Desalination and Water Treatment 317 (2024) 100037

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Desalination and Water Treatment

journal homepage: www.sciencedirect.com/journal/desalination-and-water-treatment/

Environmental engineering approach using Fe-Co-S nanomaterials for

removal of Rhodamine B in wastewater: Preparation, performance, and ]]
]]]]]]
]]

mechanism
Bai Suna,b, Chenxu Shaoa, Yunming Chenga, Fengshou Zhaoa, Menghao Suna, Mingjian Yia,
Yuxian Guoc, Yun Wanga, Xiangxiang Wanga, , Shuguang Zhua, Xinli Caia
⁎

a
Anhui Institute of Urban and Rural Green Development and Urban Renewal, College of Environment and Energy Engineering, Anhui Jianzhu University, Hefei 230601,
China
b
Environmental Materials and Pollution Control Laboratory, Hefei Institute of Physical Science, Chinese Academy of Sciences, Hefei 230031, China
c
College of Mathematics and Physics, Anhui Jianzhu University, Hefei 230601, China

A R T I C L E I N F O A B S T R A C T

Keywords: Fe-Co-S (FeCoS) nanomaterials with good recycling abilities were prepared by a hydrothermal method, and their
FeCoS adsorption properties twords Rhodamine B (RhB) were investigated. Scanning Electron Microscopy (SEM),
Rhodamine B Energy Dispersive Spectrometer (EDS), X-ray Diffraction (XRD), N2 adsorption-desorption isotherms, Brunel
Adsorption Emmett Taylor (BET) surface area, and Fourier Transform Infrared Spectroscopy (FTIR) were used to char-
Dyeing wastewater
acterize the materials and analyze their physicochemical properties. The effects of temperature, pH, and ad-
sorbent dosage on the adsorption performance of FeCoS were also investigated. The results showed that the
equilibrium time for the adsorption of rhodamine B by FeCoS was 150 min. The adsorption process followed the
Langmuir isotherm with a pseudo-second-order kinetic model. It suggests that the adsorption is mainly con-
trolled by chemisorption and belongs to homogeneous monolayer adsorption. The thermodynamic fitting of the
adsorption process showed that the adsorption of RhB by FeCoS is spontaneous and accompanied by an en-
dothermic reaction, and the maximum adsorption capacity reached 578.03 mg/g at 318 K with a removal rate of
98.3%. The removal rate of FeCoS was maintained at 89.95% after five cycles, which was of great potential for
practical application in the treatment of dyestuff wastewater.

1. Introduction responsible for the environmental pollution of dye wastewater: textile

(54%), dyeing industry (21%), paper and pulp (10%), tanning and paint
In recent years, the rapid development of global urbanization and (8%), and dye manufacturing (7%) [6]. Dyes belong to the class of
industrialization has caused tremendous pressure on the natural en- aromatic compounds with complex structures that are difficult to re-
vironment, especially the problems related to organic pollutants in move and degrade due to the toxicity, diffusivity, and stability of or-
water, which have attracted great attention from various countries and ganic dyes. It poses a serious threat to humans and the environment
have been listed as international priority issues [1]. At present, the [7,8]. Rhodamine B (RhB) is a jaundice dye that is harmful to humans
discharged industrial wastewater includes heavy metals, dyes, fuel oil, and animals for reasons such as skin, eye, and respiratory irritation,
and other pollutants [2]. carcinogenicity, and reproductive and developmental toxicity [6]. In
Dyes are organic compounds that can add different colors to other addition, RhB present in the environment and food matrices can cause
substances. As important chemicals, they have been widely used in the serious carcinogenic, genotoxic, and neurotoxic effects on public health
leather, varnish, textile, pesticide, paper, rubber, and food industries [9].
[3], and are also found in the wastewater discharged from these fac- The commonly used treatment methods for dye wastewater mainly
tories. It has been found that residual dyes are discharged with was- include flocculation, physical adsorption, membrane filtration, biode-
tewater [4,5]. The study shows that the following industries are mainly gradation, photocatalysis, etc. [10–13]. Among these removal

⁎
Corresponding author.
E-mail address: [email protected] (X. Wang).

https://doi.org/10.1016/j.dwt.2024.100037
Received 5 January 2024; Received in revised form 5 January 2024; Accepted 13 January 2024
1944-3986/© 2024 The Author(s). Published by Elsevier Inc. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

processes, the adsorption method is widely used in wastewater treat- FA2204N electronic balance, Shanghai Jinghai instrument Co., Ltd.,
ment research due to the advantages of simple operation, strong ad- (China). UV-2600i UV-Vis spectrophotometer (Shimadzu
sorption capacity, fast adsorption speed, and the reusable performance Manufacturing Co., Ltd., China). The XRD patterns of the adsorbents
of the adsorbent [14,15]. In addition, one of the key advantage of the were performed on a D/MaXIIIA X-ray diffractometer (Rigaku Co.,
adsorption method is that it is applicable to a wide range of materials Japan). AURIGA scanning electron microscope, ZEISS Co., (Germany).
and does not produce any intermediate products or split molecules, AURIGA energy spectrometer, ZEISS Co., (Germany). BET surface area,
which ensures the purification of water quality and does not produce Micromeritics Co., (USA). The FTIR spectra of the adsorbents before
secondary pollution [16–18]. In previous studies, zeolite, clay and ac- and after adsorption were recorded with a Nexus-870 FTIR spectro-
tivated carbon are commonly used adsorption materials. Even some meter (Thermo-Fisher Scientific in the USA). The specific surface area
wastes can be potential adsorbents [19,20], such as activated rice husk and void capacity of the adsorbents were measured using Brunel
ash [21], activated carbon obtained from okra wastes [22], biochar Emmett Taylor surface area (BET, Micromeritics, USA).
from lychee seed [23], spent coffee grounds based biochar and hydro-
char [24]. However, all of them exhibit drawbacks such as limited 2.2. Preparation of adsorbent
adsorption capacity, slow adsorption kinetics and poor surface func-
tionality [7,25]. So the development of efficient and economical ad- 0.2 g FeCl2•4 H2O and 0.24 g CoCl2•4 H2O were added in 60 mL
sorbents has become one of the research hotspots for dye removal ultrapure water and stirred on a magnetic stirrer for 30 min to fully
methods at present [3]. dissolve in water. 0.6 g urea and 0.3 g NH4Cl were added and stirred for
In recent years, many achievements have been reported about the 1 h to make it fully dissolved. Then 1.2 g of Na2S was added, con-
adsorption methods for the dye in water. Mina Azadfar et al. prepared tinuously stirring for 1 h to make it fully dissolved. After stirring, the
graphene oxide/chitosan nanocomposite which could adsorb methyl solution was transferred into the reaction kettle, and put in a blast
orange in water with good adsorption capacity of 107 mg/g [26]. Muna drying oven at 180 °C, place it for 12 h, and then cooled to room
Abd Ul Rasool Al-Kazragi et al. successfully prepared natural smectite temperature. Ultrapure water and absolute ethanol were washed sev-
(SMC) and SMC-nanoTiO2 which could adsorb Rhodamine B in water eral times, respectively, washed and filtered, and then placed in a blast
[27]. It has been reported that Iron-based materials have a good ad- drying oven for 12 h at 80 °C, and FeCoS nanomaterial particles were
sorption effect on dyes, among which Fe MOF can effectively remove obtained after drying [39].
RhB, CR, and Orange II multiple dyes [28–30]. Meanwhile, Co-based
materials have many applications for the removal of dyes [31,32].
2.3. Characterizations of samples
Wenbo Liu et al. prepared two Co(II)-based metal organic frameworks
that can have high-efficiency adsorption of dyes [33]. Afterwards, some
The surface morphology and structure of FeCoS nanocomposite
scholars found that modified FeCo MOF can have a better treatment
were characterized by field emission scanning electron microscopy
effect on dye wastewater [34]. Some scholars have prepared FeCo-
(SEM, AURIGA, ZEISS Company, Germany) coupled with an energy
based composites with strong adsorption capacity for RhB [35,36]. The
dispersive spectrometer (EDS, INCA X-Max 50, ZEISS Company,
unique physical and chemical properties of metal chalcogenides have
Germany). The X-ray diffractometer (XRD, PANalytical, Netherlands)
attracted the attention of many scholars [37,38]. Aniruddha Molla et al.
with a Cu Kα source was used to analyze the crystalline structure.
used the decoration of Graphene Oxide with Iron Cobalt Sulfide to re-
Fourier transform infrared spectroscopy (FTIR, Nexus-870, Thermo
move dye [39].
Nicolet, USA) was used to determine the change in surface properties.
In this paper, Rhodamine B solution was selected to simulate the dye
The wavelength change of the adsorbent was recorded by a UV-2600i
wastewater, and a nanomaterial of iron cobalt-based compound with
UV-Vis spectrophotometer (UV-2600i, UV-Vis, Shimadzu, China).
high adsorption performance was prepared and modified by further
sulfur doping. The effects of solution pH and the number of times of
regeneration of the adsorbent on the adsorption performance were in- 2.4. Experimental method
vestigated to explore the optimal conditions. The FeCoS nanomaterials
have good adsorption and recovery ability with great adsorption ca- 2.4.1. Preparation of RhB standard solution
pacity, which would inspire other emerging bimetallic sulphide com- 25 mg of RhB was dissolved in 100 mL of deionized water, sonicated
posites for related applications. for 15 min, and transferred to a 250 mL volumetric flask to complete a
constant volume, that is, 100 mg/L of RhB standard solution. The RhB
2. Experimental section solution in all adsorption experiments was obtained by diluting the
standard solution with deionized water. Prepared RhB solution with a
2.1. Reagents and instruments concentration gradient of 5, 10, 20, 30, 40, 50, and 60 mg/L, and
measured its absorbance at 554 nm wavelength by ultraviolet spec-
The main reagents used in the experiment were ferrous chloride trophotometer. Then the RhB standard curve was obtained by linear
hexatetrahydrate (FeCl2•4 H2O), cobalt chloride tetrahydrate regression analysis of the concentration and absorbance of RhB.
(CoCl2•4 H2O), urea (CO(NH2)2), ammonium chloride (NH4Cl) and
sodium sulfide (Na2S), purchased from Sinopharm Chemical Reagent 2.4.2. Calculation of adsorption capacity and removal rate
Co.,Ltd. (Shanghai, China),and used directly without further purifica- Untreated dye wastewater was simulated by employing different
tion. Anhydrous ethanol (99.7%), analytical purity, Xilong Scientific concentrations of RhB solution. The 20 mg FeCoS nanocomposite was
Co., Ltd., (China). Deionized water was prepared by FST-TOP-A24 added to 100 mL of 10 mg/L RhB solution for batch adsorption ex-
super pure water equipment by Shanghai Fushite Instrument periments. The whole experiment was carried out in a constant tem-
Equipment Co.,Ltd., (China). perature oscillation chamber with shading, with the room temperature
The instruments used in the experiment mainly included the TG16K- set at 298 k and the rotation speed at 160 rpm. After waiting for the
II table high-speed centrifuge from Shanghai Zhaodi Biotechnology Co., adsorption equilibrium, the absorption value at the 554 nm absorption
Ltd., (China). RCT basic magnetic stirrer, EKA Instrument Equipment wavelength was measured by UV-Vis. The effect of adsorbent dose and
Co., Ltd., (China). DHG-9023A air drying box, Shanghai Yiheng initial pH on the experiment was studied by the same experimental
Scientific Instrument Co., Ltd., (China). PHB-3 digital pH meter, method, and its isothermal line and kinetics were analyzed. The dye
Shanghai San-Xin Instrument Factory, (China). PTFE reaction kettle, removal rate (%) and the amount of dye adsorption were calculated by
Shanghai Jinghong Experimental Equipment Co., Ltd., (China). Eqs. (1) and (2), respectively.

2
B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

Fig. 1. (a) the SEM images before FeCoS adsorption, (b) the SEM images after FeCoS adsorbs RhB solution.

(C0 Ce) 3 min, 5 min, 7 min, 10 min, 20 min, 30 min, 40 min, 50 min, 60 min,
= × 100%
C0 (1) 90 min, 120 min, 150 min, 210 min, 270 min, 300 min, 720 min re-
spectively. Then conduct high-speed centrifugation, take an appropriate
(C 0 Ce ) × V amount of supernatant, and pass through a 0.22 µm inorganic filter
qe =
m (2)
membrane. The absorbance value was measured by UV-Vis.
where C0 (mg/L) and Ce (mg/L) were the initial concentration before
adding the adsorbent and the equilibrium concentration after adding 2.4.8. Study on the regeneration capacity of adsorbent
the adsorbent, respectively; qe (mg/g) was the adsorption capacity at In order to evaluate the regeneration ability of the adsorbent, pour a
the adsorption equilibrium; V (L) was the volume of RhB solution; m (g) certain amount of saturated adsorbent into a 0.05 mol/L NaOH solution
was the dosage of adsorbent; η is the removal rate of the adsorbent. for desorption and reuse [40]. Repeat the five-cycle regeneration ex-
periments to explore the regeneration performance of FeCoS.
2.4.3. Effect of pH
0.1 mol/L HCl and 1 mol/L NaOH solution were used to adjust the
3. Results and analysis
pH value of 100 mL RhB solution with a concentration of 10 mg/L. The
pH value range of the solution was set to 3–12. Then, 20 mg of ad-
3.1. Characterizations of FeCoS nanomaterials
sorbent was added, respectively, and the effect of pH on the adsorption
performance was investigated by shading and shaking for 12 h.
Scanning electron microscopy (SEM) was used to observe the mor-
phology of FeCoS nanomaterials before and after adsorption, as pre-
2.4.4. Effect of adsorbent dosage
sented in Fig. 1. From Fig. 1(a), it can be observed that the samples are
5, 10, 15, 20, 25, 30 and 35 mg of adsorbents were added to 100 mL
irregular particles before adsorption, which are close to each other, and
of RhB solution with a concentration of 10 mg/L, respectively. Then,
the average particle size is about 50–90 nm. In Fig. 1(a), the coral-like
shake them for 12 h under shading. Taking samples for measurement to
structure composed of particles is loose and porous, which promotes
explore the effect of the amount of adsorbent on the adsorption per-
adsorption to a certain extent. Fig. 1(b) shows the appearance of the
formance.
material after adsorption. It can be seen from the figure that a gelati-
nous substance appears on the surface of the material, indicating that
2.4.5. Study on adsorption isotherms the RhB solution is well attached to the surface of the material, in-
In the study of the adsorption isotherm of FeCoS on RhB, take dicating that the material has a significant adsorption effect on the RhB
100 mL of RhB solution with concentrations of 5, 10, 15, 20, 25, 30, 35, solution. A similar phenomenon was reported by Jia et al. who reported
40, 45, and 50 mg/L add 20 mg of FeCoS to it, respectively, and then that the residue of RhB on the surface has a significant effect on the
put 250 mL conical flask filled with RhB solution and adsorbent into a morphology [41].
constant temperature shaker for shading and shaking for 12 h (298 K, In order to investigate the composition and content of FeCoS, the
160 rpm/min). After the end of oscillation, conduct high-speed cen- adsorbent was characterized by EDS. Table 1 lists the contents of var-
trifugation, take an appropriate amount of supernatant, and pass ious elements used as adsorbent, of which the sulfate element content
through a 0.22 µm inorganic filter membrane. The absorbance value accounts for the largest proportion. In addition, it can be seen from the
was measured by UV-Vis. table that the composite contains sulfate, cobalt and iron. The EDS
spectrum of FeCoS nanocomposites is shown in Fig. 2. The result shows
2.4.6. Study on adsorption thermodynamics that the composite contains Fe, Co, and S.
In the study of adsorption thermodynamics, at 298 K, 308 K, and In order to study the crystal structure and phase purity of the ad-
318 K, the vibration frequency of 160 rpm/min was oscillated in a sorbent, XRD analysis of the adsorbent was carried out, as shown in
constant temperature shaker for 12 h. After the oscillation, centrifuge Fig. 3. It can be seen from the figure that the diffraction peak of the
and filter, measure the absorbance value of RhB solution at the ab- adsorbent is roughly consistent with the standard card of Co9S8 (JCPDS
sorption wavelength of 554 nm, and finally analyze the data to obtain
the entropy change, enthalpy change, and Gibbs free energy change of Table 1
the adsorption experiment. Elemental content of FeCoS nanomaterials.

Elements Weight % Atomic %

2.4.7. Study on adsorption kinetics
In the adsorption kinetic study, 20 mg of adsorbent was added to SK 3.77 68.13
100 mL of RhB solution at a concentration of 10 mg/L, pH 7, and then Fe K 2.45 17.76
Co K 1.96 14.11
immediately placed in a thermostatic oscillator to avoid light (25 ℃,
Totals 8.18 100
160 r/min), and the samples were taken at times of 0 min, 1 min, 2 min,

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B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

another one, which assumes that heat of adsorption of all molecules in

the layer would decrease linearly rather than logarithmic with coverage
and uniform distribution of binding energy between adsorbent and
adsorbate [45]. The equation expressions [46–48] are given below:
Ce C 1
= e +
qe qm KL × qm (3)

1
ln qe = ln Ce + ln KF
n (4)

RT
qe = ln(KT Ce)
b (5)

Fig. 2. EDS spectrum of FeCoS adsorbent. where Ce (mg/L) is the RhB concentration after equilibrium adsorption;
qe (mg/g) is the amount of RhB in the adsorbent after equilibrium; qm
(mg/g) is the maximum adsorption capacity calculated according to the
Langmuir equation; KL is the Langmuir adsorption constant; and KF and
n are Freundlich adsorption constants; KT (L/g) is the Temkin isotherm
constant; b (J/mol) is binding energy constant; T is the temperature,
and R (8.314 J/kmol) is the universal gas constant.
Langmuir, Freundlich and Temkin models were used for studying
adsorption behaviours, as shown in Fig. 5. The parameters of the cor-
responding isotherm models are listed in Table 2. The parameters in
Table 2 show that the R2 of the Langmuir isotherm model is 0.991,
which is larger than that of the Freundlich and Temkin isotherm
models, indicating that the Langmuir model better describes the ad-
sorption process of FeCoS on Rh B than the Freundlich and Temkin
models. The Langmuir model indicates that the adsorbent surface is
monolayer and homogeneous, while the Freundlich model infers that
the adsorbent surface is inhomogeneous, and the Temkin model as-
sumes that the adsorption heat distribution of all molecules is homo-
geneous and linear [48–50]. In our study, it indicates that FeCoS has a
uniform adsorption capacity and the adsorption occurs on the surface as
a monolayer, and the Langmuir model fitting yielded a saturated ad-
sorption capacity of 454.55 mg/g for the FeCoS adsorbent. In addition,
Fig. 3. XRD patterns of FeCoS adsorbent.
it can be observed from Table 2 that the value of n is in the interval of 1
and 10, which proves that the adsorption of FeCoS on RhB is chemi-
No.19–0346). The characteristic diffraction peaks are sharp, indicating sorption [51]. This result also further indicates that the adsorption of
that the material has a good crystal structure. In the figure, the dif- FeCoS on RhB is monolayer adsorption on a uniform surface.
fraction peaks at 2θ= 25.5°, 29.8°, 36.1°, 40.6°, 47.3°, 51.9°, 55.6°,
61.3°, and 73.3° correspond to (220), (311), (400), (420), (511), (440), 3.3. Adsorption thermodynamics
(600), (533), (731) planes. There are some diffraction peaks
(2θ=32.5°) in the figure, which may be the diffraction peaks presented Adsorption thermodynamics can reveal the changing pattern of the
by Fe element in the composite. The results of the XRD pattern are adsorption process with temperature [52]. The following Eqs. (5) and
consistent with the results in Table 1 for the higher elemental content of (6) were used to calculate the enthalpy change ΔH, entropy change ΔS
S and Co, and the lower elemental content of EDS for Fe. Combined and Gibbs free energy change ΔG. The expressions of the equations [46]
with the XRD analysis it is clear that no fixed crystalline form was are given below:
produced for the Fe element. The sample contains less iron, indicating G= RT ln K (6)
that the compounds of iron and cobalt do not form a fixed crystalline
form. ln K =
H
+
S
To explore the microstructure of FeCoS, N2 adsorption-desorption RT R (7)
isotherms were used to analyze the material. Fig. 4(a) The isotherm line where R is the general gas constant (8.314 J/(mol/K)), T is the tem-
is a typical IV curve with a hysteresis loop. The formation of the hys- perature (K); K is the Langmuir adsorption constant, ∆S is the entropy
teresis loop is a result of the process of capillary condensation. The change, ∆G is the Gibbs free energy change, and ∆H is the enthalpy
specific surface area of FeCoS is 36.1427 m2/g and the pore volume is change.
0.1139 cm3/g. Thermodynamic analysis of adsorption is an essential experiment to
properly understand and predict the adsorption mechanism. According
3.2. Adsorption isotherm to Fig. 6, it shows that the adsorption capacity of the FeCoS adsorbent
increases when the equilibrium concentration increases at the same
Adsorption isotherms indicate how a substance from the aqueous temperature. According to Table 3, at the same equilibrium con-
media transfers to a solid-phase when an equilibrium adsorption state is centratioIn, the increase in temperature will promote the adsorption
established [42]. In addition, the adsorption isotherm can reflect the process to a certain extent, indicating that the adsorption performance
relationship between the equilibrium concentration of the adsorbent of FeCoS improves with the increase in temperature, and the saturated
and the amount adsorbed [43]. Freundlich and Langmuir's model was adsorption capacity of FeCoS at 45 °C is 578.03 mg/g. Based on the data
used to examine the exact mechanism of the adsorption process and to in Table 3 combined with Eqs. (6) and (7), the energy change can be
calculate the adsorption capacity [44]. Also, Temkin isotherm model is calculated as in Table 4. The value of ΔG decreased from − 10.72 to

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B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

Fig. 4. (a) N2 adsorption-desorption isotherm of FeCoS; (b) pore size distribution curve of FeCoS.

Fig. 5. (a) The fitting diagram of Langmuir,Freundlich and Temkin model of FeCoS nanomaterials adsorbing RhB solution; (b), (c) and (d) are the linear fitting
diagrams of Langmuir, Freundlich and Temkin models of FeCoS nanomaterials, respectively.

− 13.35 kJ/mol when the temperature was increased from 298 K to reaction is more spontaneous and feasible. The negative value of ΔG
318 K. This negative trend confirms that the adsorption reaction is more indicates that the adsorption process is spontaneous [53,54]. In addi-
favorable at relatively high temperatures and that the adsorption tion, the value of ΔH was 30.14 kJ/mol, indicating that some chemistry

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B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

Table 2
Parameters of the isotherm model for the adsorption of RhB on FeCoS nanomaterials.

Samples Langmuir Freundlich Temkin

2 2
Parameters KL qm R n KF R KT b R2
298 K 0.1631 454.55 0.991 1.6492 66.1146 0.973 2.457 28.372 0.951

Fig. 6. (a) and (b) are the linear fitting diagrams of Langmuir model and Freundlich model for the adsorption of RhB by FeCoS nanomaterials at different tem-
peratures.

Table 3
Different adsorption isotherm model parameters for RhB adsorption at different temperatures.

Isotherm model Langmuir Freundlich

Parameters KL qm R2 n KF R2
298 K 0.1631 454.55 0.991 1.6492 66.1146 0.973
308k 0.2123 492.61 0.973 1.6216 83.0829 0.951
318k 0.3704 578.03 0.993 2.1958 139.8947 0.968

Table 4
Model parameters for adsorption of RhB at different temperatures.

Parameters T (K) Kd ∆G (kJ/mol) ∆S (kJ/ (mol·k)) ∆H (kJ/mol)

FeCoS 298 75.70 -10.72 36.07 30.14

308 112.36 -12.09
318 156.25 -13.35

Table 5 interface and irreversibility of the reaction, which favours the stability
Comparison of adsorption capacity of different adsorbents. of adsorption [56]. In conclusion, higher temperatures favour adsorp-
tion. In addition, in order to compare the adsorption capacity of dif-
Adsorbents Pollutants Efficiency (mg/g) Reference
ferent adsorbents on RhB, the comparison on adsorption capacity with
TMPTA-G-M RhB 45.64 [57] some other adsorbents is listed in Table 5. The results show that the
Fe3O4 @C Congo red 262.72 [58] maximum adsorption capacity of FeCoS is higher than that of many
Fe-BC RhB 12.41 [39]
other adsorbents at the same temperature.
AMBC RhB 53.66 [49]
C/MnCuAl-LDOs Congo red 317.2 [59]
Moroccan natural RhB 29.33 [60]
clay 3.4. Adsorption kinetics
MIL-125(Ti) RhB 180 [61]
Fe-MOFs RhB 135 [62]
FeCoS RhB 581.4 This work
In order to further understand the relationship between the struc-
ture of the adsorbent and the adsorption form, the adsorption rate and
adsorption efficiency of the adsorbent to the adsorbate molecules were
investigated by using two pseudo-first-order and pseudo-second-order
was involved throughout the adsorption process. ΔH > 0 indicates the kinetic models [63]. The linear forms of the two models are:
typical endothermic property of the adsorption process. Similar has
been reported in the literature [55]. At the same time ΔS > 0, which k1 t
log(qe qt ) = log qe
indicates increased chaos and randomness at the adsorbent-adsorbate 2.303 (8)

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B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

Fig. 7. (a) The adsorption equilibrium diagram of FeCoS nanomaterials; (b) and (c) are the linear fitting diagrams of the pseudo-first-order kinetics and pseudo-
second-order kinetics of FeCoS nanomaterials; (d) diffusion model of RhB adsorbed by FeCoS.

Table 6
Pseudo-first- and second-order kinetic parameters of FeCoS adsorption of RhB.

Pseudo-first-order kinetics Pseudo-second-order kinetics

−1
k1/min qe/mg·g−1 R2 k2/g·(mg·min)−1 qe/mg·g−1 R2
0.0119 3.9509 0.988 0.0016 43.1779 0.993

t
=
1
+
t surface of the FeCoS material were gradually saturated; ultimately, the
qt k2 qe 2 qe (9) adsorption amount reached saturation. The data of the adsorption
process were processed by Eqs. (8) and (9), and linear fitting was per-
where qe (mg/g) is the amount of RhB adsorbed at the moment of formed to obtain the proposed first-order and proposed second-order
equilibrium; qt (mg/g) is the amount of RhB adsorbed at the moment t, models as shown in Figs. 7b and 7(c), respectively, and the kinetic
and t (min) is the adsorption time; and k1 (1/min) and k2 (g/(mg·min)) parameters are shown in Table 6. According to Table 5, compared with
are the rate constants for the proposed primary and proposed secondary the correlation coefficient fitted by the pseudo-first-order kinetic model
kinetics, respectively. (R2 = 0.988), the correlation coefficient fitted by the pseudo-second-
Fig. 7a-c shows the kinetic model of the adsorption process of RhB order kinetic model (R2 = 0.993) is high relatively. It indicates that the
by the fitted FeCoS for a certain period of time. From the trend in pseudo-second-order kinetic model can more accurately describe the
Fig. 7(a), it can be seen that the removal of RhB by FeCoS material adsorption process of FeCoS on RhB, indicating that the process is
tends to increase and then equilibrate, and the reaction reaches equi- mainly controlled by chemisorption.
librium at 150 min. At the beginning of the adsorption process, a large In order to get more detailed information about the adsorption
number of active adsorption sites existed on the surface of the FeCoS mechanism of FeCoS on RhB and the changes in adsorption rate, the
adsorbent, which provided a good contact condition for the RhB mo- adsorption process was analysed using an intra-particle diffusion
lecules; however, as the reaction proceeded, the adsorption sites on the model. The fitted diffusion model is shown in Fig. 7(d), during the

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B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

Fig. 8. Effect of pH on FeCoS adsorption of Rh B.

Fig. 10. Effect of dosage on FeCoS adsorption of Rh B.

solution [69]. The effect of pH on RhB adsorption by FeCoS composites

was investigated in the range of 3–12 (Fig. 8). As shown in the figure,
the removal of RhB by the adsorbent remained good and stable in both
acidic and weakly alkaline environments. The removal of RhB by the
adsorbent remained above 90% at all pHs from 3–9 and was best at
pH= 7 with 98.3% removal. At solution pH= 10–12, the adsorption
rate of Rhodamine B by the adsorbent exhibited a decreasing trend with
the rise in solution pH, showing a decreasing trend, and was lowest at
pH= 12, with a removal rate of only 37.8%.
In order to understand the mechanism, zeta potentials of the ad-
sorbents were measured, as shown in the Fig. 9. The pH value where
the zeta potential was zero was taken as the isoelectric point (IEP). It
can be seen from Fig. 9 that when the pH increased from 3 to 12, the
Zeta potential gradually decreased from 24.21 mV to − 19.1 mV, and
the point of zero charge (PZC) of FeCoS is 8.35. When 3 ≤ pH ≤ 8, the
surface charge of FeCoS is negative, so there is a strong electrostatic
attraction between FeCoS and RhB. Under a high pH, the electrostatic
attraction between FeCoS and RhB is obvious, which is more favour-
able to the adsorption of RhB. When pH = 7, the removal rate of RhB
by FeCoS was the highest. When 9 ≤ pH ≤ 12, the adsorption effect of
Fig. 9. Zeta potential of FeCoS adsorbent. FeCoS on RhB decreased significantly with the increase of pH. This
may be due to the fact that when pH is high, RhB exists mainly as
amphoteric ions [70] and can further form dimers and aggregate with
adsorption process, the RhB solution colour changed significantly, and decreasing positive charge. Therefore, it is considered that these forms
the adsorption process showed a rapid adsorption phase, a media- may not be able to enter the microporous structure of FeCoS compo-
continuous adsorption phase and an equilibrium adsorption phase [64]. sites [71]. Furthermore, at pH > 9, due to the increase in the number
In the first phase, adsorption proceeds rapidly and the RhB diffuses of Na+ ions in solution, the Na+ ions can compete with the basic form
around FeCoS and then overcomes the resistance of the liquid to diffuse of cationic RhB for equivalent active adsorption sites in FeCoS [72].
to the surface of FeCoS (membrane diffusion) [65]. In the second phase, The zero point potentia (pHpzc) is 8.35 when pH < pHpzc. In addition,
the rate of adsorption slows down and the RhB diffuses from the outer the positive charge increases when pH > pHpzc. The zeta potential
surface to the inner surface (particle diffusion) [66]. The third phase is results are consistent with the results of the removal rate as a function
the equilibrium phase where the RhB is adsorbed to the inner surface of of pH.
FeCoS [67]. In contrast, the adsorption rate was fast during 120 min,
and the adsorption process was mainly controlled by phases I and II, as
the fitted curves for both phases did not pass through the origin [68]. 3.5.2. Influence of dosage on adsorption
Therefore, it can be concluded that the adsorption of RhB by FeCoS is When the adsorbent dosage is in the range of 5–20 mg, the removal
mainly controlled by physisorption and chemical interactions. rate of RhB increases significantly, as shown in Fig. 10. This is because
there are a large number of adsorption sites on the surface of the ad-
3.5. Single factor influence experiment sorbent. When the adsorbent is at 20 mg, the removal rate can reach
98.3%. When the amount of adsorbent continued to increase, the re-
3.5.1. The effect of pH on adsorption moval rate increased, but the growth rate decreased significantly, in-
The pH value is an important parameter affecting the adsorption of dicating that the adsorption of RhB in the solution was basically com-
dyes on adsorbents, because the structure of dyes and the chemical plete. Considering the removal rate and cost-effectiveness, here the
properties of adsorbents are highly dependent on the pH value of the optimal dosage of the adsorbent is 20 mg.

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B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

Fig. 11. FTIR spectra of FeCoS adsorbent. Fig. 13. Cyclic adsorption effect of FeCoS adsorption of Rh B.

Fig. 12. Reaction mechanism diagram.

3.6. Adsorption mechanism strong electrostatic attraction between FeCoS and RhB. When the pH is
high, RhB exists mainly as an amphoteric ion and may further form
Infrared spectroscopy is widely used to study the structural char- dimers, which affects the adsorption of RhB. FeCoS adsorbs rhodamine
acteristics of materials, and the functional groups on the surface of B mainly by both hydrogen bonding and pore filling. We speculate that
adsorbents can be qualitatively analyzed according to the infrared FeCoS adsorbs rhodamine B via hydrogen bonding, which is in agree-
spectroscopy [73]. FeCoS has a significant variation of characteristic ment with the study by Pengwei Li et al. [78]. The reaction mechanism
peaks in the 500–1200 cm−1 range. It can be seen from Fig. 11 that diagram is shown in Fig. 12.
there is no shift of the characteristic peaks before and after adsorption
by the adsorbent, but the wavelengths of the characteristic peaks have 3.7. Cyclic adsorption experiment
changed. The changes in wavelength around 1125 cm−1 and
1105 cm−1 are ascribed to the stretching of the aromatic structure [74] The reusability of the adsorbent is an essential factor for practical
and the absorption of carbonyl C]O [69]. The peak at 990 cm−1 nearly application [79]. Upon reaching adsorption equilibrium, the solution
disappeares after adsorption due to the reduction of C-O bonds [75]. was initially desorbed using 0.05 mol/L NaOH. The adsorbent was then
The shift in the peak at 760 cm−1 may be attributed to the presence of collected via centrifugation, washed with deionized water, and the
C-C bonds in the benzene ring after adsorption [76]. The peak at adsorption experiment was repeated for five cycles. As shown in Fig. 13,
617 cm−1 has decreased in intensity, presumably because of the the FeCoS nanocomposites adsorbent removed up to 98.3% of RhB.
stretching vibration of mid-C-H during the adsorption [77]. Even after five cycles, the removal rate remained at 89.95%, indicating
The adsorption isotherm, kinetic and thermodynamic results show an excellent recycling ability.
that the adsorption of RhB by FeCoS is spontaneous, endothermic and
homogeneous. In addition, FeCoS has a high specific surface area as 4. Conclusion
measured by the N2 adsorption-desorption isotherm, which provides
more adsorption sites for RhB adsorption. The zeta potential results In summary, a FeCoS nanomaterial which has good adsorption
indicate that the better adsorption effect at lower pH is due to the properties for RhB is synthesized by a simple hydrothermal method.

9
B. Sun, C. Shao, Y. Cheng et al. Desalination and Water Treatment 317 (2024) 100037

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