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Original article
13 (
1
); 1712-1719
doi:
10.1016/j.arabjc.2018.01.008

Optimisation of the removal conditions for heavy metals from water: A comparison between steel furnace slag and CeO2 nanoparticles

, , , , ,
a Instituto de Ingeniería, Coordinación de Ingeniería Ambiental, Universidad Nacional Autónoma de México (UNAM), Mexico
b Departamento de Ingeniería Química, Biológica y Ambiental, Escola d’Enginyeria, Universitat Autònoma de Barcelona, Spain
c Facultad de Ingeniería, Departamento de Materiales y Manufactura, DIMEI, Universidad Nacional Autónoma de México, Mexico

⁎Corresponding author at: Instituto de Ingeniería, Coordinación de Ingeniería Ambiental, Universidad Nacional Autónoma de México, Cd. Universitaria, Coyoacán 04510, Ciudad de México, Mexico. rmrz@pumas.iingen.unam.mx (R.M. Ramírez-Zamora) RRamirezZ@iingen.unam.mx (R.M. Ramírez-Zamora)

Received: , Accepted: ,
© The Author(s) 2018
Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Peer review under responsibility of King Saud University.

Abstract

This work studies an innovative approach to water treatment by using recycled electric induction furnace slag for the removal of Cd, Cr and Pb-ions and comparing the results to a treatment with specifically developed CeO2 nanoparticles. The slag was characterised by X-ray Fluorescence, X-ray diffraction and SEM. The effects of initial ion concentration and adsorbent dose were investigated according to an experimental design. Adsorption tests were carried out with ion solutions present in concentrations ranging from 1 to 10 mg/L and adsorbent doses from 0.064 to 0.64 g/L. The removal mechanism for CeO2 is adsorption. For slag, literature proposes a mechanism involving chemical adsorption of Cd2+, Cr6+ and Pb2+ by silanol and aluminol groups; precipitation in the form of metal silicates formed between the cations and silicic acid leached from the slag provides an alternative explanation. The removal efficiencies with nanoparticles are higher than reported for any other adsorbent (including slag) under all test combinations for the three metals investigated. The maximum removal efficiency with slag was 74% for Cr6+, 64% for Cd2+ and 34% for Pb2+, comparable to, or higher than, other materials reported in literature. The treatment with slag has clear promises in terms of economy and scalability.

Keywords

Electric induction furnace slag
CeO2
Nanoparticles
Waste valorisation
Heavy metals
Water treatment
1

1 Introduction

Over the last two centuries, industrialization has contributed to the release of toxic heavy metals into water streams. The main sources of heavy metal contamination are mining, electroplating, metal processing, textile, battery manufacturing, tanneries, petroleum refining, paint manufacture, pesticides, pigment manufacture, printing and photographic industries (Ahmaruzzaman, 2011). Exposure to heavy metals, even at trace level, represents considerable risks for human health (WHO, 2006).

Various technologies are available to remove heavy metals from aqueous solutions, including ion exchange (Kononova et al., 2019; Wang et al., 2016), nanofiltration (Nedzarek et al., 2015), phytoremediation (Mahar et al., 2016), remediation by means of fungi and bacteria (Liu et al., 2017) electrodialysis (Ebbers et al., 2015), complexation-adsorption (Houari et al. 2019) and adsorption on nanosized metal oxides (Recillas et al., 2010, 2011; Contreras et al., 2012; Insanullah et al., 2016) or on modified carbon nanotubes (Salam et al., 2019). A recent review on the use of nanotechnology in wastewater remediation was provided by Anjum et al. (2019).

Although these processes have good removal efficiencies, they have the disadvantage that they require relatively costly reagents, which increases the cost of water treatment (Bhatnagar and Sillanpää et al., 2010). Barakat (2011) provides a review of cheaper and more effective technologies with adsorbents of mineral, organic or biological origin, zeolites, industrial by-products, agricultural wastes, biomass, and polymeric materials.

Although it is commonly assumed that most of these products remove contaminants by adsorption (Srivastava et al., 1997; Ortiz et al., 2001; Ćurković et al., 2001; Bonenfant et al., 2009; Chen et al., 2011; Oh et al., 2012; Hu et al., 2012; Mercado-Borrayo et al., 2014), various studies point to mechanisms of coagulation/precipitation (Zhang and Itoh, 2005), ion exchange (Kolodynska et al., 2017) or complexation (Dimitrova, 1996).

Steel slag is an industrial by-product which is generated in very large volumes (Xue et al., 2009). The slag consists mainly of oxides and hydroxides. It has been hypothesised that the oxides in the slag could provide adsorption sites for anions. Hydroxides can also increase the pH of the surrounding system and catalyse the precipitation of dissolved heavy metal cations (Dimitrova, 1996; Oh et al., 2012).

In the beginning of the 21st century, the yearly production of steel slag in Europe and USA was around 20 million tons and in China and Japan 17 million tons (Shen and Forsseber, 2003). Mexico is the second largest producer of steel and iron in Latin America, with a production of 18.228 MT in 2016, which generates 3646 MT of slags (CANACERO, 2017).

Although most slag is still being disposed off in landfills, applications as aggregates in hydraulic concretes (Setién et al., 2009), in asphalt pavements (Huang et al., 2007) and for soil improvement (Poh et al., 2006) are becoming more common. During the past decade, studies focused on the use of slag in water treatment applications have been reported because of its availability and chemical composition, which may allow using this material as an adsorbent for metals (Ahmed and Ahmaruzzaman, 2016), phosphate (Han et al., 2016), dye (Gao et al., 2017) and as a heterogeneous Fenton-like catalyst for the degradation of different organic compounds (Cheng et al., 2016; Nasuha et al., 2016; Cheng et al., 2017).

This study compares two emerging technologies for removal of heavy metals. On the one hand, CeO2 nanoparticles present a high-technology solution which promises high removal efficiencies (Recillas et al., 2010, 2011; Contreras et al., 2012). Steel slag may be an interesting alternative where high-tech solutions are less feasible (Penn et al. 2012; Kõiv et al., 2016; Mercado-Borrayo et al., 2018). The work analyses the optimisation of the removal process for, cadmium, chromium and lead in water and compares both materials. To achieve this, an experimental design was executed to obtain reliable and statistically validated results. The factors in the study were initial ion concentration and adsorbent dose.

2

2 Materials and methods

2.1

2.1 Materials

Synthesis and characterisation of the CeO2 nanoparticles has been described in previous studies (Recillas et al., 2010, 2011; Contreras et al., 2012). Particles are synthesised in aqueous phase by oxidising Ce3+ from Ce(NO3)3 salt to Ce4+ under basic conditions by means of hexamethylenetetramine, which also serves to stabilise the nanoparticles, preventing agglomeration by the formation of a double layer at the particle surface (Recillas et al., 2010, 2011). The hydrodynamic diameter of the particles, measured by means of dynamic light scattering showed an approximately Gaussian distribution with mean 11.7 nm and standard deviation of 1.6 nm. The ζ-potential was +11.5 mV and the specific surface area, determined by physical adsorption of nitrogen gas (BET-isotherm), was equal to 65 m2/g.

The steel slag was produced in an electric induction furnace at a metallurgical plant located in the metropolitan area of Mexico City. It was ground and sieved into particle sizes ranging from 44 to 149 μm before further characterisation.

X-ray Fluorescence (XFR) measurements were carried out in triplicate on a Siemens (Burladingen, Germany) SRS 3000 fluorescent spectrometer. The sample (10 g) was calcinated for 1 h at 1000 °C to determine loss on ignition. The detection limit for each element reported as metal oxide is shown in Table 1. X-ray diffraction (XRD) was carried out using a Bruker D8 Advance diffractometer equipped with Bragg-Brentano geometry, a θ-θ configuration, Cu Kα radiation, and a Bruker Lynxeye detector. The diffraction intensity was measured in a 2θ range from 10 to 70°.

Table 1 X-ray fluorescence results of steel slag used in environmental applications.
%Fe2O3 %CaO %MgO %Al2O3 %SiO2 %MnO Environmental applications Reference
29.4 31.7 10.3 11.9 10.9 3.29 Phosphorus, fluoride and metals removal Claveau-Mallet et al. (2013)
25.2 28.8 14.5 7.7 14.5 7.96 Phosphorus, fluoride and metals removal Claveau-Mallet et al. (2013)
0.78 38.47 9.39 8.42 27.20 nr Ni, As and Sb removal Luukkonen et al. (2016)
0.71 29.87 6.38 5.87 25.81 nr Ni, As and Sb removal Luukkonen et al. (2016)
41.7 22.5 10.6 7.9 13.3 1.5 As removal Mercado-Borrayo et al. (2014)
13.3 2.9 3.8 16.7 55.1 6.8 This work
0.006 0.04 0.015 0.018 0.05 0.004 This work

All values in weight percent, nr = not reported.

Scanning electron microscope (SEM) was performed on a Philips XL20 Scanning Electron Microscope with standard Eberhard-Thornley secondary electron detector and solid-state backscattered electron (BSE) detector. Observations were made on uncoated samples using atomic number contrast with BSE at an accelerating voltage of 30 kV. Energy dispersive X-ray spectroscopy was executed with a solid-state Oxford 7593 detector.

The specific surface area, pore volume and average pore diameter were determined by the nitrogen physical adsorption technique (Brunauer-Emmett-Teller (BET) isotherm) using a BELSORP Mini II (Japan). The detection limit for specific surface area is 0.01 m2/g and for pore volume is 0.025 μL/g. The measurement accuracy is 0.5%.

2.2

2.2 Removal of Cd2+, Cr6+ and Pb2+ ions

Laboratory solutions for adsorption experiments for each of the heavy metals were prepared using the following reagents: Cd2+ (cadmium nitrate at 99.999% purity, Aldrich, Spain), Cr6+ (potassium dichromate at 99.5% purity, Panreac, Spain) and Pb2+ (lead nitrate at 99.999% purity, Aldrich, Spain). Removal experiments for each of the metals were performed separately and contaminant doses were chosen at levels which are representative for industrial waste waters (Recillas et al., 2010, 2011; Contreras et al., 2012).

The adsorption experiments were carried out in a batch system with Cd2+, Cr6+ and Pb2+ at 1, 5.5 and 10 mg/L in deionized water. Slag doses were 0.064, 0.352 and 0.64 g/L, based on earlier studies in which slag was used to remove As and B (Mercado-Borrayo et al., 2013; Schouwenaars et al., 2017). To allow quantitative comparison, nanoparticle doses were set at the same levels. The experiments were performed at pH 5.5 using 24 h of adsorption time at room temperature. These conditions ensured that the adsorption equilibrium was reached in all cases (Contreras et al., 2012; Schouwenaars et al. 2017).

This study used a 32 experimental design with four replicates at the central point (Montgomery, 2008), resulting in 12 experiments for each of the six combinations of contaminant and sorbent. The factors were Cd2+, Cr6+ and Pb2+ concentrations and the sorbent dose. The response variable studied is the removal efficiency of heavy metals. Data analysis was performed using the statistical functions included in Mathematica®.

2.3

2.3 Cd2+, Cr6+ and Pb2+ quantification

Calibration curves for the colorimetric quantification of heavy metals were constructed using standard solutions ranging from 1 to 10 mg/L of Cd2+, Cr6+ and Pb2+, based on the reaction of cadmium and lead with dithizone to form a complex that is extracted with chloroform (Ármannsson, 1979) and chromium with dyphenylcarbazide (Urone, 1955). The detection limit in all cases is 0.01 mg/L. The correlation coefficients of the calibration curves for Cd2+, Pb2+ and Cr6+ were 0.97, 0.98 and 0.98 respectively.

2.4

2.4 Sorption capacity

Given the number of experiments (72) executed under the experimental design described in Section 2.2, no additional kinetic or isotherm measurements were performed. From earlier work, it is known that no measurable contaminant removal occurs after 24 h. of exposure (Recillas et al., 2010, 2011; Contreras et al., 2012; Mercado-Borrayo et al., 2013; Schouwenaars et al., 2017). Sorption capacity was calculated as the amount of contaminant removed divided by the sorbent dose after 24 h. of contact.

3

3 Results

3.1

3.1 Slag characterisation

Table 1 shows the main slag constituents identified by XRF, which are iron, aluminium and silicon, compared to values reported in the literature for other slags used in environmental applications. Fig. 1 provides the XRD-results for the present slag, some of the compounds found may have adsorption properties for metallic ions such as silanol or aluminol surface groups which, after a hydroxylation process, can remove dissolved metal ions such as Zn2+, Cd2+, Cu2+ and Ni2+ (Xue et al., 2009; Doménico and Peral, 2006). According to this mechanism, steel slag is a good candidate to remove heavy metals according to the reaction shown in Fig. 2.

XRD-results for the EIFS. Silicates, aluminates and iron oxides are all well-known adsorbents for metals and metalloids (Xue et al., 2009; Doménico and Peral, 2006).
Fig. 1 XRD-results for the EIFS. Silicates, aluminates and iron oxides are all well-known adsorbents for metals and metalloids (Xue et al., 2009; Doménico and Peral, 2006).
Reactions for the removal of heavy metals by silanol (Doménico and Peral, 2006).
Fig. 2 Reactions for the removal of heavy metals by silanol (Doménico and Peral, 2006).

Nitrogen adsorption results are presented in Table 2. The slag has a low specific surface of 0.8 m2/g. The granular aspect of the slag used is shown in Fig. 3. It is important to point out that slag, contrary to conventional high-purity reagents, is a heterogeneous material. This is seen in Fig. 3b. and the corresponding Table 3, where EDX-results for 10 particles are summarised as an example (see Fig. 4).

Table 2 Nitrogen adsorption results for the slag. Results related to pore volume and diameter should be interpreted with care, because the data show that the material is essentially non-porous. (μ = mean, σ = standard deviation for three measurements).
Specific surface area (m2/g) Pore volume (cm3/g) Pore diametre (nm)
μ 0.8 3.2 E-03 19
σ 0.1 0 0
SEM-images of the granulated slag. 3a gives a general view of granulometry, 3b provides detail of the central part of 3a, illustrating the morphological and compositional heterogeneity of the powder. Areas where EDX was performed are indicated in the image, results are tabulated in Table 3.
Fig. 3 SEM-images of the granulated slag. 3a gives a general view of granulometry, 3b provides detail of the central part of 3a, illustrating the morphological and compositional heterogeneity of the powder. Areas where EDX was performed are indicated in the image, results are tabulated in Table 3.
Table 3 Chemical composition (wt%) of the particles identified in Fig. 3b.
Spectrum Na Mg Al Si S K Ca Ti Cr Mn Fe
1 9.2 4.1 7.8 40.1 2.1 36.8
2 3.6 3.8 1.4 91.1
3 49.2 42.2 8.6
4 4.2 19.1 5.6 41.8 3.5 3.6 3.6 18.6
5 2.7 4.5 12.2 48.7 1.2 5.4 25.4
6 6.4 9.2 7.5 40.8 1.3 6.8 28.0
7 2.3 29.7 1.8 61.5 1.2 3.6
8 5.8 15.2 4.4 39.8 1.3 31.1 2.5
9 18.3 73.2 3.6 5.0
10 67.6 32.4
11 6.6 60.8 18.6 10.6 3.4
Response surface for the removal of Cd2+, Cr6+ and Pb2+-ions with CeO2 nanoparticles and slag. The nanoparticles remove up to 100% of the contaminants over a wide range of experimental conditions. The results for slag provide high removal efficiency at low contaminant levels and high slag doses, the response surfaces indicate that an increase in slag dose will allow for higher removal efficiencies. (Parts of the response surface which are not plotted correspond to parameter values where a removal of 100% is predicted).
Fig. 4 Response surface for the removal of Cd2+, Cr6+ and Pb2+-ions with CeO2 nanoparticles and slag. The nanoparticles remove up to 100% of the contaminants over a wide range of experimental conditions. The results for slag provide high removal efficiency at low contaminant levels and high slag doses, the response surfaces indicate that an increase in slag dose will allow for higher removal efficiencies. (Parts of the response surface which are not plotted correspond to parameter values where a removal of 100% is predicted).

3.2

3.2 Optimisation of adsorption experiments

The levels for the experimental design are shown in Table 4. The experiments were fitted to a polynomial equation (Eq. (1)):

(1)
f ( x , y ) = a 00 + a 10 x + a 01 y + a 11 xy + a 20 x 2 + a 02 y 2 + a 21 x 2 y + a 12 xy 2 + a 22 x 2 y 2 where f(x, y) is the response function (% removal), the aij are the fitting coefficients, x the slag dose in g/L and y the contaminant dose in mg/L. This polynomial has equal number of fitting coefficients as there are experimental points in the scheme; a statistical analysis can be performed by comparing the effects aij to the standard deviation measured at the central point.
Table 4 Natural and coded values of factors used in factorial design.
Level Dose of adsorbent (g/L) Metal concentration (mg/L)
−1 0.064 1
0 0.352 5.5
1 0.64 10

The fitting constants are given in Table 5 for coded values of the experimental variables. The value of a00 gives the average value at the central point, a01 is the main effect of slag (nanoparticle) dose which is the most important factor. The value a10 gives the main effect of metal concentration and is much smaller, but metal concentration plays a strong role through the first-order interaction effect a11. As a consequence, for all six cases, the maximal removal efficiency (Table 6) is found at minimal metal concentration and high reagent dose. For Cd-removal by nanoparticles, the 9 combinations of variables tested have such a high efficiency that only a00 is significant.

Table 5 Fitting parameters for Eq. (1) as applied to the coded values of the six experimental data sets. By using coded values, the value of a00 gives the average value at the central point, a01 is the main effect of slag dose, a10 is the main effect of metal concentration, a11 is the first order interaction between dose and concentration; σ is the corresponding standard deviation (4 replicates at the central point).
a00 a10 a01 a11 a20 a02 a21 a12 a22 σ
CeO2 nanoparticles Cd2+ 96.7 NS NS NS NS NS NS NS NS 2.3
Slag Cd2+ 55.4 9.3 NS −29 −10.7 NS NS NS 20.8 5
CeO2 nanoparticles Cr6+ 97.5 1.4 −1.1 NS −1.2 13 NS NS −13.1 0.7
Slag Cr6+ 61.1 19.1 NS −23.2 −11.7 NS −5.6 5.7 8.5 1.8
CeO2 nanoparticles Pb2+ 67.7 −7.3 NS −8.4 −5.4 NS NS 14.5 12.8 2.5
Slag Pb2+ 18.8 9.9 −1.7 −3.3 −5.4 −1.4 −1.9 −1.3 3.6 0.2

NS indicates non-significant effects.

Table 6 Estimated optimal removal conditions for heavy metals using CeO2 nanoparticles and slag.
Maximum removal (%) Adsorbent dose (g/L) Heavy metal concentration (mg/L) qe (μg/mg)
CeO2 nanoparticles Cd2+ 100 0.5 1 150
Slag Cd2+ 64.4 0.6 1 21
CeO2 nanoparticles Cr6+ 99.9 0.4 1 122
Slag Cr6+ 76.8 0.6 1 16
CeO2 nanoparticles Pb2+ 91.4 0.6 1 9.6
Slag Pb2+ 34.3 0.6 1 6.6

The maximal achieved removal efficiency and a00 can both be used to compare the performance of slag and nanoparticles with respect to each of the pollutants. Nanoparticles are clearly more efficient in the testing range explored here, particularly for Cd2+ and Cr6+, where complete removal is achieved. Pb2+ is more problematic with slag and with nanoparticles. The lower efficiency of slag should not be considered problematic in terms of the valorisation of this waste product. Already under the present experimental conditions, residual concentrations obtained for chromium (0.24 mg Cr6+/L) and lead (0.66 mg Pb2+/L) are low enough to allow using the treated water for irrigation (US EPA, 2004). Also, the response surfaces clearly indicate that higher removal efficiencies can be achieved at higher slag doses or in a two-step process.

Another way to evaluate the results is by comparing the sorption capacity qe (μg/mg) obtained in this work to values reported in literature. Data on Cd2+ are scarce; the value of 150 μg/mg for CeO2 nanoparticles obtained in this work is higher than a previously reported result of 101 μg/mg for the same material (Contreras et al., 2012). For this pollutant, slag is clearly less efficient with a qe of 21 μg/mg.

For Cr6+, the present work reproduces the result of Recillas et al. (2010), with qe = 122 μg/mg. This is significantly higher than the 1.5 μg/mg reported for CeO2 microparticles and 0.4 μg/mg for commercial CeO2 (Di et al., 2006), Results of Zhong et al. (2007) for CeO2 nanoparticles (70 μg/mg) and for a CeO2 micro-nano composite structure are (26 μg/mg) also lower than what is reported here. Removal of Cr6+ with other adsorbents produced values of qe of 10 μg/mg using activated carbon, 7.5 μg/mg for γ-alumina (Zhong et al., 2007) and 0.23 μg/mg for slag (Srivastava et al., 1997). These values are significantly lower than what was obtained in this study using slag, i.e. qe = 16 μg/mg.

For Pb2+, Mishra and Paterl (2009) compared several materials. They report a qe of 7.6 μg/mg for bentonite, 6.7 for active carbon, 5.2 for slag, 5.0 for fly ash and 4.5 for caolin. Srivastava et al., 1997 reached qe = 7.6 μg/mg for slag. The present work reaches 9.6 μg/mg using CeO2 nanoparticles, which is almost equal to the 10.3 μg/mg reported earlier (Recillas et al., 2011). With slag, 6.6 μg/mg of Pb2+ is removed.

In summary, the CeO2 nanoparticles tested in this study are superior, by a wide margin, to the other materials reported in literature. It is also clear that their high surface area, which is derived from the small particle diameter, is an essential element in their use. Hu et al. (2008) argue that the removal mechanism consists either of chemisorption by ion exchange at the surface of the oxide or by the formation of bidentate surface complexes.

The removal capacity of slag compares favourably to other reagents (except CeO2). The low specific surface area of the slag argues against adsorption as the main mechanism. A monolayer adsorption mechanism as suggested by Fig. 2 would saturate the available surface of 0.8 m2/g relatively quickly. An alternative reaction mechanism was proposed by Dimitrova (1996), who provides evidence that the formation of insoluble silicates occurs in the aqueous phase, leading to the precipitation of metal silicates on the slag surface. This question will be addressed into more detail in future research.

Production of nanoparticles requires the use of high-purity specialised reagents. After use, the particles must be regenerated and the regeneration medium must in turn be treated, which increases the cost of the process. Slag, being a high-volume waste product from steel industry has a negative value, i.e. industry must pay to discard it. However, the raw slag must be ground and transported from the steel plant to the water treatment plant. Both operations may generate considerable costs. Once used, the slag is not regenerated but can be stabilised, for example by using it as a fine aggregate in concrete and road surface material, which is already a common use for metallurgical slag. Preliminary tests have shown that stabilisation in cementitious materials produces a non-hazardous residue.

4

4 Conclusions

The CeO2 nanoparticles used in this work were chosen as a reference material because they have one of the highest removal efficiencies for heavy metals reported in literature. This was confirmed in the present study: removal capacities for Cd2+ and Cr6+ were found to be higher than reported in previous work, while the results for Pb2+ were comparable. Considering the known surface properties of CeO2 and the high surface area of the nanoparticles, it can be safely concluded that removal occurs through an adsorption mechanism for this material.

The performance of electric induction furnace slag was comparable or slightly better than other reagents reported in literature (except CeO2). The maximum removal efficiencies were: Cr6+ 74%, Cd2+ 64% and Pb2+ 34%, giving residual concentrations of Cr6+ and Pb2+ in water below the criteria for irrigation purposes. For slags, an adsorption mechanism by aluminol and silanol compounds has been postulated. However, given the low specific surface area, it is unlikely that this is the main removal process. Precipitation with silicate ions lixiviated from the slag may be an alternative explication.

Both materials studied are highly promising with regard to applications. CeO2 nanoparticles require careful synthesis from pure precursors and must be regenerated after use, which will increase the cost of water treatment. However, in high-technology environments where the high removal capacity of this material is required, they may present the optimal solution. Steel slag is a waste material which is massively available. It can be neutralised and disposed of after use. This makes it a promising material for use in smaller, low technology treatment plants, for example in rural settings and developing countries.

Acknowledgements

B.M. Mercado-Borrayo gratefully acknowledges the financial support through the PhD Scholarship from “Coordinación de Estudios de Posgrado”, Universidad Nacional Autónoma de México (CEP, UNAM). R. Contreras acknowledges Becas en el extranjero (2011–2014) CONACYT. The authors acknowledge the financial support of DGAPA under fund IV100616, which provided the resources required to complete this investigation.

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