a r t i c l e i n f o a b s t r a c t
Article history: In this article, graphene oxide (GO) was synthesized by the Hummers and the modified
Received 24 May 2018 Hummers methods and functionalized with chitosan and used as adsorbents for salty water
Received in revised form 24 July 2018 desalination application. The results demonstrated that GO prepared via the modified Hum-
Accepted 11 August 2018 mers method has higher adsorption capacity of sodium ions than GO prepared via the
Available online 20 August 2018 Hummers method. Also, functionalization with chitosan improved sodium ions adsorption
capacity of the GO prepared via the modified Hummers method from 770.2 to 830.3 mg/g at
Keywords: an initial sodium ion concentration of 40,000 mg/l. Langmuir and Freundlich isotherms and
Adsorption two kinetic models were applied to fit the experimental data. Regeneration performance of
Desalination the prepared adsorbents was also studied. The results demonstrated that both isotherms
Carbon nanomaterials and the pseudo-second-order kinetic model match the obtained experimental data very
Graphene oxide (GO) well. It was found out that the chitosan functionalized GO with higher adsorption capacity
Functionalization and better regeneration performance can be considered as an effective adsorbent for salty
water desalination.
© 2018 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
1. Introduction acteristics of the used adsorbent like specific surface area and surface
functional groups (active adsorption sites). In recent years, tremendous
Desalination is a process that extracts dissolved mineral components effort has been undertaken to develop new adsorbents for wastewa-
from salty water such as sea water, brackish water and treated water. ter treatment. Carbon nanomaterials such as carbon nanotubes (CNTs)
The seas, the oceans, and the ices in the poles cover about 71% of and graphene and its derivatives such as graphene oxide (GO) have
the earth’s surface and contain 99% of the earth’s water. Less than attracted considerable attention as good candidates for adsorbent
1% of the earth’s water is fresh and suitable for drinking. The water materials due to their unique physical and chemical properties (Kyzas
of the seas and the oceans is salty and not directly useable. There- et al., 2014; Zhao et al., 2011; Banerjee et al., 2017).
fore, in order to overcome the water shortage, special processes are Graphene is a two-dimensional carbon based nanomaterial that
needed to desalinate the salty water (Sadrzadeh and Mohammadi, is composed of a planar monolayer of sp2 -hybridized carbon atoms
2008; Mohammadi and Kaviani, 2003; Tofighy and Mohammadi, 2010; arranged in a regular hexagonal pattern. Pristine graphene, GO, and
Belessiotis and Delyannis, 2001; Hadadin et al., 2010; Kaldellis and reduced graphene oxide (RGO) are various forms of graphene used in
Kondili, 2007). different applications. Graphene requires special oxidation processes
There are many conventional desalination methods including pre- to introduce hydrophilic functional groups to improve its ion adsorp-
cipitation, oxidation, reduction, ion exchange, membrane filtration, tion capacity. GO is the oxidized form of graphene that can be produced
and adsorption. Considering from ease of process, efficiency and econ- by graphite oxidizing. After graphite oxidation, oxygen molecules inter-
omy point of view, adsorption is regarded as one of the most promising sperse the graphite carbon layers. By increasing the interplanar spacing
and widely used methods (Tofighy and Mohammadi, 2010; Rao et al., between the layers by exfoliation, graphite oxide changes into GO. The
2007; Bele et al., 2016). Adsorption efficiency directly depends on char- preparation of GO from graphite using the Hummers and the modi-
∗
Corresponding author.
E-mail address: torajmohammadi@iust.ac.ir (T. Mohammadi).
https://doi.org/10.1016/j.cherd.2018.08.022
0263-8762/© 2018 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 358–365 359
Fig. 1 – Schematic of GO synthesis by (a) the Hummers and (b) the modified Hummers methods.
fied Hummers methods introduce many oxygen containing functional 2.2. Methods
groups on the GO surface (hydroxyl and epoxy groups on the basal
plane and carboxylic acid groups at the edges of GO). These oxygen 2.2.1. GO preparation
containing functional groups on GO make a significant contribution to
GO was synthesized by the Hummers and the modified Hum-
its hydrophilicity and high negative charge density that are essential
mers methods. According to the Hummers method, graphite
for desalination application. Compared to other adsorbents including
(2 g) and NaNO3 (2 g) were mixed in 50 ml H2 SO4 (98%), and
activated carbon (AC), fly ash, sewage sludge ash, zeolites, biomateri-
als, recycled alum sludge, manganese oxides, peanut hulls, kaolinite,
the mixture was stirred for 2 h in an ice bath at a temperature
resins, rice husk, clay, sawdust and CNTs, GO with its unique physical of about (0–5 ◦ C). Then KMnO4 (6 g) was added to the mixture
and chemical properties such as large theoretical specific surface area slowly to keep the temperature under 15 ◦ C during KMnO4
(about 2620 m2 /g), surface – interaction, high negative charge den- addition. The ice bath was then removed and the mixture
sity and hydrophilicity is regarded as the most promising absorbent was stirred at 35 ◦ C for 2 days. Next 100 ml water was dropped
to adsorb various heavy metal ions (Thangavel et al., 2018; Paulchamy gently, and the temperature increased to 98 ◦ C, rapidly. Also
et al., 2015; Dai, 2002; Loryuenyong et al., 2013; Hegab and Zou, 2015; the mixture color was changed to brown. It was then diluted
Ramesha et al., 2011; Gopalakrishnan et al., 2015; Zaaba et al., 2017). with additional 200 ml of water. The reaction was completed
Therefore, GO should exhibit high adsorption capacity in salty water
by addition of 10 ml H2 O2 to react with additional KMnO4 .
desalination (sodium ions removal from sea water).
Then, the mixture was washed with HCl (10%) and deion-
As reported in literature, functionalization of GO can increase its
ized (DI) water by rinsing and centrifugation. The product was
adsorption capacity, improve its adsorption selectivity and facilitate
separation of the spent GO from water (Peng et al., 2017). For exam- dried under vacuum at room temperature and GO powder was
ple, introduction of ethylene diaminetetraacetic acid (EDTA) groups to obtained.
GO via silanization could dramatically increase its active adsorption In the modified Hummers method, graphite (2 g) and
sites i.e. EDTA-GO has more sites than GO (Madadrang et al., 2012). NaNO3 (2 g) were mixed in 90 ml H2 SO4 (98%) in an ice bath.
Additionally, poly (amidoamine) (PAMAM) was used for GO functional- Then after adding KMnO4 (12 g) slowly, 184 ml water was added
ization via grafting, and the functionalized GO demonstrated excellent to the mixture slowly. After 2 h, the ice bath was removed
adsorption capacity toward heavy metal ions such as Cu(II), Zn(II), and the mixture was stirred at 35 ◦ C for 2 h. Then the mix-
Fe(III), Pb(II) and Cr(III) (Yuan et al., 2013). For this aim, chitosan (CS), a
ture temperature was increased to 98 ◦ C, and when it was
partially deacetylated derivative of chitin, with exceptional properties,
cooled to room temperature, it was stirred for 2 h. Finally, it
such as high hydrophilicity, wide availability and biocompatibility, good
was treated with 40 ml H2 O2 and 200 ml water. Finally, the mix-
film forming ability, moderate chemical resistance, and its abundant
hydroxyl and amino functional groups as reactive sites can be used
ture was washed with HCl (10%) and DI water by rinsing and
for GO functionalization. Covalently bonded chitosan on GO combine centrifugation and the product was dried under vacuum at
the innate characteristics of chitosan and the unique features of GO room temperature (Paulchamy et al., 2015). Fig. 1 shows the dif-
(Bustos-Ramírez et al., 2013; Tofighy and Mohammadi, 2015; Nguyen ferent steps of the GO preparation procedure by the Hummers
et al., 2017). No previous published study on sodium ions removal from and the modified Hummers methods.
water using chitosan functionalized GO as adsorbent could be found in The morphology and structure of the GO prepared by the
the literature. Hummers and the modified Hummers methods were charac-
In this research, application of GO synthesized by the Hummers and terized by SEM (Tescan, A VEGA), XRD (Bourevestnik, Dron-8)
the modified Hummers methods and the chitosan functionalized GO
and FTIR (Shmadzu, IR solution 8400S) analysis.
as adsorbents for salty water desalination was investigated.
Fig. 2 – SEM images of (a) the Hummers and (b) the modified Hummers synthesized GO.
the experiments, 100 mg of the prepared adsorbents were dis- mass of dry adsorbent used (g) and V is the volume of sodium
persed in 25 ml of the solutions (with natural pH ∼ 6) at 25◦ C. ions solution (l).
Each experiment was performed twice and the average results
were reported with max error percent of about 5%. Atomic
adsorption spectroscopy was used to measure the sodium ion
3. Results and discussion
concentration of the solutions. After removing the adsorbents
SEM images are usually used to study structure and surface
from the solutions, at equilibrium, the amounts of adsorbed
morphology of nanomaterials. Fig. 2 shows SEM images of the
ions were obtained using the following equation:
synthesized GO via the Hummers and the modified Hummers
(C0 − Ce )V methods. As can be observed, the platelet-like form of GO is
qe = (1) seen in the both images.
w
XRD is a technique to determine distance between layers
Where qe is the equilibrium adsorption uptake (mg/g), C0 is of crystalline materials. After oxidation, the layers distances
the initial sodium concentration (mg/l), Ce is the equilibrium of the starting graphite and the product (GO) are highly dif-
sodium concentration (mg/l), V is the solution volume (l) and ferent and the XRD spectrum is a conclusive proof of the
w is the adsorbent mass (g). degree of oxidation. XRD patterns of the synthesized GO via
the Hummers and the modified Hummers methods as shown
2.2.4. Regeneration studies in Fig. 3 display 2 peaks at 11.3◦ and 11.7◦ , so the correspond-
ing interlayer spacing of the synthesized GO is 7.8 and 7.6 Å,
For regeneration study, after adsorption equilibrium at initial respectively. The interlayer spacing of the starting graphite is
sodium ions concentration of 10,000 mg/l, the adsorbents were about 3.4 Ȧ (inset in Fig. 3 a) that indicates the prepared GO via
retrieved and dried at 60◦ C for 2 h, and then dispersed in DI two methods are completely oxidized and the exfoliation pro-
water. After the solutions attained equilibrium, the sodium cess increases the interlayer spacing (Paulchamy et al., 2015;
ion concentrations were measured and desorption percentage Gopalakrishnan et al., 2015).
was calculated as follows: FTIR is a method to examine the obtained oxygen con-
taining functional groups after oxidation of graphite flakes.
qe (de)
DE (%) = × 100 (2) FTIR spectrums of the prepared GO by the Hummers and
qe (ad)
the modified Hummers methods, as seen in Fig. 4, show that
the synthesized GO via both methods are functionalized suc-
whereqe (ad) and qe (de) are the amounts of adsorption and
cessfully with different types of oxygen containing functional
desorption at equilibrium, respectively.
groups. The spectrums confirm presence of the C O bond in
the alkoxy group (1060 cm−1 ), the C O bond in epoxy group
2.2.5. Batch kinetics studies
(1226 cm−1 ), the unoxidized CC bonds (1620 cm−1 ), the car-
bonyl, and the starching vibration of carboxylic acid (COOH)
Kinetics studies were carried out with the similar procedure
groups (1733 cm−1 ), and the hydroxyl groups (3359 cm−1 ). It is
as the adsorption experiments with initial sodium ions con-
clear that both of the spectrums are similar, except one peak
centration of 10,000 mg/l. The aqueous samples were taken
at 1431 cm−1 in the modified Hummers method that indicates
at preset time intervals and the sodium ions concentration
the C OH bonding (Lai et al., 2016; He et al., 2015).
was similarly measured. The adsorption amount at time (t), qt
For better comparison, FTIR spectra of the neat chitosan,
(mg/g), was calculated using the following equation:
the prepared GO by the modified Hummers method and the
(C0 − Ct ) V chitosan functionalized GO (before and after adsorption pro-
qt = (3) cess) are shown in Fig. 5. As can be observed, the peaks of the
w
chitosan functionalized GO FTIR spectrum (curve c) are similar
where C0 is the initial sodium ions concentration (mg/l), Ct to those of the chitosan and the GO spectra (curves a and b).
(mg/l) is the sodium ions concentration at time (t), w is the The peaks at 1733 cm−1 and 1620 cm−1 of curve b are assigned
Chemical Engineering Research and Design 1 3 8 ( 2 0 1 8 ) 358–365 361
Hummers GO 1330
Modified Hummers GO 1228
Chitosan functionalized GO 1085
Table 3 – Pseudo-first-order and pseudo-second-order kinetic models parameters at initial ion concentration of
10,000 mg/l.
Adsorbents qe,exp (mg/g) Pseudo-first-order kinetic model Pseudo-second-order kinetic model
Table 4 – Comparison of the maximum monolayer ion adsorption capacities of the chitosan functionalized GO and the
other adsorbents documented in literature.
Adsorbents Adsorbed ions Maximum monolayer adsorption Conditions Refs
capacity, q (mg/g)
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The authors would like to thank Iran National Science Foun- gelöster stoffe, Kungliga Svenska Vetenskapsakademiens.
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