Adsorptive Removal of Toxic Dye Using Fe3O4–TSC Nanocomposite

Article pubs.acs.org/jced

Adsorptive Removal of Toxic Dye Using Fe3O4−TSC Nanocomposite: Equilibrium, Kinetic, and Thermodynamic Studies Ayoub Abdullah Alqadami, Mu Naushad,* Mohammad Abulhassan Abdalla, Mohammad Rizwan Khan, and Zeid Abdullah Alothman Department of Chemistry, College of Science, Building #5, King Saud University, Riyadh 11451, Kingdom of Saudi Arabia ABSTRACT: Herein, trisodium citrate based magnetite nanocomposite (Fe3O4−TSC) was used for malachite green (MG) dye expulsion from aqueous medium. The adsorption tests were executed at different parameters. The maximum adsorption were took place at pH 4 in 40 min. The equilibrium studies were demonstrated using Langmuir and Freundlich isotherms and better agreement was attained with the Langmuir model. The maximum adsorption capacity (qe) was calculated 435 mg g−1 using Langmuir equation. The kinetic parameters displayed that MG adsorption onto Fe3O4−TSC followed pseudo-second-order kinetic model. Furthermore, the thermodynamic analysis suggested the adsorption of MG onto Fe3O4−TSC was impulsive and exothermic. The desorption studies showed the best recovery of MG dye in 0.1 M HCl. Finally, it was found that Fe3O4−TSC can be effortlessly separated from mixed solutions using external magnetic field. oil palm trunk fiber,33 pine sawdust,34 carbon developed from Arundo donax root,35 degreased coffee bean,36 bentonite,37 polyurethane foam,38 poly(acrylic acid)/SiO2 composite nano fiber membranes,39 and sodium alginate-coated Fe3O4 nanoparticles.40 Among these adsorbents, magnetic metal oxide based adsorbents have better adsorption properties owing to their high surface area and small internal diffusion resistance.41 To offer a better surface specificity for the expulsion of different types of dyes, the researchers have been concentrated on the modification of Fe3O4 nanoparticles. For this purpose, various types of chemicals viz. humic acid,42 poly(acrylic acid) ,43 yeast,44 zinc oxide,45 carboxymethyl-β-cyclodextrin,46 multiwall carbon nanotube,47 and grapheme oxide48,49 have been utilized for the modification of Fe3O4 magnetic nanoparticles surface. In the present work, we have synthesized the Fe3O4−TSC nanocomposite, which was efficiently used for MG dye expulsion from aqueous medium. The impact of influential factors, that is, pH, temperature, contact time, and dose, was studied. The desorption effectiveness was performed using different solvents.

1. INTRODUCTION Due to the rapid industrialization and other human activities, the use of dyestuff has been increased worldwide.1−3 The discharge of dye effluents from various industries like plastic, paper, cosmetic, and textile is causing serious environmental problems.4−7 More than ten thousand of diverse marketable pigments and dyes are present and more than 7 × 105 metric tons are produced yearly throughout the world.8 About 12 percent of synthetic dyes are misplaced at the time of manufacturing and handling and 20 percent of these lost dyes move in the industrial wastewaters.9 Once these dyes contaminated water mixes up with the water bodies causes water pollution. The occurrence of dye in water bodies, even at very low levels, is extremely noticeable and unwanted. Mostly, all dyes create numerous health problems like allergic dermatitis, skin problems, and cancer in human.10 Malachite green (MG) is easily solvable in water and used for dyeing wool, nylon, polyacrylonitrile, cotton, silk, leather, and paper. But, when the concentration of MG increases from the permissible level, it may cause various health problems.11 Hence, the treatment of dye-containing water is necessary before it is released to the environment. Many methods have been proposed for the expulsion of MG from the aqueous medium like advance oxidation,12 coagulation,13 membrane filtration,14 adsorption,15 photocatalysis,16 capillary electrophoresis,17 spectrophotometric method,18,19 and liquid chromatography method.20−25 Nevertheless, some of these methods have the limitations of being time-consuming, costly, complex, and less sensitive. However, adsorption is one of the best methods due to its simplicity, high effectiveness, reusability, and ease of process.26,27 Several adsorbents have been already used for the expulsion of MG dye such as Prosopis cineraria,28 iron humate,29 bagasse fly ash,30 sea shellpowder,31 cyclodextrin-based adsorbent,32 © XXXX American Chemical Society

2. EXPERIMENTAL SECTION 2.1. Materials and Methods. FeCl2·6H2O, FeCl3·6H2O, MG dye, and trisodium citrate solution were bought from SigmaAldrich, U.S.A. Fe3O4−TSC nanocomposite was synthesized by the same technique as designated in our earlier study.50 2.2. Batch Studies. The efficiency of Fe3O4−TSC for the adsorption of MG was studied by batch method. Then, 25 mL of 10 mg L−1 MG dye solutions was shaken with 100 mg Received: June 1, 2016 Accepted: October 3, 2016

A

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Figure 1. FTIR spectra of Fe3O4−TSC and MG dye adsorbed Fe3O4−TSC.

2400 cm−1 after MG dye adsorption. The intensity of two peaks (1400 and 1620 cm−1) was changed after adsorption which confirmed that carboxylate group played the main part in the MG dye adsorption onto Fe3O4−TSC nanocomposite material. The transmission electron microscope images of Fe3O4−TSC and MG dye loaded Fe3O4−TSC were recorded using JEM2100F, JEOL, Japan; which are given in Figure 2a and b. The average particle size of Fe3O4−TSC was found to be 5−10 nm and well isolated owing to the occurrence of TSC coating on Fe3O4. But, after adsorption of MG dye, the nanoparticles were agglomerated and particle size was increased because MG dye was adsorbed onto Fe3O4−TSC nanocomposite. The composition of Fe3O4 and Fe3O4−TSC were quantified by EDS.50 The detected elements were Fe and O in Fe3O4 and Fe, O, and C in Fe3O4−TSC. To find the porosity and surface properties of Fe3O4 and Fe3O4−TSC, N2 adsorption−desorption measurements were performed.50 The BET surface area and the total pore volume for Fe3O4−TSC was higher than that of parental Fe3O4 and found to be 245.42 m2 g−1 and 0.368 cm3 g−1, respectively. 3.2. Effects of Different Parameters. The effect of the initial pH was seen at the pH range from 2.5 to 10 (Figure 3a). The value of qe was increased from 12 to 24 mg g−1 with increasing the pH from 2.5 to 7. But, after pH 7, the value of qe was not changed apparently up to pH 10. The maximum adsorption was obtained at optimum pH of 7. The comparable results were stated for adsorption of MG on deoiled soya,52 treated ginger waste,53 coal,54 maize cob powder,55 and chemically modified rice husk.56 Actually, MG exists in positively charged ions form in the aqueous medium due to its cationic nature. In the acidic medium, the protonation of the functional groups of Fe3O4−TSC nanocomposite materials took place easily and thus constrained the approach of MG dye (which is positively charged) to the surface of the Fe3O4−TSC nanocomposite, resulting in low adsorption of dye at low pH. As the pH increased, Fe3O4−TSC nanocomposite surface functional groups were becoming deprotonated, which resulted in an increase in the negative charge density on the Fe3O4−TSC nanocomposite surface and help the binding of MG dye cations. There were two types of interactions (electrostatic interaction as well as hydrogen

Fe3O4−TSC nanocomposite in the Erlenmeyer flasks for 24 h to get the equilibrium. After the complete adsorption, the samples were separated using external magnetic field and examined by UV−vis spectrophotometer at 620 nm. The quantity of the MG dye adsorbed at the equilibrium was evaluated as qe =

(Co − Ce)V m

(1)

Adsorption kinetic, isotherms and thermodynamic factors were also assessed for MG dye adsorption onto Fe3O4−TSC. 2.3. Desorption Studies. The study of desorption is very significant as the regeneration of the adsorbent governs the commercial accomplishment of the adsorption procedure.51 The desorption effectiveness was performed using different solvents (0.1 M HCl, 0.1 M HNO3, 0.1 M H2SO4, and 0.1 M NaOH). In the present study, 100 mg of Fe3O4−TSC nanocomposite was kept in the Erlenmeyer flask containing 100 mL of 10 mg L−1 MG dye solution and agitated for 40 min at 120 rpm. After getting the equilibrium, the nanocomposite was separated using the external magnet, washed with Milli-Q water to eliminate the extra MG dye. Then, MG dye loaded Fe3O4−TSC nanocomposite was treated with 100 mL of aforesaid solvents at aforesaid parameters. After 40 min, the remaining concentration of MG dye in the solution phase was determined using UV−vis spectrophotometer.

3. RESULTS AND DISCUSSION 3.1. Characterization. The FTIR spectra of bare Fe3O4− TSC and MG dye loaded Fe3O4−TSC were performed using FTIR Spectrometer (Nicolet 6700, Thermo Scientific, U.S.A.) in the range of 4000−400 cm−1. It is clear from Figure 1 that the band at 550−620 cm−1 was owing to Fe−O bond. The bands at 1400 and 1620 cm−1 were corresponding to the symmetric and asymmetric vibrations of carboxylate groups from ligands on the surface of Fe3O4 due to the presence of TSC, which supported the idea that TSC has been grafted on the surface of Fe3O4. Also, the broad band between 3300 to 3500 cm−1 was attributed to the stretching vibrations of O−H bond in hydroxyl groups. The FTIR spectrum of MG dye loaded Fe3O4−TSC was also recorded and it was found that one more peak seemed at B

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Figure 2. (a) TEM of Fe3O4−TSC and (b) TEM of MG dye adsorbed Fe3O4−TSC.

bonding) between the MG dye and Fe3O4−TSC nanocomposite as can be seen in Figure 4. It was found that the value of qe was decreased from 24.5 to 21.3 mg g−1 with increasing the temperature from 25 to 65 °C, which showed the exothermic nature of MG adsorption onto Fe3O4−TSC (Figure 3b). The effect of Fe3O4−TSC nanocomposite dose for the removal of MG dye was seen in the range of 0.01 g to 1.0 g shaken with 25 mL solution of 10 mg L−1 MG dye. MG dye removal was increased from 96% to 98.5%, as Fe3O4−TSC nanocomposite dose was increased from 0.01 to 0.05 g (Figure 3c). This might be owing to the high adsorptive surface area and the accessibility of more binding sites. Further increase in Fe3O4−TSC nanocomposite dose did not show substantial increase in the removal percentage of MG dye, consequently, 50 mg/25 mL adsorbent dose was selected for the consecutive studies. While, the adsorption capacity was decreased with increasing the dosage of Fe3O4−TSC nanocomposite. The increase in the Fe3O4−TSC nanocomposite dose may cause the aggregation or overlapping of adsorbent, and consequently, the available adsorp-

tion sites may decrease, so the adsorption capacity was decreased. The similar results were observed by the other workers.57,58 The contact time effect was studied at pH 7; adsorbent dose 50 mg/25 mL and temperature 25 °C. The adsorption capacity was increased with increasing the contact time (Figure 4d). It was 19.4 mg g−1 at 5 min, suggested that Fe3O4−TSC nanocomposite had fast adsorption kinetics toward MG dye solutions. After that, the adsorption capacity was increased gradually and the equilibrium was attained in 40 min where the adsorption capacity was 24.3 mg g−1. At the starting, the adsorption rate was fast due to the adsorption of MG dye molecules onto the exterior surface of Fe3O4−TSC nanocomposite. After that, the MG dye molecules enter into the pores (interior surface), which is comparatively a low process. Initially, the fast adsorption rate may also be ascribed due to the accessibility of large number of binding sites at the surface of Fe3O4−TSC nanocomposite and the slow rates at the end might be due to the saturation of the binding sites and achievement of equilibrium.56 Desorption studies tells about the adsorption nature and the possibility to reuse the adsorbent. Herein, the desorption study was accomplished using 0.1 M HCl, C

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Figure 3. Effects of (a) initial pH, (b) temperature, (c) dose, and (d) contact time on the adsorption of MG dye onto Fe3O4−TSC nanocomposite.

The values of RL in the present study were 0.1 M H2SO4 (69.7%) > 0.1 M HNO3 (55.9%) > 0.1 M NaOH (22.3%). 3.3. Adsorption Kinetics. Pseudo-first-order59 and pseudosecond-order60 kinetic models are given as

log qe = log K f +

kt log(qe − qt) = log qe − 1 2.303

(2)

t 1 t = + 2 qt qe k 2qe

(3)

(4)

The qm and b values were assessed from the intercept and slope of linear plots of 1/qe vs 1/Ce, respectively which are shown in Table 2. The dimension less equilibrium factor was evaluated as62,63 RL =

1 1 + bCo

(6)

The Freundlich isotherm constants (Kf and n) were evaluated from the intercept and slope of the linear plots of log qe vs log Ce, respectively (Table 2). It was found that the values of Kf decreased with increasing the temperature, which revealed the exothermic nature of adsorption process. In this study, n > 1 recommended the promising adsorption of MG dye onto Fe3O4−TSC nanocomposite. The Langmuir isotherm fitted fairly well due to better correlation coefficient values (R2 > 0.99) (Figure 6 c,d). 3.5. Comparison of Monolayer Adsorption Capacity with Other Magnetite-Based Adsorbents. An assessment of maximum MG dye adsorption capacities of Fe3O4−TSC nanocomposite with that of the other previously reported adsorbents has been done and presented in Table 3. It was found that Fe3O4−TSC nanocomposite had better adsorption capacity compared to other adsorbents. So, Fe3O4−TSC nanocomposite is a prospective adsorbent for MG dye expulsion from aqueous medium. 3.6. Adsorption Thermodynamics. The enthalpy change (ΔH°), Gibbs free energy change (ΔG°), and entropy change (ΔS°) were assessed using the van’t Hoff equation which is given as

The values of various constants found from these two models are listed in Table 1. Pseudo-second-order model was better fitted due to the better value of correlation coefficient (Figure 6a,b). The values of experimental equilibrium adsorption capacity (qe,exp) was also in good covenant with the calculated equilibrium adsorption capacity values (qe,cal) which also showed the better fitting of this model. 3.4. Adsorption Isotherms. The equation of Langmuir isotherm model61 which describes the monolayer adsorption, is given as 1 1 1 = + qe Qm bQ mCe

1 ln Ce n

ln Kc = −

(5) D

ΔH ° ΔS ° + RT R

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Figure 4. Adsorption/desorption mechanism for the MG dye onto Fe3O4−TSC nanocomposite.

Table 1. Kinetic Parameters for the Adsorption of MG Dye onto Fe3O4−TSC pseudo-first-order qe,exp (mg/g)

qe,cal (mg/g)

K1 (1/min)

24.38

5.56

0.062

pseudo-second-order R2

qe,cal (mg/g)

K2 (g/mg-min)

R2

0.983

24.63

0.0337

0.999

The negative value of ΔG° showed the feasibility and spontaneity of MG dye adsorption onto the adsorbent (Table 4). The negative values of ΔS° suggested the decrease in randomness at the solid/solution interface. The adsorption of MG dye onto Fe3O4−TSC nanocomposite was exothermic and physical.

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CONCLUSION The current study was performed to see the adsorption efficacy of Fe3O4−TSC nanocomposite for MG dye removal by batch method. The optimum time and pH was found to be 40 min and 7, respectively. It was prominent that the adsorption percentage was decreased with increasing the temperature which exhibited the exothermic nature of adsorption. The isotherm studies showed that the Langmuir fitted well at all temperatures, which

Figure 5. Desorption efficiency plots of MG dye using various eluents.

The values of ΔG° were calculated as ΔG° = ΔH ° − T ΔS °

(8) E

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Figure 6. Plots of (a) Pseudo-first-order, (b) Pseudo-second-order, (c) Langmuir, and (d) Freundlich models.

Table 2. Isotherm Constants for the Adsorption of MG Dye onto Fe3O4−TSC Nanocomposite Langmuir isotherm

Freundlich isotherm 2

temperature (K)

qm,exp (mg/g)

qm,cal (mg/g)

b (L/mg)

RL

R

298 308 318 328

503.09 495.88 484.28 472.23

435 313 238 232

0.05 0.09 0.21 0.25

0.79 0.69 0.49 0.44

0.9974 0.991 0.994 0.9911

Table 3. Thermodynamic Parameters for the Adsorption of MG Dye onto Fe3O4−TSC

Kf (mg/g)(L/mg)1/n

n

R2

47.8 39.0 29.5 24.4

1.35 1.32 1.23 1.19

0.964 0.978 0.969 0.967

Table 4. List of Magnetite-Based Adsorbents Available for the Adsorption of MG Dye

−ΔG° (kJ/mol) Co (mg/L)

−ΔH° (kJ/mol)

−ΔS° (J/(mol·K))

298 K

308 K

318 K

328 K

5 100 250

26.14 19.87 7.91

61.13 44.06 14.65

7.76 6.89 3.51

7.66 6.09 3.44

6.46 5.76 3.26

6.46 5.76 3.26

adsorbents Alg@Fe3O465 Fe3O4@Mel66 magnetic litchi pericarps67 Magnetic MWCNTs68 Fe3O4/reduced graphene oxide (MRGO)69 Fe3O4@ chitosan70 Fe3O4@TSC (present study)

indicated a homogeneous surface binding of MG dye onto Fe3O4−TSC nanocomposite. In addition, the adsorption followed the pseudo-second-order kinetic model. The changes in the FTIR peaks noticeably exhibited the adsorption of MG dye onto the Fe3O4−TSC nanocomposite. The desorption studies showed the best recovery of MG dye in 0.1 M HCl.

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AUTHOR INFORMATION

Corresponding Author

*E-mail: [email protected]. F

experimental condition

adsorption capacity

equilibration time (min)

initial concentration (mg L−1)

temperature/ pH

qm (mg g−1)

20 240 60

10 3 150

298/7 298/6.5 298/6

47.84 9.06 70.42

60

20

298/6

77.5

30

5

298/7

22

30

50

298/2

183.2

40

10

298/7

435

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Notes

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The authors declare no competing financial interest. Funding

The authors would like to extend their sincere appreciation to the Deanship of Scientific Research at King Saud University for funding this work through the Research Group No. RG-1437-004.

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DOI: 10.1021/acs.jced.6b00446 J. Chem. Eng. Data XXXX, XXX, XXX−XXX