A low-cost and eco-friendly fabrication of an MCDI-utilized PVA/SSA/GA cation exchange membrane
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Green Processing and Synthesis 2022; 11: 563–571
Research Article
Hoang Long Ngo*, Ngan Tuan Nguyen, Thi Thanh Nguyen Ho, Hoang Vinh Pham,
Thanh Nhut Tran, Le Thanh Nguyen Huynh, Thi Nam Pham, Thanh Tung Nguyen,
Thai Hoang Nguyen, Viet Hai Le*, and Dai Lam Tran
A low-cost and eco-friendly fabrication of an
MCDI-utilized PVA/SSA/GA cation exchange
membrane
https://doi.org/10.1515/gps-2022-0056 ratio of 100:5:5) had the best water adsorption and
received January 15, 2022; accepted May 02, 2022 charge efficiencies that could be utilized for CDI appli-
Abstract: The alternative desalination technique of mem- cation. The membrane’s ability to desalinate water was
brane capacitive deionization (MCDI) has emerged in the assessed using electrical properties such as total resis-
last 15 years and received a lot of research attention since tance, specific capacitance, and electro adsorption coated
then. By using a voltage applied between two electrodes with the best ratio composite CEM. The salt absorption
covered with ion-exchange membranes, MCDI has attempted capacity of 19.06 mg·g−1 with stable performance was found
to challenge established methods such as reverse osmosis or to be encouraging.
electrodialysis. In this study, through the crosslinking of sul- Keywords: cation exchange membrane, capacitive deio-
fosuccinic acid (SSA) and glutaric acid (GA) with polyvinyl nization, polyvinyl alcohol, sulfosuccinic acid, glutaric acid
alcohol (PVA), cation exchange membrane preparation and
characterization were introduced. For the CDI system, mem-
branes were chosen based on their water absorption and ion
exchange properties. The PVA/SSA/GA composite (mass 1 Introduction
Climate change and global warming are now the most
crucial problems leading to many issues all over the
* Corresponding author: Hoang Long Ngo, Graduate University of
world. In Vietnam, there are sea-level rise and saliniza-
Sciences and Technology, Vietnam Academy of Science and
tion, together with drought, flood, and critical weather
Technology (VAST), Hanoi, Vietnam; NTT Hi-Tech Institute, Nguyen
Tat Thanh University, 300A Nguyen Tat Thanh, District 4, 700000 Ho [1]. Especially, it can affect the quantity and quality of the
Chi Minh City, Vietnam, e-mail: longnh@ntt.edu.vn water, resulting in the lack of water in many regions,
* Corresponding author: Viet Hai Le, Faculty of Materials Science typically the agricultural regions such as The Mekong
and Technology, VNUHCM-University of Science, 227 Nguyen Van Delta or The Long Xuyen Quadrangle in the dry season.
Cu, District 5, 700000 Ho Chi Minh City, Vietnam,
According to the recent reports, the salinization level of
e-mail: lvhai@hcmus.edu.vn
Ngan Tuan Nguyen, Thi Thanh Nguyen Ho, Hoang Vinh Pham,
the Mekong Delta reached 25 km of 10–30 g·L−1 [2]. There-
Thanh Nhut Tran, Le Thanh Nguyen Huynh, Thai Hoang Nguyen: fore, desalination is becoming more and more critical,
Department of Physical Chemistry, Faculty of Chemistry, VNU-HCM in terms of both agriculture and people’s life quality
University of Science, 227 Nguyen Van Cu, District 5, 700000 Ho Chi assurance.
Minh City, Vietnam In recent years, there have been a lot of desalination
Thi Nam Pham: Graduate University of Sciences and Technology,
technologies that have been utilized in a large scale for
Vietnam Academy of Science and Technology (VAST), Hanoi,
Vietnam; Institute for Tropical Technology, Vietnam Academy of agriculture all over the world, including various thermal,
Science and Technology, 18 Hoang Quoc Viet, Nghia Do, Cau Giay, electrical, and osmotic technologies [3]. Reverse osmosis
100000 Ha Noi, Vietnam (RO) was used in agriculture in Europe from the 1960s.
Thanh Tung Nguyen: NTT Hi-Tech Institute, Nguyen Tat Thanh Despite its high cost, this technology was applied for the
University, 300A Nguyen Tat Thanh, District 4, 700000 Ho Chi Minh
growth of highly economic vegetables and was usually
City, Vietnam
Dai Lam Tran: Institute for Tropical Technology, Vietnam Academy of
employed in the greenhouse [4]. In addition, RO technology
Science and Technology, 18 Hoang Quoc Viet, Nghia Do, Cau Giay, is remarkably effective when applied in the brackish water,
100000 Ha Noi, Vietnam as well as high membrane stability and good salt recovery;
Open Access. © 2022 Hoang Long Ngo et al., published by De Gruyter. This work is licensed under the Creative Commons Attribution 4.0
International License.
564 Hoang Long Ngo et al.
however, the price is very expensive due to its high cost of more noticeable, not only in the fields of desalination and
energy, installation, and operation. Nanofiltration (NF) uses water treatment but also in the food industry and the fuel
the membranes with the pore size of 0.5–1.5 nm, which is cell fabrication [17–19]. Compared to the conventional CDI,
able to work at lower pressure, higher water flux, and lower MCDI exhibits better salt removal efficiency [18,20–22],
cost, and is utilized for water softening or organic com- faster desalination rate [18], higher current efficiency
pound removal from brackish water [5]. Electrodialysis [9,21–23], and lower energy consumption [9,24]. Further-
(ED) is the technology to separate the ions from the solution more, MCDI can operate at thermodynamic efficiencies
using ion exchange membrane under the potential gradient comparable to that of RO [25].
[5], where the cations (Na+, K+, NH4+) will come to the Nevertheless, there are two distinct disadvantages
cathode and the anions (Cl–, SO42–, PO43–) will come to that hinder the performance and the commercialization
the anode. Cation exchange membranes (CEM) or anion of MCDI: the high cost of the ion exchange membranes,
exchange membranes (AEM) are also employed to enhance and the high bulk resistance caused by the adhesive
the ion removal capability and improve clean water supply between the electrode and the ion exchange membrane
[6]. ED technology is usually used for brackish water filtra- [26]. As a result, many scientists have focused on the mate-
tion to provide clean drinkable water with very low-energy rials for ion exchange membrane with better mechanical
usage [7]. Ion exchange (IX) uses ion exchange resins to properties, higher chemical resistance, and lower cost [27].
filter and remove the contaminants from water and other Among the researched materials, polyvinyl alcohol (PVA)
solutions. These cation- or anion-exchange resins can be is popular, easy to dissolve in water, and environmentally
regenerated using the corresponding acids or bases [5]. friendly, and has been utilized in many membrane fabrica-
IX technology has many advantages, namely, low cost, tion processes [28,29] thanks to its excellent film forming
high quality of water, simple operation and equipment, ability, high thermal and chemical stability, and good cross-
and reduced energy and labor requirement. However, the linking capability [30–32]. The PVA cross-linking process
ion exchange-based desalination process may encounter a helps modify its physical properties, flexibility, thermal sta-
drawback, which is the regeneration process greatly depending bility, as well as its solubility in water, water uptake, and
on the chemicals. water swelling ability [33–35]. However, due to the lack of
Besides the aforementioned desalination technolo- the functional groups, PVA normally exhibits low ionic con-
gies, capacitive deionization (CDI) is emerging as an ductivity [36]; thus, it is usually necessary to provide the
advanced technology that has been attracting significant organic functional groups such as hydroxyl (–OH), carboxylate
attention in the recent years, thanks to its low cost and (–COOH), sulfonate (–RSO3), amine (–NH2), and quaternary
reduced energy demand compared to the conventional ammonium (–NR4) [37]. The compounds with multiple
technologies such as reverse osmosis or electrodialysis. functional groups are also able to go through cross-linking
CDI can desalinate water by storing ions in an electrical reaction with the hydroxyl groups in PVA to form a net-
double layer (EDL) on the electrode surface, which can work structure [38,39]. Sulfosuccinic acid (SSA), as a
also be utilized in various water treatment processes such cross-linking agent (–COOH) as well as a hydrophilic func-
as water softening and waste water treatment [8–10]. tional group donor (–SO3H), can also be employed to man-
However, there are also some downsides in the CDI tech- ufacture cation exchange membrane together with PVA to
nology. One of them is the electrode deterioration as enhance the desalination efficiency of CDI [21,40]. In addi-
an amount of ions cannot be washed completely from tion, citric acid (CA) can also be utilized to reduce the cost
the electrode, leading to performance degradation [11,12]. of cation exchange membrane, as the CA/SSA/PVA mem-
To solve this problem, membrane capacitive deionization brane exhibited high desalination efficiency thanks to the
(MCDI), an upgrade from the traditional CDI, was pro- sulfonic acid (–SO3H) and carboxyl (–COOH) groups that
posed [13,14]. MCDI utilizes the ion exchange membrane did not participate in the cross-linking process [41]. There
with high ion selectivity that can block the reverse adsorp- are many cross-linking agents that can provide PVA with
tion and prevent the co-ion transportation. In MCDI, anion hydrophilic functional groups, such as poly(4-styrene sul-
exchange membrane (AEM) is put before anode to prevent fonic acid-co-maleic acid) (PSSA_MA) [42], glutaric acid
the moving of cations, and cation exchange membrane (GA) [43], and sulfonated PVA (sPVA) [44] and polysul-
(CEM) is placed before cathode to inhibit the transfer of fone (SPSf) [44].
the anions, reducing the co-ion effect and ameliorating the In this research, we present a low-cost and environ-
salt removal efficiency, as well as preventing the faradaic mentally friendly fabrication of PVA/SSA/GA membrane
reactions on the electrode surface [15,16]. MCDI is becoming and its application as cation exchange membrane. Physical,
Low-cost and eco-friendly fabrication of an MCDI-utilized PVA membrane 565
mechanical, and chemical properties of the membranes To fabricate the free-standing ion exchange mem-
were examined; electrochemical properties and desalination brane, the PVA/SSA composite solution was spread on
efficiency were also investigated. a petri dish and dried at 40°C to obtain a dry membrane
and then continued to be dried at 80°C in 1 h for the high-
temperature cross-linking reaction to proceed. Next, the
membrane was immersed in the distilled water in 6 h for
2 Materials and methods three times to remove the unreacted components and
then was dried at 60°C for 4 h. The GA and SSA concen-
trations were varied as specified in Table 1. This free-
2.1 Materials and chemicals
standing ion exchange membrane was utilized to investigate
the properties such as water uptake or ion exchange
Polyvinyl alcohol (98%, M = 146,000–186,000 g·mol−1)
capacity.
and glutaric anhydride (95%) were purchased from Acros,
PVA/SSA composite gel solution was also coated on
Belgium. Commercial activated carbon was supplied from
the electrode by the doctor blade with the dried thick-
Trabaco (Vietnam). Multiwalled carbon nanotube (MWCTN)
nesses of 20–30 µm. The composite membrane electrode
was supplied from Ntherm (USA). Sulfosuccinic acid (SSA),
was dried at 120°C in 4 h.
concentrated nitric acid, concentrated sulfuric acid, hydro-
chloric acid (37%), and ammonia solution (25%) were
acquired from Sigma Aldrich (USA) and were used without
any further purification. Graphite sheet (thickness of
2.4 Membrane characterization method
200 µm) was supplied by Mineral Seal (USA).
FT-IR spectra were recorded on Cary 630 FT-IR (Agilent
Technologies Inc., Santa Clara, CA) in the range of
2.2 Preparation of composite membrane 4,000–650 cm−1 using the free-standing membrane in
electrode the ATR mode. The morphology of the materials was inves-
tigated using a scanning electron microscope (SEM; JSM-
Glutaric anhydride (GA) was added into the 6% PVA solu- 6510LV instrument JOEL).
tion, and the mixture was stirred for 1 h. Then, MWCNT
was added, and the mixture continued to be stirred for
another 1 h. The resultant mixture was homogenized in
5 min at 15,000 rpm, and then, AC was added at the ratio 2.5 Water uptake capacity
suggested in the published literature [45], and the mix-
ture was further homogenized in 5 min. The mixture was The composite membrane was soaked in water for 24 h at
then coated on a graphite sheet (200 mm × 300 mm, room temperature, and then, it was taken out, and the
thickness of 200 µm). Finally, the composite membrane excess water on the surface was blotted quickly. The
electrode was dried at 120°C in 4 h. soaked sample was weighed (mw) and then dried at
45–50°C until unchanged weight (md). Water uptake
capacity of composite membrane was calculated based
2.3 Preparation of PVA/SSA/GA membrane on the following formula:
mw − md
First, PVA was dissolved in H2O at 80–90°C until the MC (%) = (1)
md
solution became clear. Next, sulfosuccinic acid (SSA)
solution was added, and the mixture was continually
stirred at 50°C for 4 h. The resultant solution was the
composite obtained from the reaction between PVA and
Table 1: Composition of the composite membranes by molar ratio
SSA. This composite solution could be directly coated on
the electrode surface or spread on a petri dish to receive
Sample name PVA SSA GA
the ion exchange membrane. The composite solution or
the PVA/SSA membrane could be further mixed with glu- PVA 100 0 0
G-PVA 100 0 5
taric anhydride (GA) for the cross-linking reaction to
SG-PVA 100 5 5
modify the properties of the membrane.
566 Hoang Long Ngo et al.
where mw and md (g) were the wet and dry membrane each other by an insulating silicone plate. The feed water of
mass, respectively. 200 ppm NaCl solution was pumped through the CDI cell at
a constant rate of 10 mL·min−1. The conductivity (G) of the
inlet solution was observed until remain unchanged (G0).
2.6 Cation-exchange capacity Next, the potential of 1.2 V was applied to the CDI cell, and
the decreasing specific conductivity (Gt) was noted every
The cation exchange capacity is an essential electroche- 30 s until remain unchanged (Gc).
mical property of an ion-exchange membrane and is a Salt adsorption capacity (SAC) was calculated from
measure of the number of fixed charges per unit weight the following formula:
of the dry membrane. To determine CEC, the membrane
(C0 − Ct ) × V
was immersed in H2SO4 for 24 h to convert it to H+ forms SAC = (3)
m
and then rinsed with distilled water to remove the excess
acid. Finally, the membrane was soaked in NaCl for 24 h, The following formula determined the salt adsorp-
and the released H+ amount was titrated with NaOH in tion rate (SAR):
the presence of phenolphthalein. The cation exchange SAC
SAR = (4)
capacity (CEC; mmol·g−1) was calculated from the fol- t
lowing equation:
where SAC (mg·g−1) is the salt adsorption capacity; SAR
CEC =
CNaOH × VNaOH
(2) (mg·g−1·min−1) is the salt adsorption rate; C0 and Ct
g (mg·L−1) are the concentrations of the NaCl solution,
which were calculated from the conductivity of the solu-
where m is the mass of the dry membrane, CNaOH is the
tion at the beginning and at t (min), respectively; V (L) is
concentration of the NaOH solution, and VNaOH is the
the volume of the NaCl solution; m (g) is the mass of the
volume of the NaOH solution.
electrode; and t (min) is the adsorption time.
2.7 Salt adsorption on composite membrane
electrode
3 Results and discussion
To investigate the desalination performance, the MCDI
system was set up as described in Figure 1, consisting 3.1 FT-IR analysis
of a CDI cell, a peristaltic pump, and a conductivity meter.
The CDI cell is composed of a pair of parallel electrodes The incorporation of sulfosuccinic acid (SSA) onto the
(3.0 cm × 2.5 cm, thickness of 100–300 µm) separated from PVA chain was determined using Fourier-transform
Figure 1: Schematic illustration of CDI system.
Low-cost and eco-friendly fabrication of an MCDI-utilized PVA membrane 567
Figure 2: FT-IR spectra of PVA, G-PVA, and SG-PVA.
infrared spectroscopy (FTIR), and the results are dis-
played in Figure 2 and are consistent with the previous
researches [46,47]. Particularly speaking, the peaks at
Figure 3: Water uptake capacity of PVA, G-PVA, and SG-PVA.
3,500–3,300 and 3,000–2,800 cm−1 are attributed to the
–OH and the –CH groups of PVA, respectively. In the
presence of GA and/or SSA, the peak at 1,735–1,715 cm−1 635.70% of PVA to 175.20% and 137.40% of G-PVA and
appeared, which is ascribed to the C]O bond of the car- SG-PVA, respectively). This phenomenon can be eluci-
boxyl group (–COO–) [46], confirming that the cross- dated by the cross-linking reaction between SSA and GA
linking reaction happened in the G-PVA and SG-PVA with PVA as displayed in Scheme 1, where the carboxylic
samples. Furthermore, a new peak at 1,040–1,020 cm−1 groups of GA and the anhydride carboxylic groups of
can also be observed, which is accredited to the S–O SSA reacted with the hydroxyl groups of PVA, reducing
bond of the sulfonic acid group (–SO3) of SSA, verifying the number of –OH groups in the PVA chain and thus
the successful addition of SSA to the PVA structure, as diminishing the hydrophilicity of the PVA-based com-
cross-linking agent as well as functional group donor. posite membrane. Furthermore, there is a chance that
the remaining free uncross-linked hydroxyl groups could
also be blocked by the cross-linked ones, leading to lim-
3.2 Water uptake capacity ited contact with H2O and consequently inferior water
uptake capacity of G-PVA and SG-PVA compared to the
Water uptake capacity is one of the most important fac-
pure PVA membrane.
tors to assess the performance of the ion exchange
membrane, as water is mostly utilized as the working
environment. The swelling behavior investigation was
performed at room temperature, and the water uptake 3.3 Ion exchange capacity
capacities of PVA, G-PVA, and SG-PVA samples are shown
in Figure 3. The water uptake capacity recorded a dramatic The ionic conductivity and ion exchange capacity of an
70% drop in the presence of the cross-linking agents (from ion exchange membrane are two of their most important
Scheme 1: Expected cross-linking reaction between SSA with PVA.
568 Hoang Long Ngo et al.
Figure 4: Cation exchange capacity of PVA, G-PVA, and SG-PVA. Figure 6: The SAC as a function of desalination time for all PVA
membrane electrodes (voltage: 1.2 V; flow rate: 10 mL·min−1).
properties: the ionic conductivity specifies how easy the
ions can transport through the membrane, while the ion and consequently the improvement of the ion exchange
exchange capacity indicates the amount of replaceable capacity of the composite membrane.
ions in the membrane. In this case, ion exchange capacity
is determined by the number of active sites or the number
of functional group possessing the ion exchange ability,
which in this research is the sulfonic group. As observed 3.4 Scanning electron microscopy analysis
in Figure 4, in the case of PVA and G-PVA membranes,
without the ion exchange groups, the IEC values were Figure 5 displays the SEM image of the SG-PVA mem-
very low (0.0168 and 0.0224 mmol·g−1, respectively). In brane electrode, showing its differences with the carbon
the presence of the –SO3 functional group from SSA, the electrode. It can also be observed that direct coating of
IEC value of SG-PVA increased to 2.423 mmol·g−1, proving the PVA/SSA/GA composite onto the electrode surface
the successful incorporation of SSA onto the PVA chain provided good contact between the membrane and the
Figure 7: The conductivity as a function of desalination time for all
Figure 5: SEM image of SG-PVA membrane electrode. PVA membrane electrodes (voltage: 1.2 V; flow rate: 10 mL·min−1).
Low-cost and eco-friendly fabrication of an MCDI-utilized PVA membrane 569
electrode, resulting in lower bulk resistance compared to and right corner of the graph, which means higher elec-
when using free-standing membrane. trosorption capacity and faster electrosorption rate simulta-
neously. The Ragone plots for three-membrane electrodes of
PVA, G-PVA, and SG-PVA are exhibited in Figure 8. Among
3.5 Deionization tests the curves, SG-PVA appears in the most upper and right
corner in this group, indicating that SG-PVA membrane elec-
To determine the salt adsorption capability of the fabri- trode displayed the highest salt adsorption capacity and
cated cation exchange membranes, the deionization tests fastest electrosorption rate compared to other electrodes.
were performed in the aforementioned MCDI system as
illustrated in Figure 1. Figure 6 represents the salt adsorp-
tion capacity (SAC) of PVA, G-PVA, and SG-PVA mem- 4 Conclusion
brane electrodes as a function of the desalination time. It
can be observed that the SAC value increased rapidly In this study, to develop a CDI cell with ion-exchange
within the first 15 min and then became saturated after membrane, a PVA-based composite was synthesized and
30 min at 1.2 V and a flow rate of 10 mL·min−1. PVA displayed the desalination performance on the NaCl adsorption was
the highest SAC value of 9 mg·g−1, higher than that of G-PVA investigated. According to the results, the salt adsorption
(4 mg·g−1) but lower than that of SG-PVA (19 mg·g−1). It is of the PVA/SSA/GA composite membrane appeared to be
clearly observed that the incorporation of SSA into PVA superior to that of the PVA and PVA/GA. The Ragone plot
enhanced the salt adsorption capability of the membrane shows that the electrode coated by SG-PVA membrane
through the sulfonic groups (–SO3H). Conversely, the cross- exhibited higher adsorption ability and higher charge
linking with GA consumed and reduced the number of rate. Water and ion conductivity were improved by the
hydroxyl groups (–OH) in the PVA chain, leading to the dete- incorporation of SSA into the PVA backbone. Overall,
rioration of the salt removal capability of MCDI. These results this study sheds light on the introduction of a low-cost
are also consistent with the conductivity test demonstrated in and long-lasting ion-exchange membrane for MCDI sys-
Figure 7, where SG-PVA membrane electrode reduced around tems used in the desalination process.
75% of the conductivity (from 400 to 100 μS), higher than
pure PVA (325 μS), and G-PVA (250 μS). Funding information: The research is funded by The
The salt adsorption rate (SAR), which describes the Graduate University of Science and Technology under
rate of adsorption, is also an important parameter in CDI grant number: GUST.STS. ĐT2020-HH08.
applications. The performance of a CDI system becomes
evidently clear when the SAR is plotted against SAC, Author contributions: Hoang Long Ngo: methodology,
which is also known as the Ragone plot. Obviously, writing – original draft; Ngan Tuan Nguyen: investigation,
an ideal state is that the curve appears in the upper visualization; Thi Thanh Nguyen Ho: software, visualiza-
tion; Hoang Vinh Pham: investigation; Thanh Nhut Tran:
methodology; Le Thanh Nguyen Huynh: investigation;
Thanh Tung Nguyen: writing – original draft; Thi Nam
Pham: project administration, funding acquisition; Thai
Hoang Nguyen: resources, supervision; Viet Hai Le:
writing – review and editing, supervision; Dai Lam Tran:
funding acquisition.
Conflict of interest: The authors state no conflict of interest.
Data availability statement: Available data are presented
in the manuscript.
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