Evaluation of the potential cationic dye removal using adsorption by graphene and carbon nanotubes as adsorbents surfaces

Akbar Elsagh; Omid Moradi; Ali Fakhri; Fahimeh Najafi; Reza Alizadeh; Vahid Haddadi

doi:10.1016/j.arabjc.2013.11.013

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Original article

10 (

2_suppl

); S2862-S2869

doi:

10.1016/j.arabjc.2013.11.013

Evaluation of the potential cationic dye removal using adsorption by graphene and carbon nanotubes as adsorbents surfaces

Akbar Elsagh^{^a,⁎}, Omid Moradi^{^b,⁎}, Ali Fakhri^{^b}, Fahimeh Najafi^{^c}, Reza Alizadeh^{^d}, Vahid Haddadi^{^e}

a Faculty of Chemistry, Department of Chemistry, North Tehran Branch, Islamic Azad University, P.O. Box: 1913674711, Tehran, Iran

b Department of Chemistry, Shahre-Qods Branch, Islamic Azad University, Shahre-Qods, Iran

c Department of Chemistry, Roudehen Branch, Islamic Azad University, Roudehen, Iran

d Faculty Engineering, Khatam Alanbia University of Technology, Iran

e Department of Chemistry, Islamshahr Branch, Islamic Azad University, Islamshahr, Iran

⁎Corresponding authors. Tel.: +98 2146896000. akbarelsagh@yahoo.com (Akbar Elsagh), o.moradi@shahryaiu.ac.ir (Omid Moradi) moradi.omid@gmail.com (Omid Moradi)

Received: 2013-2-12, Accepted: 2013-11-16, Published: 2013-05-01

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

We are employed in the present study of single-walled carbon nanotubes (SWCNTs), carboxylate group functionalized single-walled carbon nanotubes (SWCNT-COOH), graphene (G) and graphene oxide (GO) as alternative adsorbents for the removal of cationic dye Basic Red 46 (BR 46), from aqueous solution. Various physico-chemical parameters were studied such as electrical conductivity behaviors, contact time, solution pH, and dye concentration. The experimental results show that SWCNTs, SWCNT-COOH, G and GO are promising adsorbents for removing BR 46. The adsorption equilibrium data were analyzed using various adsorption isotherms, and the results have shown that adsorption behavior of BR 46 could be described reasonably well by the Langmuir isotherm. Results showed that the removal of BR 46 increased with increasing initial dye concentration, contact time and pH. Adsorption kinetics data were modeled using the pseudo-first and pseudo-second order, and intra-particle diffusion models. Results show that the pseudo-first order kinetic model for SWCNTs, SWCNT-COOH and the pseudo-second order for G and GO were found to correlate the experimental data well.

Keywords

Adsorption

Basic Red 46 removal

Isotherms

Kinetic models

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1 Introduction

Effluents from the textile industry contain various kinds of synthetic dyestuffs, and there has been increasing scientific interest in regard to decolorization of these effluents in the last few decades (Karadag et al., 2007). Removing color from wastes is often more important than other colorless organic substances, because the presence of small amounts of dyes (below 1 ppm) is clearly visible and influences the water environment considerably (Daneshvar et al., 2003). Many industries, such as plastics, textile, paper and printing use dyes in order to color their products. Most of dye wastes are toxic and even carcinogenic and this poses a serious hazard to aquatic living organisms.

Physical, chemical and biological processes are the principles used in treating dyes in effluent wastewater (Barragán et al., 2007; Habib et al., 2013). Methods used to treat wastewater containing dye include coagulation-flocculation (Rahbar et al., 2006) and advanced oxidation process (Ai et al., 2010). However, these methods are expensive and present operational problems such as the development of toxic intermediates, lower removal efficiency, and higher specificity for a group of dyes, among others (Pelekani and Snoeyink, 2000; Jin et al., 2008). Adsorption is the most versatile and widely used method of water treatment because of its low cost, ease of operation, and efficiency in treatment (Najafi et al., 2013; Saadi et al., 2013).

Adsorption is the transfer of a constituent from a liquid phase to a solid phase. The adsorbent refers to the solid, liquid, or gas phase in which the adsorbate accumulates. The substance that is being removed from the liquid phase is known as the adsorbate (Metcalf and Eddy, 2004). Adsorption processes are the most effective in dye removal compared to other methods of wastewater treatment (Rajamohan, 2009). In industrial processes, adsorption is a crucial step in downstream processing. The behavior of a fixed-bed adsorption column and the adsorption breakthrough analysis can be done using mathematical models. The breakthrough point is important to determine the stopping time of the adsorption operation. This is because the operating time of the adsorption system affects the effectiveness of adsorption by the column (Gupta and Babu, 2009).

Graphene is considered as the mother element of some carbon allotropes, which is a basic building block for graphitic materials of all other dimensionalities, and can be converted into fullerenes, carbon nanotube (CNT) (Sedaghat, 2013), or 3D graphite via wrapping, rolling, or stacking, respectively (Singh et al., 2011). Because of its unique nanostructure, graphene has many novel properties, such as high surface area, excellent electrical conductivity and electron mobility at room temperature, and has unique thermal and mechanical properties (Choi et al., 2010). Graphene oxide (GO) is similar to graphene, but presents oxygen-containing functional groups (Dreyer et al., 2010; Zhu et al., 2012; Kim et al., 2012 ). In comparison with classical adsorbents such as activated carbon and clay, CNTs is more attractive because of its favorable physicochemical stability, high selectivity, and structural diversity. Extensive experiments have been conducted on the adsorption of inorganic or organic contaminants on CNTs such as Zn²⁺ (Lu and Chiu, 2006), Cd²⁺ (Li et al., 2003a,b), Pb²⁺ (Kabbashi et al., 2009), Cu²⁺ (Wu, 2007), Cr⁶⁺ (Di et al., 2006), fluoride (Li et al., 2003a,b) and dioxin (Long and Yang, 2001). Therefore, CNTs might be ideal sorbents for the removal of dyes from water.

Therefore, the present objective of this study is to evaluate the Basic Red 46 removal potential and adsorption ability of the dye using SWCNTs, SWCNT-COOH, G and GO was investigated. Finally, the rates and mechanism of the adsorption process were investigated. The objective of this study is to investigate the effect of Basic Red 46 on contact time, initial concentration, pH and temperature on the adsorption process. Various kinetic evaluations have been used to describe the adsorption process. Here we attempted to apply pseudo first-order rate equation and pseudo second-order and intraparticle diffusion model for the adsorbent phase concentration.

2 Experimental methods

2.1

2.1 Chemicals and reagents

SWCNTs and SWCNT-COOH were purchased from NanoAmor Nanostructured & Amorphous Materials, Inc., USA. SWCNTs (Armchair (6,6), Young’s Modulus (0.94T TPa), Tensile strength (GPa 126.2T), purity, >95; diameter 1–2 nm; length, 5–30 nm; surface area, ∼400 m²/g; and manufacturing method, catalytic chemical vapor deposition (CVD)) and SWCNT-COOH (content of COOH, 6 wt%; with purity >95%; average diameter 1–2 nm; length 5–30 nm and SSA ∼400 m²/g). Purified natural graphene (Monolayer graphene film) was purchased from Sigma–Aldrich Inc. The BR 46 is from the commercial manufacturing company DyStar Co. (Germany). The structure of the dye is given in Fig. 1.

2.2

2.2 Batch adsorption experiments

Tests were carried out with the removal in 100 mL conical flasks containing 20 mL BR 12 and BR 46 solutions in a water bath to elucidate the values of the test parameters including solution pH (2–9), dye concentration (20–80 mg/L), temperature (20–40 °C), contact time (0–90 min) and amount of each adsorbent SWCNTs, SWCNT-COOH, G and GO as adsorbents were equal to 0.05 g. After each removal condition experiment, the samples were centrifuged (2000 rpm, 20 min) for separation of adsorbents from dye solutions and the residual dye molecules concentration in solution was analyzed by a UV–Vis spectrophotometer at 530 nm for BR 46. The kinetic and thermodynamic studies were performed by determining removal conditions. The removal efficiency and adsorption by solid surface as adsorbents, q (mg/g) capacity were calculated with the following equations (Tadjarodi et al., 2013):

(1)

q_{e} = \frac{(C_{i} - C_{f}) V}{W}

where q_e is the concentration of the adsorbed solute, BR 46 (mg/g adsorbent); C_i and C_f are the initial and final (equilibrium) concentrations of the solute in solution (mg/L); V (L) is the volume of the solution and W (g) is the mass of the adsorbent.

2.3

2.3 Preparation graphene oxide (GO)

GO was obtained following a modified Hummers–Offeman method (Zhou et al., 2011). Briefly, graphene (2.0 g), sodium nitrate (1.0 g), concentrated sulfuric acid (98%, 50 mL), and potassium permanganate (6.0 g) were consistently mixed in an ice bath for 2 h, with the mixture gradually becoming pasty and black-greenish. Next, the mixture was placed in a 35 °C water bath and kept at that temperature for 60 min, followed by the slow addition of distilled water (100 mL) to keep the solution from effervescing; the resulting solution was placed well below 100 °C for 3 h. With the progression of the reaction, the color turned a little yellowish. After further treatment with H₂O₂ (5%, 100 mL), the filtered cake was washed with distilled water several times until its supernatant was without ${SO}_{4}^{2 -}$ , as tested using barium chloride (0.1 mM). Then the cake was dispersed in water for further ultra-sonication for 1 h. Of note, for facilitating the following experiments, we selected solutions with GO centrifuged at speeds ranging from 2500 to 5000 rpm. GO-based samples were characterized using various techniques such as the Fourier transform infrared spectrum (FT-IR).

3 Results and discussion

3.1

3.1 Characterization of graphene (G) and graphene oxide (GO) surfaces

Electrical conductivity behavior of graphene was measured 0.005 S/m and for graphene oxide was 0.14 S/m by a conductivity-meter in aqueous solution at 25 °C. These results indicated that electrical conductivity behavior of graphene improved by oxidation of graphene. The FTIR pattern of graphene has a characteristic peak at 1610 cm⁻¹ due to the aromatic C⚌C skeletal vibrations are shown in Fig. 2a. The FTIR pattern of GO, which is shown in Fig. 2b, reveals the presence of the oxygen-containing functional groups. The peaks at 1071, 1380, 1630 correspond to C–O–C stretching vibrations, C–OH stretching, C–C stretching mode of the sp² carbon skeletal network, respectively, while peaks located at 1730 and 3440 cm⁻¹ correspond to C–O stretching vibrations of the COOH groups and O–H stretching vibration, respectively (Fan et al., 2013).

Fourier transform infrared spectrum (FT-IR) for pristine graphene (a) and oxidized graphene (b).

3.2

3.2 Effect of contact time and dye concentration

The effect of contact time on the adsorption of BR 46 by SWCNTs, SWCNT-COOH, G and GO surfaces as adsorbents is shown in Fig. 3. The experiments were carried out at 60 mg/L initial dye for and concentration with 0.05 g adsorbent mass for adsorbent surfaces at temperatures of 25 °C. The amount of each dye adsorbed increased with increase in contact time and reached equilibrium after 80 min for SWCNTs, SWCNT-COOH and 90 min for G and GO.

Effect of contact time on the adsorption of BR 46 by SWCNTs, SWCNT-COOH, G and GO surfaces, (temperature: 298 K, mass each of adsorbent: 0.05 g and pH 9).

Effect of initial concentration on BR 46 adsorption by SWCNTs, SWCNT-COOH, G and GO as adsorbent surfaces is shown in Fig. 4. Furthermore, the amount adsorption dye is increased with the increase in initial dye concentration. It is because of the fact that at higher concentration, the ratio of the initial number of dye molecules to the available surface area is high and subsequently the fractional adsorption becomes independent of initial concentration. However, at high concentration the available sites of adsorption becomes more and hence the adsorption of dye depends upon concentration (Al-Rashed and Al-Gaid, 2012).

Effect of initial BR 46 concentration on adsorption of BR 46 by SWCNTs, SWCNT-COOH, G and GO surfaces, mass each of adsorbents = 0.05 g, initial pH 9 and Temperature 298 K.

3.3

3.3 Effect of pH

The pH is one of the most important factors controlling the adsorption of dyes onto suspended particles, because both adsorbed molecules and adsorbent particles may have functional groups which are affected by the concentration of hydrogen ions (H⁺) in the solution and which are involved in the molecular adsorption process at the active sites of the adsorbent. The pH of the dye solution affects not only the surface charge of the SWCNTs, SWCNT-COOH, G and GO surfaces adsorbents, the degree of ionization of the materials and the dissociation of functional groups on the active sites of the adsorbents surface, but also the structure of the dye molecule (Lin and Leu, 2008). The results of the pH studies at different pH values are shown in Fig. 5. Adsorption capacity of the BR 46 increased with increasing pH and reached a maximum level at the pH of 9.0. Similar pH trends were also reported by other researchers (Nandi et al., 2009). The lower adsorption of BR 46 by surfaces adsorbents at low pH values may be explained by the competition of excess H⁺ ions with the dye cation for active adsorption sites (Batzias and Sidiras, 2007). However, it did not explain the slight decrease of the dyes by both surfaces adsorption at higher pH values.

Effect of initial pH of solution on adsorption of BR 46 by SWCNTs, SWCNT-COOH, G and GO surfaces, mass each of adsorbents = 0.05 g, initial pH 9, and Temperature 298 K.

3.4

3.4 Adsorption isotherms

From the various isotherm equations that may be used to analyze adsorption data in aqueous phase, the Langmuir (Najafi et al., 2013; Ayad and El-Nasr, 2012)—the theoretical equilibrium isotherm and the Freundlich (Najafi et al., 2013; Moradi et al., 2012)—the empirical equilibrium isotherm are the most common models. The linear forms of these equations are displayed as equation (2) (Langmuir) and (3) (Freundlich):

(2)

\frac{1}{q_{e}} = \frac{1}{q_{m}} + \frac{1}{K_{L} q_{m} C_{e}}

(3)

\log q_{e} = \log K_{F} + \frac{1}{n} \log C_{e}

where q_m (mg g⁻¹) is the maximum adsorption capacity, q_e (mg g⁻¹) is the amount of adsorbed 4C2NP, C_e (mg L⁻¹) is the equilibrium BR46 concentration, K_F and n are the Freundlich constants, and K_L (L mg⁻¹) is the Langmuir constant. The Langmuir and Freundlich parameters, along with the coefficients of determination (r²) of the linear plots, are presented in Table 1. Adsorption of BR46 on SWCNTs, SWCNT-COOH, G and GO surfaces can be fitted by the Langmuir model.

Table 1 Isotherm constants for the adsorption of BR 46 by adsorbents.

Isotherm	Langmuir			Freundlich
Isotherm	q_m(mg/g)	K_L(L/mg)	r²	K_F	1/n	r²
SWCNTs	38.35	1.71	0.942	16.12	0.233	0.912
SWCNT-COOH	49.45	1.57	0.955	15.11	0.458	0.931
G	30.52	2.24	0.972	18.23	0.184	0.927
GO	55.57	1.25	0.984	14.21	0.519	0.939

3.5

3.5 Kinetics study

The adsorption process on a porous adsorbent in a stirring chamber generally involves several transport stages (Robati, 2013); external diffusion, internal diffusion, and actual adsorption. Although many theoretical model equations have been proposed to describe the adsorption kinetics based on mass balance, pore diffusion rate, and initial/boundary conditions, these equations are not only complicated and impractical in industry, but also require detailed data such as the characteristics of adsorbate and adsorbent. The conformity between experimental data and the model predicted values was expressed by the correlation coefficient (r², values close or equal to 1). A relatively high r² value indicates that the model successfully describes the kinetics of BR46 adsorption.

3.6

3.6 Pseudo first-order model

The sorption kinetics may be described by a pseudo first order equation (Hossain et al., 2005; Özacar, 2003; Robati, 2013; Ho and Chiang, 2001 ). The linear form equation is as follows:

(4)

\log (q_{e} - q_{t}) = \log (q_{e}) - k_{1} t

where q_e and q_t are the amounts of dye adsorbed at equilibrium and at time (mg/g), respectively, and is the equilibrium rate constant of pseudo first-order adsorption, (1/min). Fig. 6 shows a plot of linearization form of pseudo first-order model. The slopes and intercepts of plots of versus were used to determine the pseudo first-order constant and equilibrium adsorption. However, the experimental data deviated considerably from the theoretical data. A comparison of the results with the correlation coefficients is shown in Table 2. The correlation coefficients for the pseudo first order kinetic model obtained at all the studies concentrations were high for SWCNTs, SWCNT-COOH. This suggests that this adsorption system is a pseudo first-order reaction (Fig. 7).

Plot of the pseudo first-order kinetics for adsorption of BR46.

Table 2 Comparison of the kinetic models for adsorption of BR46.

Kinetic model	SWCNTs	SWCNT-COOH	G	GO
Pseudo-first-order
q_e (mg/g)	137.52	126.64	0.0075	0.3624
k₁ (1/min)	0.0076	0.0105	0.0027	0.0252
r²	0.9978	0.9973	0.9929	0.9960

Pseudo-second-order
q_e (mg/g)	149.25	227.27	3.194	50.00
k₂ (g/mg min)	0.0004	0.0009	2.4449	0.0740
r²	0.9909	0.9901	1.0000	1.0000

Intra particle diffusion
K_i (mg/g min^0.5)	13.464	15.254	0.3844	5.1805
C (mg/g)	6.3588	27.312	0.3715	2.6327
r²	0.9954	0.9970	0.9789	0.9939

Plot of the pseudo second-order kinetics for adsorption of BR46.

3.7

3.7 Pseudo second-order model

The adsorption kinetics may also be described by a pseudo second-order equation (Özacar, 2003; Robati, 2013; Ho and Chiang, 2001 ). The linear form equation is as follows:

(5)

t / q = 1 / k_{2} q_{e}^{2} + t / q_{e}

where k₂ is the equilibrium rate constant of pseudo second-order adsorption (g/mg.min). The slopes and intercepts of plots t/q versus t were used to calculate the pseudo second-order rate constants k₂ and q_e. The straight lines in plot of t/q versus t (Fig. 8) show good agreement of experimental data with the pseudo second-order kinetic model for different initial dye concentrations. Table 2 lists the computed results obtained from the pseudo second-order kinetic model. These indicate that the adsorption system studied belongs to the second order kinetic model.

Plot of the intra-particle diffusion model for adsorption of BR46.

3.8

3.8 The intra-particle diffusion model

The intra-particle diffusion model is expressed as (Moradi and Zare, 2011; Moradi et al., 2013):

(6)

q = k_{i} t^{1 / 2} + C

where C is the intercept and k_i is the intra-particle diffusion rate constant (mg/g h^0.5), which can be evaluated from the slope of the linear plot of q versus t^1/2. Fig. 8 shows a plot of the linearized form of the intra-particle diffusion model.

As can be seen from these figures, the pseudo first-order kinetic model provides the best correlation for all of the adsorption process, whereas the other models fits the experimental data well not for initial periods of the adsorption process only. Hence it was concluded that the pseudo second-first kinetic model was found to be rate limiting.

4 Conclusions

Single-walled carbon nanotube (SWCNTs), carboxylate group functionalized single-walled carbon nanotube (SWCNT-COOH), graphene (G) and graphene oxide (GO) can be used as effective adsorbents for removing Basic Red 46 from contaminated water sources. Increasing the temperature decreased the BR46 adsorption rate but the maximum adsorption capacity was similar. The adsorption isotherms are fitted by the Langmuir equation. The pseudo first-order kinetic model for SWCNTs, SWCNT-COOH and the pseudo second-order kinetic model for G and GO accurately described the adsorption kinetics. The adsorption mechanism was found to be physic-sorption and the rate-limiting step was mainly surface adsorption.

Acknowledgements

This project was financial support by the Islamic Azad University, North Tehran Branch of Iran.

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Show Sections

[1] Ai Z., Li J., Zhang L., Lee S., . Rapid decolorization of azo dyes in aqueous solution by an ultrasound-assisted electrocatalytic oxidation process. Ultrason. Sonochem.. 2010;17:370-375.
[Google Scholar]

[2] Al-Rashed S.M., Al-Gaid A.A., . Kinetic and thermodynamic studies on the adsorption behavior of rhodamine B dye on Duolite C-20 resin. J. Saudi Chem. Soc.. 2012;16:209-215.
[Google Scholar]

[3] Ayad M.M., El-Nasr A.A., . Anionic dye (acid green 25) adsorption from water by using polyaniline nanotubes salt/silica composite. J. Nanostruct. Chem.. 2012;3:3.
[Google Scholar]

[4] Barragán B.E., Costa C., Carmen Marquez M., . Biodegradation of azo dyes by bacteria inoculated on solid media. Dyes Pigm.. 2007;75:73-81.
[Google Scholar]

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Evaluation of the potential cationic dye removal using adsorption by graphene and carbon nanotubes as adsorbents surfaces

Abstract

Keywords

Adsorption

Basic Red 46 removal

Isotherms

Kinetic models

1 Introduction

2 Experimental methods

2.1 Chemicals and reagents

2.2 Batch adsorption experiments

2.3 Preparation graphene oxide (GO)

3 Results and discussion

3.1 Characterization of graphene (G) and graphene oxide (GO) surfaces

3.2 Effect of contact time and dye concentration

3.3 Effect of pH

3.4 Adsorption isotherms

3.5 Kinetics study

3.6 Pseudo first-order model

3.7 Pseudo second-order model

3.8 The intra-particle diffusion model

4 Conclusions

Acknowledgements

References

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