Graphene and Nano Tubes For Water Filtration
Graphene and Nano Tubes For Water Filtration
Graphene and Nano Tubes For Water Filtration
A R T I C L E I N F O A B S T R A C T
Keywords: Enhanced use of heavy metals for commercial and non-commercial applications has resulted in industrial and
Carbon nanotubes domestic discharge loaded with toxic metal ions creating increased environmental concern. Owing to the wide
Heavy metal array of heavy metals that can be effectively removed, relatively low cost and economical process conditions,
Adsorption
removal of heavy metals by adsorption has attracted the scientific community over years. Search for novel ad
Functionalization
sorbents which are cost-effective with higher adsorption affinity and reusability has been an area of active
research. Carbon based adsorbents, which offer enhanced surface area, higher surface to volume ratio and ease of
surface functionalization, have proven to be more effective than conventional adsorbents for removal of both
inorganic and organic contaminants. Among the various carbon based adsorbents, carbon nanotubes, graphene
and modified graphene oxide composites are gaining increasing importance as effective adsorbents for heavy
metal removal from waste waters. This paper presents a comprehensive review on use of these adsorbents for
adsorptive removal of various heavy metals. Optimal conditions for maximum removal of various metal ions are
highlighted. Case studies on approach to surface functionalization of adsorbents and the mechanism of metal ion
removal by the functionalized surface are discussed for practical application.
* Corresponding author at: Department of Chemistry, M S Ramaiah Institute of Technology, Bengaluru-560054, Karnataka, India.
** Corresponding author at: Department of Biotechnology, M S Ramaiah Institute of Technology, Bengaluru-560054, Karnataka, India.
*** Corresponding author at: Department of Chemistry, RV College of Engineering, Bengaluru-560059, Karnataka, India.
E-mail addresses: rhk.chem@gmail.com (R.H. Krishna), chandraprabhamn@yahoo.co.in (M.N. Chandraprabha), girichem@yahoo.co.in (S.G. Kumar).
https://doi.org/10.1016/j.apsadv.2023.100431
Received 30 January 2023; Received in revised form 10 June 2023; Accepted 17 June 2023
Available online 29 June 2023
2666-5239/© 2023 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
R.H. Krishna et al. Applied Surface Science Advances 16 (2023) 100431
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Fig. 1. Basic terms of adsorption process. Figure reproduced with permission from [53]
Fig. 2. different geometry of CNTs – (a) unrolled graphene sheet showing SWCNT geometry, (b) zig-zag, (c) armchair and (d) chiral (Figure reproduced with
permission from [65].)
toward the pollutants in wastewater at lower concentrations, compounds, bisphenol A, aromatic dyes, etc) and heavy metal ions (Ex.
industrial-scale use, mechanical strength. As(III) or As(V), Pb(II), Cu(II), Cr(III) or Cr(VI), Co(II), Cd(II), Hg(II), U
(VI), Eu(III), Sr(II), etc) [59,60]. The following paragraphs highlight the
5. Carbon based materials as adsorbents application of carbon nanotubes and graphene-based materials for
adsorptive removal of metal ions.
Demand for novel materials that can overcome the limitations of
conventional adsorbents has led to increased application of carbon-
based materials (ex. carbon nanotubes, graphene and its composites, 5.1. Carbon nanotubes (CNTs)
fullerene etc) for adsorptive removal of organic and inorganic pollutants
[7,57,58]. These materials have an advantage of excellent physical and Carbon nanotubes (CNTs) are allotropic forms of carbon with tubular
chemical properties with high surface area resulting in good adsorption nano- architecture that are made of cylindrical graphene sheets
capability. Their unique chemically reactive structure enabling easy composed from carbon atoms arranged in hexagonal beehive pattern
functionalization coupled with ease of synthesis by various routes has [61]. It was first detected in 1952 by Radushkevish and Lukyanovich,
resulted in use of these materials as new generation adsorbents for the but in recent history, the discovery is ascribed to S. Iijima who obtained
removal of various organic compounds (Ex. phenol, antibiotics, benzene multi-walled carbon nanotubes from carbon soot during the fabrication
of C60 carbon molecule by arc evaporation process [62–64]. The
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wastewater [78].
CNTs have shown promise as adsorbents for adsorption of various
metal ions such as Co(II), Ni(II), Pb(II), Sr(II), Zn(II), Cu(II), Cr(VI) and
Cd(II) from wastewater of many industries such as battery industries,
metal plating facilities, chemical manufacturing and mining operation
[79–81]. In addition, CNTs are used as promising adsorbents in textile
industries for removal of synthetic dyes from wastewater [82].
Based on the target contaminants chemical nature and intended
application, various functional groups are introduced on CNT surfaces,
at sidewalls and at the tips to remove environmental contaminants
especially from wastewater effectively. Functionalization or modifica
tion is carried out to improve the affinity of CNTs towards hydrophilic
ions or molecules. The statistical data obtained from scopus data base for
the different terms given in Fig. 4 shows that the recent trend and
Fig. 3. Structure of (A) SWCNT and (B) MWCNT (Figure reproduced with increased interest among the researchers for the functionalized carbon
permission from [66].) nanotubes.
CNTs are commonly functionalized through chemical oxidation, in
thickness of CNTs is of about 1/50000th of human hair. Depending on which oxygen containing functional groups are incorporated (e.g.,
the geometry, CNTs exist in three forms such as chiral, zig-zag and -COOH, -C=O and –OH) resulting in CNTs affinity to heavy metal cations
armchair (Fig. 2). Further, CNTs are classified into two types based on [80,83,84]. Surface oxidation is usually carried out under reflux con
the number of layers, as single-walled carbon nanotubes (SWCNTs) and dition using single or combination of inorganic acids (e.g., H2SO4 and
multi-walled carbon nanotubes (MWCNTs) (Fig. 3). The diameter of HNO3) and oxidizing agent (e.g., NaOCl, KMnO4 and H2O2) via liquid
SWCNTs is about 0.4 to < 3 nm, whereas in case of MWCNTs diameter phase oxidation method [85]. Datsyuk et al., [86] observed higher de
ranges from 1.4 to 100 nm. gree of functionalization of MWCNTs in the presence HNO3 than
Numerous methods have been developed to synthesize CNTs with H2SO4-H2O2 mixture treatments. Further, microwave irradiation can
different morphology and structure. But most commonly used methods accelerate acid functionalization by irradiating for 20 to 40 min
are chemical vapour deposition (CVD), laser ablation and arc discharge. [87–89].
The elements required for synthesis of CNTs are carbon source, sufficient To overcome the problems of low surface area and formation of
energy and catalyst. The feature of all above methods is to provide en mesoporous structure by aggregation of CNTs resulting in structural
ergy to the source of carbon leading to production of carbon fragments alternations, alkali activation of CNTs are carried out. In this method,
which undergo recombination, generating of CNTs. The source of energy powder form of MWCNTs are mixed with KOH and heated to 750◦ C for 1
might be electricity, heat or high-intensity light from arc discharge, h, sparged with argon gas followed by washing with concentrated HCl,
furnace used in CVD and laser (laser ablation), respectively [67]. deionized water and dried. The CNTs activated by alkali treatment were
Due to their superior optical activity, electrical conductivity, thermal successful in adsorbing both cationic and anionic dyes, as well as m-
properties, mechanical strength and chemical reactivity [61], CNTs have xylene, ethylbenzene and toluene found in aqueous solutions [90,91].
been used in numerous applications such as energy storage and con Separation of spent adsorbents after contaminants or heavy metal
version devices [68], sensors [69], hydrogen storage media [70], removal from aqueous solutions or remediation treatment is one of the
nanosized semiconductor devices [71], field emission displays [72] and critical aspects in adsorption process. Tiny nanoparticles may be sepa
radiation sources [73], probes [74], drug delivery systems [75] and rated using centrifugation or filtration from aqueous solution, but cost
artificial implants [76], high strength composites [77] etc. and energy involvement is high. Thus, developing cost-effective tech
Apart from this, CNTs have been used in wastewater treatment as nology by providing magnetic properties to adsorbents has significantly
well as for drinking water purification due to enhanced adsorption, gained importance [85]. Incorporation of magnetic properties to
catalytic and electrochemical properties combined with high mechani MWCNTs is usually obtained by grafting magnetic iron oxide nano
cal strength, high specific surface area, superior water transport prop particles (magnetite (Fe3O4) or maghemite (γFe2O3)) via multistep
erty and excellent chemical inertness. Various water treatment sol-gel process. The obtained MWCNTs will have increased affinity to
applications of CNTs includes oil-water separation, water desalination, wards anionic dye compounds and heavy metals [92,93]. Further, alkali
removal of emerging pollutants such as persistent organic pollutants, precipitation method are also used to achieve incorporation of magne
pharmaceutical products etc. and removal of heavy metals from tite (Fe3O4) nanoparticles on oxidized MWCNTs [94–97]. It was found
Fig. 4. Bar graph showing the number of articles in year wise in last decade appeared in Scopus data base for the keywords “Functionalized carbon nanotubes”,
“Modified carbon nanotubes” and “Functionalized carbon nanotubes+ Adsorption”.
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Table 3
Adsorptive capacity of carbon nanotubes modified with supports and different functionalization materials.
Adsorbent Metal pH Specific surface area of Sorption References
ion adsorbent efficiency/
(m2/g) sorption capacity
(mg/g)
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Table 3 (continued )
Adsorbent Metal pH Specific surface area of Sorption References
ion adsorbent efficiency/
(m2/g) sorption capacity
(mg/g)
that magnetic nanoparticle – CNTs composite effectively removed heavy In recent years, modification of CNTs with nano-zero-valent iron
metals [98], dye compounds [99], atrazine [100] and arsenic [101] (nZVI) has been successfully achieved for application in adsorptive
form wastewater. removal of azo dyes [107], hexavalent chromium [108], nitrobenzene
CNTs are also functionalized with different non-magnetic metal ox [109] and selenite [110] from wastewater.
ides such as ZrO2, TiO2, Fe3O4, CeO2, as well as bimetallic Pd/Fe-Fe3O4 Apart from this, to improve the adsorption affinity towards specific
to achieve higher affinity towards contaminants. The metal oxide-CNTs compound or element, CNTs are also functionalized or modified with
hybrids successfully adsorbed toxic metal ions such as Cd(II), Fe(II) or Fe polymers of different types such as poly(propyleneimine)dendrimers
(III), Cu(II) and As(III) or As(V) from water [88,89,101–106]. Modifi [111], poly(methyl methacrylate) [112], polyamine [113] and natural
cation of CNTs with metal oxides is carried out by functionalization of biopolymers (e.g., guar gum) [114]. MWCNTs modified with polymers
CNTs by chemical oxidation method followed by alkali precipitation of were efficient in adsorbing single and multicomponent organic dye so
metal oxides on nanotubes surface [88,89]. lutions as well as heavy metals. Other CNTs functionalization or
Fig. 5. Mechanism of adsorption of metal ions by PAMAM/CNT nanocomposite (Figure reproduced with permission from [115].)
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modification procedures include specific chemical derivatization, poly be broadly classified into two categories such as,
mers and coupling with other carbon based adsorbents (such as gra
phene or biochars) [85]. 1 Graphene oxide (GO) and reduced graphene oxide (rGO)
In summary, CNTs have been explored for removal of various heavy 2 Organic, inorganic, metallic and polymeric composites of GO and
metal ions with modification by organic or inorganic groups. Adsorptive rGO.
capacity of carbon nanotubes modified with supports and different
functionalization materials is tabulated in table 3. CNTs modified with GO, which is obtained by chemical exfoliation of graphite, is an
poly(amidoamine) PAMAM dendrimer showed highest adsorption ca oxidative form of graphene which contains a large number of oxygen
pacity of 4870 mg/g for Pb(II), while oxidized MWCNTs modified with functional groups like hydroxyl, carbonyl, carboxyl, epoxy etc. [152].
surfactant (benzalkonium) showed lowest adsorption capacity of 3.27 Presence of these oxygen functional groups in the GO structure results in
mg/g for Pb(II) [115,116]. Similarly, significantly high amount of As increased interlayer separation compared to graphite. This leads to
(III) (432 mg/g) was adsorbed by CNTs modified with dendrimers while changes in carbon hybridization resulting in a mixture of sp2 and sp3
poor adsorptive removal of 1.897 mg/g was exhibited by Fe-inserted hybridization in GO. The oxygen groups, due to their binding to inor
carbon nanotubes oxidized with nitric acid (FCNT-OX) [117,118]. In ganic metal ions and organic molecules via electrostatic interaction and
case of adsorptive removal of Co(II), maximum capacity of adsorption coordination, makes GO an ideal adsorbent material for removal of
was observed in CNTs coated with poly(amidoamine) PAMAM den inorganic and organic pollutants [153].
drimer (494 mg/g) while the lowest was obtained for bare CNTs (9.78 Reduced GO (rGO) is obtained by chemical or thermal reduction of
mg/g) [117,119]. Adsorption capacity of Cd(II) was highest in 3-amino GO resulting in removal of oxygen functional groups from GO. It has
pyrazole modified multi-walled carbon nanotubes (400 mg/g) and properties similar to graphene, yet with altered structure, presenting
lowest in unmodified CNTs (2.02 mg/g) [120,121]. In case of Hg(II), the carbon vacancies and clustered pentagons and heptagons, as well as
adsorptive capacity was highest for KMnO4 oxidized and Deep Eutectic some residual oxygenated groups [154,155]. Although GO has a
Solvent (DES) from Allyltriphenylphosphonium bromide (ATPB) - chemically reactive structure compared to rGO, the hydrophilic nature
Glycerol functionalized CNTs (186.97 mg/g) while Sulphur containing of GO can lead to poor adsorption capability and difficulty in its removal
multi-walled carbon nanotubes exhibited very poor adsorption (0.0728 from the solution. Reduced GO is therefore explored extensively for
mg/g) [122,123]. The adsorption of mercury onto sulphur containing adsorption applications.
multi-walled carbon nanotubes was controlled due to chemisorption Selective and enhanced adsorption by graphene based materials
process via Hg-S bond formation. Form the above results and literature have been reported to be enhanced by suitable chemical modification
review it is clear that polymer and organic molecule modified CNTs are and functionalization of GO and rGO [156]. The widely utilized func
more efficient in removal of heavy metals from aqueous solutions and tionalized graphene-based materials are organic, inorganic, metallic and
wastewater. The optimal pH for Pb(II), As(III), Co(II), Cd(II) and Hg(II) polymeric composites of GO and rGO. Some of the reported synthetic
removal is 5-7, 3-7, 6-7, 6-9 and 5-8, respectively for various modifi routes of these composites include hydrothermal, co-precipitation, solid
cation of CNTs. Hayatiet al., [115] reported that super adsorptive ca state dispersion, solution combustion etc. Some of the functionalization
pacity of polymer (PAMAM dendrimer) modified CNTs is due to the high strategies include use of inorganic materials, organic molecules, metal
surface area of composite and amino terminal groups leading to organic frameworks, polymers, zeolites and combinations of these.
adsorption of heavy metal ions by van der Waals, hydrogen, and elec Inorganic materials for functionalization of graphene include various
trostatic force. The mechanism which plays an important role in removal metals, metal oxides, ceramic materials. Magnetic inorganic materials
of Pb(II) and Cu(II) ions by PAMAM/CNT composite is based on van der are most commonly considered due to their ease of separation after
Waals, electrostatic, encapsulating and chelating interactions. Metal ion adsorption. Nanoscale inorganic materials with enhanced magnetic
encapsulation and chelating can be attributed to the transfer of charge of properties and catalytic adsorption have been used to obtain GO com
ligand to the metal as well as coordination of metal ion with one or more posites with excellent adsorption capacity. Extensive studies have been
of the tertiary amine sites of the PAMAM’s as depicted in Fig. 5. In reported on Fe3O4 impregnated GO and rGO sheets for sustainable and
addition to above, contaminants get encapsulated also due to the pres efficient removal of several metal ions [157]. Other inorganic materials
ence of nanopores in the composite sorbent structure [115,124]. considered are MnO2, SiO2, TiO2, layered double hydroxides, semi
conducting materials like CdS etc.
5.2. Graphene based adsorbents Functionalization with organic molecules is achieved by covalent
modification or non-covalent decoration. Ethylenediaminetetraacetic
Graphene, owing to its advantages like availability from several acid (EDTA) is one of the commonly used organic molecules in GO
facile synthesis techniques, excellent mechanical, physical and chemical composites. Ethylenediaminetetraacetic acid (EDTA) decorated GO
properties, large surface area, possibility to form surface active sites shows enhanced adsorption of metal ions due to increased surface
with ease of modification and functionalization, and characterized by functional groups. Cetyltrimethylammonium bromide (CTAB) prevents
their delocalized π-electron systems has attracted immense attention as agglomeration of GO and contributes to enhanced adsorption. Some of
an efficient adsorbent for removal of various contaminants like heavy the other organic molecules considered for GO composites used in
metals and complex organic pollutants like pharmaceuticals, dyes, an adsorption are triisopropanolamine, aminopyrazole etc.
tibiotics etc. Graphene is a 2D material made of one atom thick layer of Polymers are considered as functionalising molecules due to the
hexagonally arranged sp2-hybridized carbon atoms with close-packed large functional groups present in them. Some of the polymers used for
honeycomb crystal lattice connected by σ and π bonds. It can be easily GO and rGO composites are polypyrrole, polyaniline, poly(amido
modified by chemical reactions. amine), poly(N-vinylcarbazole), chitosan, cellulose, epoxy resin. Poly
Graphene can be synthesized by bottom-up or top-down approaches. mer impregnated GO composites have shown excellent improvement in
Common bottom-up methods reported for the synthesis of graphene adsorption capacity for most of the metal ions. This is attributed to the
include chemical vapour deposition, epitaxial growth while the top- complexation between the polymer functional groups and the metal
down methods used are mechanical and chemical (solution-assisted) ions. In addition, the polymer impregnated GO sheets have reduced
exfoliation of graphite. Top-down synthesis is considered most conve aggregation which results in enhanced adsorptive behaviour of the
nient for large-scale production of graphene [151]. composite.
Graphene as an adsorptive material is used in various forms like The following paragraphs discusses on the application of bare and
nanosheets, nanotubes, membranes, 3-D structures, hydrogels etc. functionalized graphene-based adsorbents for removal of heavy metal
Graphene-based materials used for adsorptive removal of pollutants can ions.
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Table 4
Summary of Lead removal by graphene based adsorbents.
Adsorbent Metal ion pH Adsorption capacity (mg/g) Specific surface area of adsorbent Reference
(m2/g)
5.2.1. Lead explored for removal of Pb(II). GO functionalized with inorganic metal
Lead is one of the commonly occurring pollutant and several studies ions have shown higher adsorptive removal of Pb(II) [161–163] while
have been reported on the adsorptive for the removal of lead by GO and magnetic GO composites conjugated with chitosan and cellulose
graphene-based materials. Adsorption studies of lead Pb(II) by GO, rGO have shown poor adsorption capacity [158,164–166]. Among the
and their composites are listed in the Table 4. Removal capacity of Pb(II) various organic molecule conjugated GO composites, poly(N-vinyl
by graphene materials ranged from as low as 20 mg/g for GO-cellulose carbazole)–GO has shown highest adsorption capacity of 983 mg/g
composite [158] to as high as 1119 mg/g with unmodified GO sheets [167], which was attributed to improved availability of GO oxygen
[159]. The optimum pH for removal of Pb(II) is 5-7. Graphene and GO groups. EDTA-GO, prepared via silylation process, enhanced the
sheets have shown excellent binding capacity to Pb(II). Sitko et al [159] adsorption capacity of GO from 328 mg/g to 525 mg/g because of in
have obtained significant removal of Pb(II) (1119 mg/g) with GO sheets. crease in surface functional groups [168]. Organic-inorganic hybrids of
They also observed the change in the GO dispersivity in water after GO have also been used for heavy metal removal. A typical example is
adsorption. GO complexed with metal ion showed tendency to use of nano-Fe3O4/triisopropanolamine (TI) functionalized graphene
agglomerate and precipitate, which is an essential step for removal of oxide composites for enhanced Pb(II) removal [169]. Maximum uptake
complexed adsorbent. Peng et al [160] have also reported high of 392.5 mg/g of Pb(II) was obtained at pH 5. The adsorption of Pb(II)
adsorption capacity of 766 mg/g for GO sheets. onto nano-Fe3O4/TI functionalized graphene oxide composites was
GO modified with inorganic and organic groups have also been through complexation between the nitrogen groups of TI and Pb(II)
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Fig. 6. Schematic representation of adsorption mechanism of Pb(II) ions on nano-Fe3O4/triisopropanolamine (TI) functionalized graphene oxide composites
(Graphical abstract reproduced with permission from Cao et al, [169])
Fig. 7. Possible adsorption mechanism for Pb(II) on LS-GO-PANI (Reproduced with permission from Yang et al, [170])
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Table 5
Summary of Copper removal by graphene based adsorbents.
Adsorbent Metal pH Adsorption capacity (mg/ Specific surface area of Reference
ion g) adsorbent
(m2/g)
coupled with electrostatic interactions between oxygen containing abundant amine and imine functional groups on PANI fibres form strong
functional groups of GO surface and Pb(II). The synthesis and adsorption metal conjugates with Pb(II), electronegative sulfonic groups of LS chain
mechanism are depicted in Fig. 6 where the formed nitrilotriacetic acid interact electrostatically with the Pb(II). LS chains also possess abundant
is also involved in Pb(II) complexation. carboxyl and phenolic groups which can result in formation of com
Thiol groups have also been considered for functionalization since plexes with Pb(II). Amino groups of PANI fibres may enhance the
they offer high binding sites. Pirveysian et al. [160] functionalized GO coordinative ability of carboxyl groups of GO nanosheets and sulfonic
using Na2S when various sulfur-derived groups such as SH, CS, SO, SO3− groups of LS chains for lead ions. This synergistic effect of the functional
were generated by one pot facile method. Sulfur -derived groups func groups thus contributes to the enhanced adsorption capability of the
tionalized GO (GO-SOxR) was further coated with TiO2 and SiO2 and tertiary composite. Possible adsorption mechanisms for Pb(II) on
were used as adsorbents for the removal of various metal ions (Zn(II), Cr LS-GO-PANI is represented in Fig. 7.
(III) or Cr(VI), Ni(II), Pb(II)). Thiol functionalized GO exhibited good Recently, Huang et al [171] have synthesized amino-functionalized
adsorption capacity for all the metal ions tested. Composites of thiol GO (GO-NH2) by grafting (3-aminopropyl) triethoxysilane on GO
functionalized GO with TiO2 (GO-SOxR-TiO2) and SiO2 (GO-SOxR-SiO2) sheets. The resultant composite with high surface area with numerous
showed enhanced adsorption capacity for all the metal ions. active sites was used as an adsorbent for effective removal of various
GO-SOxR-TiO2 (312 mg/g) composite showed increase in the adsorption metal ions like Pb(II), Cu(II), Cd(II) and Cr(II). Adsorption of the metal
of Pb(II) when compared to GO-SOxR (285 mg/g). In case of Ni(II) the ions onto GO-NH2 was shown to occur via chemical adsorption.
adsorption capacity almost doubled for GO-SOxR-TiO2 (344 mg/g) when
compared to GO-SOxR (175 mg/g). Similar enhancement was observed 5.2.2. Copper
with respect to adsorption of Cd(II) and Zn(II). Higher adsorption by Copper finds extensive applications in microelectronics and the use
GO-SOxR-TiO2 was attributed to the high surface area of the composite. of graphene-based materials for removal of copper ions and copper
Electrostatic interaction coupled with hydrogen bonding between the complexes from water has been attempted by various researchers
positive metal ions and the oxygen containing functional groups (hy (Table 5). GO sheets/membranes, magnetic GO sheets and amine
droxyl, carbonyl, sulphonyl/sulphonate, etc) on the surface of the functionalized GO are the commonly used graphene-based adsorbents
adsorbent were the contributing factors for the adsorptive removal of for the removal of Cu ions. Amongst these, composites of metallic GO are
metal ions. widely used because of ease of separation and reuse. Amino modified GO
Lignosulfonate-GO-polyaniline (LS-GO-PANI) ternary nano substrates (GO-NH2) are the other class of adsorbents researched for Cu
composites have shown excellent adsorption for Pb(II) (216.4 mg/g at ion removal. Amino groups on the layered GO sheets provide additional
pH 5) [170]. The adsorption process occurred due to the chemical sorption sites for the heavy metal ions due to their ability to form
interaction between the binding sites of the functionalized adsorbate complexes with those ions. The adsorption of metal ions on amino
and the adsorbent. Synergetic effect of the lignosulfonate and polyani functionalized GO substrates occurs by ion exchange, surface complex
line functional groups was evident by the enhanced order of uptake of Pb ation and electrostatic attraction. Under acidic pH conditions, depro
(II) by the binary and ternary composites compared to GO. While the tonation of the functional groups on the GO-NH2 surface is inhibited
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Fig. 8. Complexation and chelation interaction of Pb(II) and Cu(II) adsorption on MWCNT-PDA hybrid aerogel (Reproduced with permission from Zhan et al [205].
resulting in the repulsion between positive ammonium groups from magnetic GO (578 mg/g) [204]. Copper uptake of the magnetic GO
substrate and metal cations. Also, H3O+ in solution compete for the sheets (MGO) were found to be almost doubled when functionalized
adsorption sites leading to poor uptake of metal ions by the GO-NH2 with amino groups (319 mg/g for MGO to 578 mg/g for amino-MGO) in
surface. With increase in pH, protonation of amino groups is decreased, all pH conditions.
which results in availability of more NH2 groups on the surface, Amino-functionalized (via polydopamine) CNT partially reduced
increasing the uptake of the metal ions. Huang et al [171] used graphene oxide aerogels (prGO-MWCNT-PDA) for the uptake of Cu has
amino-functionalized graphene oxide (GO-NH2) for removal of several been reported by Zhan et al [205]. These hybrid aerogels have highly
metal ions. The uptake capacity for Cu(II) was found to be 26.25 mg/g. porous structure coupled with unique adsorption properties of CNTs and
The highest copper uptake has been reported for amino modified 3D architecture of graphene. Incorporation of CNTs not only improved
Table 6
Summary of Chromium removal by graphene based adsorbents
Adsorbent Metal ion pH Adsorption capacity (mg/ Specific surface area of Reference
g) adsorbent
(m2/g)
Graphene oxide-zinc oxide nanohybrid (ZnO-GO) Cr(VI) 8.02 3.69 32.95 [235]
RGO - β-cyclodextrin epichlorohydrin (RGO-βCD-ECH) composite Cr(VI) 1 1321.0 12.207 [236]
GO-NH2-AHMT (4-amino-3-hydrazino-5-mercapto-1,2,4-triazole) Cr(VI) 2 734.2 85.8 [237]
graphene oxide-dicationic (bisimidazolium) ionic liquid composite (GO- Cr(VI) 3 260.92 10.46 [238]
DIL)
Amino-functionalized graphene oxide Cr(VI) 7 280.11 — [171]
EDTA-GO composite Cr(VI) 3 36.59 100.93 [228]
Epoxy-GNP NC Cr(IV) - 85 47.63 [239]
GO/Chitosan Cr(VI) 2 86.17 – [240]
Amine modified GO-Chitosan composite Cr(VI) 2 219.5 11.69 [241]
Polypyrrole/GO Cr(III) 2 625 59.92 [233]
Graphene nanosheets Cr(VI) - 1.66 594.7 [242]
Exfoliated graphene oxide impregnated with Aliquat-336 Cr(IV) 2.5- 37.08 —- [226]
3.5
Poly(amidoamine) modified GO Cr(VI) – 4.15 — [195]
GO/Polyaniline Cr(VI) 2-3 1149.4 —- [230]
Magnetic cyclodextrin–chitosan/GO Cr(VI) 3 61.31 445.6 [243]
Graphene/MgAl-layered double hydroxide Cr(VI) 2 183.82 34.97 [234]
CTAB modified graphene Cr(VI) 2 21.57 —- [232]
Graphene/Fe@Fe2O3@Si\S\O Cr(VI) 7 1.03 42.1 [229]
Polypyrrole/GO Cr(VI) – 495 84.8 [244]
RGO–Fe(0)/Fe3O4 Cr(VI) 7 31.1 384.62 [194]
Graphene/Fe Cr(VI) 4.25 162 56 [227]
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Fig. 9. (A) Illustration of interaction between IL and EGO. (B) Illustration of interaction between EGO, IL and chromium(VI). (Reproduced with permission from
Kumar et al, [226]).
the mechanical strength and stability of the graphene sheet, but also the removal of chromium from a solution. The dominant forms of
prevented restacking of the graphene sheets. CNTs in the graphene chromium anions at various pH are Cr2O2− 7 at pH<2, HCrO4 in the pH
−
Fig. 10. Schematic adsorption mechanisms on graphene and MGNCs (Reproduced with permission from Zhu et al, [229]).
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Table 7
Summary of Arsenic removal by graphene based adsorbents.
Adsorbent Metal pH Adsorption capacity (mg/ Specific surface area of Reference
ion g) adsorbent
(m2/g)
Chitosan-magnetic GO grafted polyaniline doped with cobalt oxide (CSMGOP- As(V) 7 90.91 — [251]
Co3O4)
Carboxymethylcellulose incorporated Fe-Al layered double hydroxide - rGO (FAH- As(V) 7 258.39 156.24 [252]
rGO/CE)
Magnetic chitosan modified with Graphene oxide and Polyethyleneimine (MCS/GO- As 7 220.26 — [253]
PEI) (III)
Nitrile functionalized calix [4]arene grafted onto magnetic As 6 67.12 68.2 [254]
graphene oxide (N-Calix-MgO) (III)
Graphene oxide - Fe3+-modified clinoptilolite zeolite composite (GOFeZA) As(V) 7- 557.86 — [255]
8
Graphene oxide iron nanohybrid (GFeN) As 7 306 159.62 [256]
(III)
As(V) 431
Chitosan-graphene oxide-gadolinium oxide (CS-GO-Gd2O3) nanocomposite As(V) 6 252.12 61.28 [257]
Epoxy resin - Graphene nanoplates nanocomposite (Epoxy-GNP NC) As - 98 47.63 [239]
(III)
Graphene - Spinel CuFe2O4 composite As(V) 4 172.3 —- [246]
EDTA-Magnetic Chitosan/GO (EDTA-MCS/GO) As 7 42.8 81.36 [258]
(III)
Aminopyrazole-f-GO As 7.6 131.6 —- [259]
(III)
Fe3O4@SiO2/GO As 4 7.51 —- [260]
(III)
Fe3O4@SiO2/GO As(V) 4 11.46 —- [260]
Fe3O4–GO composite As 4 7.57 —- [245]
(III)
Fe3O4–GO composite As(V) 6 4.9 —- [245]
Fe3O4–RGO composite As 6 5.79 —- [245]
(III)
Fe3O4–RGO composite As(V) 7 4.23 —- [245]
RGO–Fe3O4/TiO2 As 7 99.5 275.23 [247]
(III)
RGO–Fe3O4/TiO2 As(V) 7 77.7 275.23 [247]
nZVI-RGO As 6.5 35.83 100.65 [261]
(III)
nZVI-RGO As(V) 4 29.04 100.65 [261]
GO-MnFe2O4 As 7 146 196 [162]
(III)
GO-MnFe2O4 As(V) 7 207 196 [162]
GO–FeOOH As(V) 7 73.42 117 [262]
GO–ZrO(OH)2 As 7 95.15 420.9 [263]
(III)
GO–ZrO(OH)2 As(V) 7 84.89 420.9 [263]
RGO–Fe(0) As 7 37.3 124.34 [194]
(III)
RGO–Fe3O4 As 7 21.2 140.70 [194]
(III)
RGO–Fe(0)/Fe3O4 As 7 44.4 384.62 [194]
(III)
Graphene/Mn2+ 3+ 2−
x Fe2-x O4 nanocomposite As 7 14.42 280 [264]
(III)
Fe3O4-RGO As 7 10.2 148 [265]
(III)
Fe3O4-RGO As(V) 7 13.1 117 [265]
GO/ferric hydroxide As(V) 6 23.78 — [266]
surface, thereby reducing the adsorption efficiency if Cr(VI). Cations like charged HCrO−4 anion and the adsorbent at acidic pH conditions [228].
Zn(II), Cd(II), Pb(II), Co(II) and Ni(II) did not interfere with the Dependence of chromium removal efficiency on temperature is also
adsorption of Cr(VI). However, Mn(II) and Fe(II) could interfere with the studied by several researchers. Adsorption of Cr(VI) in general is fav
adsorption of Cr(VI) by reducing it to Cr(III). oured by lower temperature indicating the exothermic nature of the
Optimal removal of chromium by iron nanoparticle decorated gra process. Contrary to this, Jabeen et al [227], using iron nanoparticle
phene was reported as pH 2-3 by Jabeen et al [227]. Recent studies by decorated graphene, have shown adsorption was favoured by high
amino-functionalized graphene have also shown similar pH related temperature. This was attributed to pore size enlargement and/or acti
interaction between chromium ions and the adsorbent [171]. Optimal vation of the adsorbent surface.
removal of hexavalent chromium was therefore obtained below pH 3. Zhu et al [229] have studied removal of chromium ions by magnetic
Similar behaviour is exhibited by EDTA-GO composite, which contains graphene nanocomposite (MGNC). Nanoparticles dispersed on the gra
oxygenic and amine groups, that can be protonated under acidic con phene sheet comprised of iron core, inner Fe2O3 shell, and the outmost
ditions resulting in maximum interaction between the negatively amorphous Si− S− O compound shell. They observed significant increase
14
R.H. Krishna et al. Applied Surface Science Advances 16 (2023) 100431
Table 8 and from a minimum of 4.23 mg/g [245] to maximum of 207 mg/g
Summary of Cadmium removal by graphene based adsorbents. [162] for As(V). Adsorptive removal of arsenic ions was found to be
Adsorbent Metal pH Adsorption Specific Reference maximum with metal oxide modified GO followed by organic molecule
ion capacity surface area modified GO. Inorganic composites of GO showed relatively lower
(mg/g) of adsorption of arsenic ions. Maximum arsenic removal of 207 mg/g has
adsorbent
been reported for GO-MnFe2O4 [162]. Recently, La et al [246] have used
(m2/g)
graphene-spinel CuFe2O4 and have shown excellent adsorptive capacity
Reduced graphene Cd(II) 4 1185.27 553.69 [173] of 172 mg/g for As(V). Chitosan GO nanocomposite functionalized by
oxide hydrogel
(rGOH)
EDTA exhibited moderate adsorptive capacity of 42.8 mg/g for As(III).
Tannin- reduced Cd(II) 4 395.80 122.2 [174] Apart from good adsorption capacity, an ideal adsorbent is one which
graphene oxide can be retrieved and reused several times with high capacity. Among the
aerogel (TRGA) various composites used for arsenic removal, we observe that magnetic
Graphene oxide Cd(II) 6-7 108.70 510.59 [270]
graphene composite materials have been extensively explored to obtain
aerogel (GOA)
FLMGO Cd(II) 8 401.14 224.10 [214] enhanced adsorption coupled with effective retrieval and regeneration
Amino- Cd(II) 7 10.04 — [171] of the adsorbent. Reduced GO supported core shell Fe- Fe2O3 exhibited
functionalized excellent magnetic properties and high binding capacity for As(III) and
graphene oxide Cr(VI) [229]. Few papers have reported use of magnetic Go and rGO
GO/Calcium Cd(II) 7 181 [271]
further modified with organic, inorganic and metallic materials. Babu et
—
alginate-PEI
rGO Cd(II) 4 433.2 — [268] al [247] have used rGO supported mesoporous Fe2O3/TiO2 with
rGO/Fe3O4 Cd(II) 4 292.8 — [268] adsorptive efficiency of 99.5 mg/g and 77.7 mg/g for As(III) and As(V)
rGO/Ag Cd(II) 4 372.8 — [268] respectively. It is noteworthy to mention that the adsorptive capacity of
rGO/ Fe3O4/Ag Cd(II) 4 386.7 [268]
—
most of the GO and rGO composites used for arsenic removal is higher
GO-SOxR Cd(II) - 217 102 [183]
GO-SOxR@SiO2 Cd(II) - 277 92 [183] than some of the conventional adsorbents like functionalized cellulose
GO-SOxR@TiO2 Cd(II) - 384 208 [183] (~75 mg/g) [248], nano-chitosan (~97 mg/g) [249], rice husk (~28
Aminopyrazole-f- Cd(II) 7.6 285.7 — [259] mg/g) [250].
GO
GO Cd(II) 6-7 23.9 [267]
5.2.5. Cadmium
—
Graphene Cd(II) < 72.39 625.8 [188]
nanosheets 6.5 Removal of cadmium, another toxic metal ion, using various gra
GO membrane Cd(II) 5.5 90.72 — [222] phene based materials has been reported by several researchers
GO Cd(II) 5 530 — [159] (Table 8). Compared to conventional adsorbents, GO and rGO based
RGO–Fe(0)/Fe3O4 Cd(II) 7 1.91 384.62 [194]
adsorbents have shown better adsorption of Cd(II) with adsorption ca
GO–TiO2 Cd(II) 5.6 72.8 132.74 [197]
FGO Cd(II) 6 106.3 — [203] pacity as high as 530 mg/g [159]. Majority of the adsorbents used for Cd
C8mim+PF−6 ionic Cd(II) 6.2 30.05 — (II) removal are GO and rGO composites with inorganic materials.
[202]
liquid Composites with magnetic Fe3O4 are extensively used because of ease of
functionalized separation and retrieval of the adsorbent.
graphene
The effect of oxygen containing functional groups on the surface of
(GNSC8P)
GO on adsorption of Cd(II) has been investigated by Bian et al [267].
FTIR and XPS studies confirmed the role of the phenolic hydroxyl and
in adsorption of chromium on MGNC compared to plain graphene. This carboxyl group on the surface of GO to be responsible for adsorption of
was attributed to the difference in the adsorption mechanism with Cd(II). The optimum pH for maximum adsorption was found to be 6-7,
respect to MGNC and graphene. While the adsorption is single layer type with electrostatic interactions leading to binding of Cd(II) with the
on graphene, adsorption on MGNC occurs by surface complexation be negatively charged surface groups of GO. Higher pH resulted in repul
tween Cr(VI) and sulphur on the outer shell of MGNC coupled with sion and reduced adsorption.
single layer adsorption on bare graphene (Fig. 10). The kinetics of Contrary to most of the reported work on enhanced adsorption ca
removal was very fast with complete removal of Cr(VI) achieved within pacity of graphene composites, functionalization by metal nanoparticles
5 min at a dose of 3 g/L. have also shown decreased adsorption capacity of GO nanosheets [268].
Highest adsorption capacity for hexavalent chromium ions has been Park et al. [268] synthesized rGO nanosheets conjugated by either silver
reported by Zhang et al [230] using polyanaline (PANI) nanorods or magnetic iron oxide (rGO/Fe3O4, rGO/Ag, rGO/Fe3O4/Ag) and
decorated GO nanosheets. The adsorbent was highly acid resistant with evaluated the adsorption capacity of the nano composites for removal of
maximum adsorption capacity of 1149.4 mg/g in the optimal pH range Cd(II). Adsorption capacity of the composites for Cd(II) was in the order
of 2-3. XPS studies indicated that chromium removal occurred by Cr(VI) rGO (433.2 mg/g) > rGO/ Fe3O4/Ag (386.7 mg/g) > rGO/Ag (372.8
adsorption coupled with reduction to Cr(III). TiO2-rGO composite was mg/g > rGO/Fe3O4 (292.7 mg/g). Although functionalization resulted
used for photocatalytic reduction of Cr(VI) [231]. The chemical reduc in decreased adsorption capacity, the adsorption capacity was higher
tion of Cr(VI) using EDTA-rGO composite and CTAB modified GO has than most of the other sorbents reported for Cd(II) removal.
been reported by [228,232]. Polymer-based and carbon-based magnetic The authors have reported extensive studies towards understanding
nanocomposites have also been explored [229,233]. Optimal pH for the mechanism of adsorption and the observed decrease in the adsorp
chromium removal with these nanocomposites was found to be pH 2-4. tion capacity of rGO composites. XPS studies indicated binding of Cd(II)
Yuan et al [195] have reported poly-amidoamine conjugated graphene was mediated by complexation with deprotonated sites on rGO and
for improved removal of Cr(III). Graphene@MgAl- double layered cation exchange of Na+/H3O+ by Cd(II). Competitive adsorption of
hybrid nanomaterial exhibited good adsorption capacity of 172.55 mg/g multi metal ion system was examined and the order of adsorption was
[234]. found to be Cu(II), Zn(II) > Ni(II) > Co(II) > Pb(II), Cd(II). Average
hydrodynamic diameters of the composites were examined and it was
5.2.4. Arsenic observed that the order of adsorption matched with the ionic radii of the
Adsorption of arsenic (As(III) and As(V)) by GO, rGO and their metal ions. Similar behavior was observed for GO sheets decorated with
composites is listed in Table 7. Adsorption of arsenic ranged from a Fe/Cu bimetallic nanoparticles [269] and it was attributed to the
minimum of 5.79 mg/g [245] to maximum of 146 mg/g [162] for As(III) decrease in the specific area and adsorption sites of inorganic material
15
R.H. Krishna et al. Applied Surface Science Advances 16 (2023) 100431
Table 9 (GO/2-PTSC) ligand exhibited high uptake capacity for Hg(II) ranging
Summary of Mercury removal by graphene based adsorbents. from 309 to 555 mg/g [273] under ultrasonic assisted conditions. Apart
Adsorbent Metal pH Adsorption Specific Reference from the surface oxygen groups of graphene, 2-PTSC, a
ion capacity surface tridentate-chelating ligand, also contributes to uptake of metal ion by
(mg/g) area of complexation and chelation mechanism. Sulphur and nitrogen atoms in
adsorbent
2-PTSC, having lower electronegativity than oxygen atoms, are actively
(m2/g)
involved in the complexation and chelation of Hg(II) via electron
rGO/PEI Hg(II) 4.5 219 227 [275] pair-sharing forming metal complexes. pH has a significant influence on
rGO Hg(II) 6.4 110.21 [276]
the removal of mercury ions by GO/2-PTSC. Under acidic pH conditions,
—-
GO-EDTA-CS Hg(II) 4.5 324 ± 3.30 1.326 [209]
poly- Hg(II) 5 174.7 — [277] protonation of 2-PTSC results in weak affinity to mercury ions. With
cyanoguanidine/ increase in pH to 4, more mercury ions are removed via complexation
graphene oxide and chelation. Additionally, ionization of the graphene surface func
composite (DCDA-
tional groups containing oxygen results in electrostatic adsorption of
GO
MCS/GO-PEI Hg(II) 9 124.84 — [253] mercury ions on the graphene adsorbent. At pH>5, mercury exist as
GO-NH2-AHMT Hg(II) 2 1091.1 85.8 [237] divalent ions resulting in surface complexation with heteroatoms. pH 5
Polyamine modified Hg(II) 5 63.8 63 ± 8 [274] was therefore found to be optimum for removal of Hg(II) by GO/2-PTSC.
rGO Polyamine functionalized rGO prepared by hydrothermal/chemical
Selenocarrageenan- Hg(II) 3 331 [278]
reduction for removal of Hg(II) from real systems (river and sea water)
—
GO hydrogel
Tourmaline/GO Hg(II) 5 294 — [279] has been attempted by Yap et al [274]. Mechanism of Hg(II) removal is
GO/Calcium Hg(II) 7 374 — [271] depicted in Fig. 11. Hg(II) uptake by the prepared polyamine/rGO
alginate-PEI adsorbent was >85% as against ~16% reported for commercial acti
dithiocarbamate Hg(II) 6 181.8 194.8 [280]
vated carbon. Zeta potential studies indicated positive charge on the
(DTC)-magnetic
rGO adsorbents up to pH 6 resulting in repulsion and poor removal of mer
Graphene-MoS2 Hg(II) - 719 - 1245 — [272] cury ions. At pH 5 drastic increase in adsorption was observed. The
hybrid aerogels optimum pH for mercury uptake was found to be 5. The adsorbent also
Aminopyrazole-f-GO Hg(II) 7.6 227.3 — [259] exhibited high selectivity towards Hg(II) (>70%) in multimetallic so
GO/2-PTSC Hg(II) 5 309 - 555 [273]
lution containing Hg(II), Pb(II), Co(II), Cd(II) and Cu(II). The Hg(II)
—
CoFe2O4-rGO Hg(II) 4.6 157.9 169.9 [190]
RGO–Fe(0)/Fe3O4 Hg(II) 7 22 384.62 [194] uptake efficiency of the adsorbent in real water system was ~74% for
Graphene/c-MWCNT Hg(II) 5 93.3 435 [199] river water and ~56.5% for sea water. The reduction in the uptake of
Polypyrrole–RGO Hg(II) 3 979.54 166 [281] mercury in sea water was attributed to the existence of mercury as
RGO–MnO2 Hg(II) 9.5 [282]
– —
chloro complexes (HgCl2− 4 and HgCl3 ) due to the presence of large
−
RGO–Ag Hg(II) – 9.53 — [282]
amount of chloride ions.
modified GO. Presence of functionalized group is not only required for 5.2.7. Other metals
good adsorption but also for effective separation of the adsorbent and The other metal ions remediated using graphene based materials are
hence is desirable even when it inhibits the adsorption capacity of the Co(II), Ni (II), Zn(II), Fe(III), Ag(I), Au(III), Mn(II), etc. Table 10 lists few
graphene material. For instance, the functionalisation of magnetic ox of the reported studies on removal of these metal ions by graphene based
ides helps in the magnetic separation and followed by the regeneration adsorbents.
of the adsorbents.
5.2.8. Radioactive metal ions
5.2.6. Mercury Ore mining, processing of spent nuclear fuels and other related ac
Various graphene based adsorbents have been used for removal of Hg tivities has resulted in release of various radioactive elements to the
(II) as listed in Table 9. Highest values for Hg(II) sorption ranging from environment necessitating the need for effective remediation of these
719 to1245 mg/g were reported or Graphene-MoS2 hybrid aerogels metal ions. Uranium exists commonly as U(VI) and is one of the widely
[272]. Graphene composites modified with organic compounds are the studied radioactive metal ion for remediation. Several graphene based
commonly used adsorbents for removal of Hg(II). Graphene oxide materials have been reported for removal of Uranium and other radio
modified chemically with 2-pyridinecarboxaldehyde thiosemicarbazone active metal ions (Table 11).
Fig. 11. Schematic mechanism of Hg(II) removal by Polyamine functionalized rGO (Graphical abstract reproduced with permission from Yap et al, [274]).
16
R.H. Krishna et al. Applied Surface Science Advances 16 (2023) 100431
17
R.H. Krishna et al. Applied Surface Science Advances 16 (2023) 100431
Table 11
Summary of radioactive metal ions removal by graphene-based adsorbents.
Adsorbent Metal pH Adsorption capacity Specific surface area of Reference
ion (mg/g) adsorbent
(m2/g)
Data availability
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