe–Ce/Al O , suggesting uniform shape and pore 2 3 Fe/Al O size. The hysteresis loop determined for Mn–Fe–Mg/Al O , 2 3 2 3 Mn/Al O however, resulted in a combination of H and H types. This 2 3 1 3 suggests the potential presence of silt pores that are a result of Mn-Fe/Al O 2 3 metal oxide particle accumulation. Different hysteresis types Mn-Fe-Mg/Al O 2 3 are potentially a result of interactions between the oxides and Mn-Fe-Ce/Al2O3 the Al O support. All deposited oxide catalysts have a pro- 2 3 510 15 20 25 30 35 40 nounced pore distribution peak at 5–6 nm. The surface areas Time, min (S ), pore volumes (V ), and average pore sizes (D )were BET P a 2 3 230–250 m /g, 0.35–0.38 cm /g, and 5.7–6.1 nm, respec- 70 (b) Fe/Al O Mn/Al O 2 3 2 3 tively (Table 1). Mn–Fe–Mg/Al O showed the lowest S 2 3 BET Mn-Fe/Al O Mn-Fe-Mg/Al O 2 3 2 3 and V values among these catalysts. Mn-Fe-Ce/Al O 2 3 Figure 5 shows the UV–Vis spectra of metal oxide- loaded catalysts. Fe/Al O had a wide absorbance peak 2 3 with a lower intensity centered at 200–600 nm, attributed 3? to isolated Fe , oligomeric FeO clusters, and large Fe O x 2 3 Al2O3 particles (Santhosh Kumar et al. 2004). Mn/Al O dis- 2 3 played an absorption peak centered at 250 nm and a wide peak with lower intensity centered at 400–600 nm, asso- Single ozonation 2- 2? ciated with a charge transfer (CT) O ?Mn and poorly 3? resolved absorbance bands (d-d transitions) from Mn - 4? and Mn -oxo species, respectively (Wu et al. 2015). Mn– 510 15 20 25 30 35 40 Fe/Al O exhibited peaks at 250, 350, and 480 nm, due to 2 3 Time, min composite Fe and/or Mn oxide presence. Mn–Fe–Mg/ Al O and Mn–Fe–Ce/Al O showed significantly 2 3 2 3 (c) Initial PRW-ROC increased absorbance intensity at 250 nm, suggesting Effluents homogenous dispersion of Ce and Mg oxides. Figure 6 shows the XPS spectra of Mn2p, Fe2p, Mg1s, and Ce3d for metal oxide-loaded catalysts. Table 2 shows the binding energies and surface atomic ratios for these metallic elements. The Mn2p3/2 peaks of Mn/Al O , Mn– 2 3 Fe/Al O , Mn–Fe–Mg/Al O , and Mn–Fe–Mg/Al O are 2 3 2 3 2 3 2? 3? attributed to Mn oxides (MnO or Mn(OH) ), Mn 2 4 4? oxides (Mn O or MnOOH), and Mn oxide (MnO ) 2 3 2 (Zhang et al. 2015). The Fe2p3/2 peaks of Fe/Al O , Mn– 2 3 Fe/Al O , Mn–Fe–Mg/Al O , and Mn–Fe–Mg/Al O are 2 3 2 3 2 3 2? 3? related to Fe oxides (FeO or Fe(OH) ) and Fe oxides (Fe O or FeOOH) (Shwana et al. 2015). The surface 2 3 atomic ratios of Fe2p to Al2p (0.011 * 0.018) and Mn2p Catalysts to Al2p (0.014 * 0.016) for catalysts changed little and Fig. 7 COD removal from PRW-ROC by adsorption (a) and over were close to the bulk molar ratio of Fe to Al (0.0129) and single ozonation and various COPs (b); pH value changes of PRW- Mn to Al (0.01547). The asymmetrical distribution of the ROC over single ozonation and various COPs (c): 1 single ozonation, Mg1s peak is likely a result of interactions between Mg, 2 Al O -COP, 3 Fe/Al O -COP, 4 Mn/Al O -COP, 5 Mn–Fe/Al O - 2 3 2 3 2 3 2 3 Mn, and Fe. The surface atomic ratio (0.010) of Mg1s to COP, 6 Mn–Fe–Mg/Al O -COP, and 7 Mn–Fe–Ce/Al O -COP 2 3 2 3 pH values, % COD removals, % COD removals, % 612 Pet. Sci. (2017) 14:605–615 Table 3 Influences of OH Systems COD removals (%) scavengers on COD removals of PRW-ROC using Mn–Fe/ No OH scavenger tBA NaHCO Al O -COP, Mn–Fe–Mg/ 2 3 0.5, g/L 1.0, g/L 0.5, g/L 1.0, g/L Al O -COP, and Mn–Fe–Ce/ 2 3 Al O -COP 2 3 Mn–Fe/Al O -COP 55.8 24.9 22.7 30.5 28.7 2 3 Mn–Fe–Mg/Al O -COP 57.3 37.6 14.9 34.3 31.3 2 3 Mn–Fe–Ce/Al O -COP 56.6 34.9 16.9 31.7 27.8 2 3 0.5 g catalyst, 5 mg/min ozone, 30 C, and 40 min (a) 60 Al2p for Mn–Fe–Mg/Al O is far greater than that in bulk 2 3 (0.0038), suggesting high surface area distribution of the Mg oxide. Similarly the surface atomic ratio (0.004) of Ce3d to Al2p for Mn–Fe–Ce/Al O is higher than that in 2 3 bulk (0.0009), again suggesting high surface area disper- 54 4? sion of Ce oxide (Ding et al. 2016). The surface atomic ratios of the sum of Mn2p ? Fe2p ? Mg1s ? Ce3d to Al2p for Mn–Fe–Mg/Al O , Mn–Fe–Ce/Al O , and Mn– 2 3 2 3 Fe/Al O catalysts were similar to each other and doubled 2 3 compared to Mn/Al O and Fe/Al O . 2 3 2 3 46 Mn-Fe/Al O 2 3 Mn-Fe-Mg/Al O 3.3 Mechanisms of catalytic ozonation 2 3 Mn-Fe-Ce/Al O 2 3 The adsorption onto the catalysts reached saturation by 40 min. Adsorption on Al O , Fe/Al O , Mn/Al O , Mn– 2 3 2 3 2 3 234 5 6789 10 11 12 Fe/Al O , Mn–Fe–Mg/Al O , and Mn–Fe–Ce/Al O con- 2 3 2 3 2 3 Initial pH values tributed to COD removals by 7.3%, 6.6%, 6.6%, 6.1%, 6.5%, and 6.3%, respectively (Fig. 7a). No significant (b) differences for adsorption capacity among catalysts were observed, likely due to similar surface areas (Table 1). pH 10 PZC COD removals using various COPs increased by 23.9%– 11.8% compared with single ozonation (Fig. 7b). These results are significantly greater than simple adsorption Mn-Fe-Ce/Al2O3 (7.3%–6.1%). The observed difference can be attributed to 2 the application of catalytic ozonation. Mn–Fe/Al O 2 3 exhibited better catalytic performance than Mn/Al O and 2 3 pH PZC Fe/Al O , and the introduction of Mg and/or Ce further 2 3 improved the catalytic performance. The active surface areas for all the material comparisons were similar and 4 Mn-Fe/Al O 2 3 would not have an impact on differences in catalytic activity (Table 1). The enhanced catalytic activity of Mn– Fe–Mg/Al O , Mn–Fe–Ce/Al O , and Mn–Fe/Al O pH 2 3 2 3 2 3 PZC resulted from the metal oxide components themselves, interactions between the metal oxides, interactions between the metal oxides and Al O support, as well as its envi- 4 2 3 Ce/Al2O3 ronment (Table 2). Similar relationships between reaction 2 4 6 8 10 12 14 times and COD removals using different COPs were pH values obtained (Fig. 7b), suggesting the similarity of catalytic mechanisms for the various catalysts. Small pH changes in Fig. 8 a Influences of the initial pH values on COD removals using the effluents from single ozonation and COPs were found Mn–Fe/Al O -COP, Mn–Fe–Mg/Al O -COP, and Mn–Fe–Ce/Al O - 2 3 2 3 2 3 compared to that of the initial PRW-ROC (Fig. 7c). COP; and b pH values of three catalysts pzc COD removals, % pH values pH values pH values Pet. Sci. (2017) 14:605–615 613 Several reports have suggested that OH generation catalyst. Initial pH values of 8.3 (Fig. 8a) were close to the induced by catalysts increased removal of pollutants during pH (Fig. 8b) of the three composite catalysts and pzc COP treatment (Qi et al. 2013). In order to identify whether resulted in efficient COD removal. Alkaline pH values these treatments result in the generation of OH, COD around 11 may result in the formation of carbonate and removals in the presence of tBA and NaHCO were bicarbonate during organic mineralization, again decreas- examined. From this it was determined that the COD ing the efficiency of COP (Xiong et al. 2003). The positive removal of PRW-ROC was lessened due to the introduction impact of surface hydroxyl groups (–OH), on active sur- of tBA and NaHCO in bulk (Table 3). NaHCO may faces, has been determined for the removal of organics (Lu 3 3 impair catalytic decomposition of ozone into OH on the et al. 2014; Zhang et al. 2007, 2008). It is believed that pH catalyst surface because of its high affinity to Lewis acid values near the pH of the catalyst can result in acceler- pzc sites on the catalyst surface. In contrast, tBA can quench ated OH generation, due to a neutral –OH state (Qi et al. aqueous ozone decomposition by reacting with OH in 2012). Based on OH quenching experiments and the bulk, generating inert intermediates. As such, the catalytic impact of initial pH values, the surface –OH likely does ozonation of PRW-ROC was dominated by OH both on have a significant role in COP treatment of PRW-ROC. the catalyst surface and in bulk in COPs over Mn–Fe–Mg/ The surface MnOOH and FeOOH of catalysts are the Al O , Mn–Fe–Ce/Al O , and Mn–Fe/Al O . The principle drivers for COP according to XPS results 2 3 2 3 2 3 decreased extent of COD removals by both tBA and (Table 2). The enhanced COD removal compared with NaHCO in Mn–Fe–Mg/Al O -COP and Mn–Fe–Ce/ Mn–Fe–Mg/Al O and Mn–Fe–Ce/Al O may suggest 3 2 3 2 3 2 3 Al O -COP was greater than that in Mn–Fe/Al O -COP. It greater OH-related activity due to interactions between the 2 3 2 3 is reasonable to then expect that the introduction of small various metal oxides and/or changes of metallic states concentrations of Mg or Ce can be used to further promote influenced by the environment. Ozone reacts with surface – OH generation. In addition, the inhibitory effect for OH OH groups during COP treatment and results in highly generation using tBA was greater than that by NaHCO , active OH generation in bulk and/or on the surface, suggesting more OH oxidation occurred in bulk rather than resulting in organics oxidation (Fig. 9). on the catalyst surface. COD was still, however, reduced in spite of the addition of OH scavengers and can be ascribed 3.4 Reusability and stability of catalysts to direct ozonation. Initial pH values that were either acidic, at the pH ,or Catalysts were reused ten times for COD removal from pzc alkaline, significantly influenced the COD removal during PRW-ROC with Al O -COP, Mn–Fe–Mg/Al O -COP, and 2 3 2 3 COP treatment of PRW-ROC (Fig. 8a). An initial pH value Mn–Fe–Ce/Al O -COP. Conditions for experiments 2 3 of 3 resulted in reduced efficiency of COP and was prob- included, 0.5 g catalyst, 5 mg/min ozone, 30 C, 40 min ably a result of the metal species being leached from the treatment, and initial pH values. COD removal from PRW- Solution Intermediates Organics Adsorption OH ·OH Organics OH Metal oxides OH agglomerates Mg or Ce OH Catalysts Mn OH Fe ·OH Organics Intermediates in solution Fig. 9 Proposed ozonation mechanisms of organics in PRW-ROC upon Mn–Fe–Mg/Al O and Mn–Fe–Ce/Al O 2 3 2 3 123 614 Pet. Sci. (2017) 14:605–615 generation and OH-mediated oxidation and are effective at degrading bio-recalcitrant organics in PRW-ROC. The composite metal oxide-loaded Al O -catalyzed ozonation 2 3 exhibited great potential and industrial feasibility for advanced treatment of bio-recalcitrant PRW-ROC. Mn-Fe-Mg/Al O -COP 2 3 Acknowledgements This project was supported in part by the National Science and Technology Major Project of China (No. Mn-Fe-Ce/Al2O3-COP 2016ZX05040-003). 45 Open Access This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creative commons.org/licenses/by/4.0/), which permits unrestricted use, distri- bution, and reproduction in any medium, provided you give appropriate Al2O3-COP credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. 02 46 8 10 References Runs Altenor S, Carene B, Emmanuel E, et al. Adsorption studies of Fig. 10 COD removals in 10 COP runs using Al O , Mn–Fe–Mg/ 2 3 methylene blue and phenol onto vetiver roots activated carbon Al O , and Mn–Fe–Ce/Al O 2 3 2 3 prepared by chemical activation. J Hazard Mater. 2009;165:1029–39. doi:10.1016/j.jhazmat.2008.10.133. Bagastyo AY, Keller J, Poussade Y, et al. 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Petroleum Science – Springer Journals
Published: Jul 13, 2017
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