Chemical Engineering Research and Design 189 (2023) 530–571

Available online at [Link]

Chemical Engineering Research and Design

journal homepage: [Link]/locate/cherd

A comprehensive review of recent advances in

nanofiltration membranes for heavy metal
]]
]]]]]]
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removal from wastewater

⁎
Zahra Samavati a, , Alireza Samavati b, Pei Sean Goh a,
⁎
Ahmad Fauzi Ismail a, , Mohd Sohaimi Abdullah a
a
Advanced Membrane Technology Research Centre, Universiti Teknologi Malaysia (UTM), 81310 Johor Bahru,
Malaysia
b
Department of Physics, Faculty of Science, Universiti Teknologi Malaysia (UTM), 81310 Johor Bahru, Malaysia

a r t i c l e i n f o a b s t r a c t

Article history: Despite several technological advancements and achievements, wastewater treatment
Received 2 October 2022 continues to be a fundamental global issue. The wastewater, which contains heavy metal
Received in revised form ions, poses an acute threat to human health if not properly cleaned, making its disposal of
16 November 2022 paramount importance. Due to its adaptable design, efficient operation, and low cost, the
Accepted 25 November 2022 nanofiltration (NF) membrane is one of the most successful methods for removing heavy
Available online 1 December 2022 metals from wastewater. NF membranes made from innovative materials are gaining
popularity as a result of their many advantageous features, including their ability to treat
Keywords: wastewater in a variety of situations. To remove heavy metal ions from wastewater, the
Heavy metal removal modification of NF membrane using interfacial polymerization (IP) and grafting techni-
Nanofiltration ques, as well as its subsequent development via nanofiller addition, is the most effective
Interfacial polymerization way to tailor the properties of NF membranes. Many aspects of NF membrane modifica-
Grafting tion in terms of their preparation, characteristics, and performance have been introduced.
Nanofiller materials This review discusses the modification processes and performances of NF membranes for
Wastewater heavy metal remediation from wastewater. The findings elucidated the roles and benefits
of innovative membranes for the treatment of wastewater containing heavy metals. It has
been observed that high rejection is enabled by electrostatic charge induction, the

Abbreviations: NF, Nanofiltration; IP, Interfacial polymerization; MCL, Maximum contamination limit; MF, Microfiltration; UF,
Ultrafiltration; RO, Reverse osmosis; USEPA, The United states environmental protection agency; BIS, The Bureau of Indian standards;
BSI, The british standards institution; WHO, World health organization; PVC, Polyvinyl chloride; CA, cellulose acetate; PSU, Polysulfone;
PES, Polyethersulfones; PA, Polyamides; PVC, Chlorinated polyvinyl chloride; PVDF, Polyvinylidene fluoride; TFC, Thin film composite;
MPD, M-phenylenediamine; TMC, Trimethyl chloride; DOW, Dow chemical company; PIP, Piperazine; HBPs, Hyperbranched polymers;
3D, Three-dimensional; HPG, Hyperbranched polyglycerol; HPE, Hyperbranched polyester; GA, Glutaraldehyde; TPC, Terephthaloyl
chloride; BiOCl, Bismuth oxychloride; NMP, N-Methylpyrrolidone; EG, Ethylene glycol; KCl, Potassium chloride; PDA, polydopamine; GO,
Graphene oxide; SiO2, Silica; TiO2, Titanium dioxide; Ag NPs, Silver nanoparticles; ZnO, Zinc oxide; BaSO4, Barium sulfate; SrSO4,
Strontium sulfate; Ca3(PO42), Calcium phosphate; Fe(OH), ferrous hydroxide; Al(OH), Aluminium hydroxide; Ag, silver; Ca, Calcium; Mg,
Magnesium; Fe, Iron; Si, Silicon; Al, Aluminum; CaSO4.2 H2O, Calcium sulfate dihydrate; PEG, Polyethylene glycol; EDA,
Ethylenediamine; Cadmium, (II) ion (Cd2+); Mercuric, (II) ion (Hg2+); Lead, (II) ion (Pb2+); Nickel, (II) ion (Ni2+); Cupric, (II) ion (Cu2+);
Aluminum, (II) ion (Al2+); Cobalt, (II) Ion (Co2+); Zinc, (II) ion (Zn2+); Manganese, (II) ion (Mn2+); Chromium PAA, (VI) ion (Cr4+)Peroxyacetic
acid; [AMIm]PF6, 1-Allyl-3-methyl imidazolium hexafluorophosphate; B-Cur, Curcumin; PAMAM, Poly amidoamine; PA, Phytic acid; EB,
Electron beam; HPAMAM, Hyperbranched poly amidoamine; PTFE, Polytetrafluoroethylene; DA, Diels-Alder; DETA, Diethylenetriamine;
MPC, 2-methacryloyloxyethyl phosphorylcholine; AEMA, 2-aminoethyl methacrylate hydrochloride; PWP, Pure water permeability;
R3Al, Alkyl aluminium; DPC, Diphenylcarbazide; CMPI, 2-chloro-1-methyliodopyridine; OP, Operating pressure; IEP, Isoelectric point;
ISA, Skinned asymmetric; CVD, Chemical vapor deposition; SHSO, Superhydrophobic and super oleophilic; MW, Molecular weight; CNF,
Commercial NF; POE, Polyelectrolyte; ALD, Atomic layer deposition; PP, Polypropylene; MSiO2-NPs, Modified mesoporous silica nano-
particles
⁎
Corresponding authors.
E-mail addresses: szahra@[Link] (Z. Samavati), afauzi@[Link] (A. Fauzi Ismail).
[Link]
0263-8762/© 2022 Institution of Chemical Engineers. Published by Elsevier Ltd. All rights reserved.
 Chemical Engineering Research and Design 189 (2023) 530–571 531

creation of chelating complexes and the tuning of pore size while the high permeability
and antifouling properties can be achieved through the addition of hydrophilic nanofillers.
The economical and non-toxic application of polyhydroxy phenols compounds for en-
hancing the permeability and capture rate of heavy metal ions is also suggested for study.
Finally, the research gaps and uncertainties of these NF membranes in the treatment of
water contaminated with heavy metals are highlighted.
© 2022 Institution of Chemical Engineers. Published by Elsevier Ltd. All rights reserved.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 531
2. NF membrane overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 534
2.1. Historical development . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 534
2.2. Proposed rejection mechanism NF membrane. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 535
2.2.1. Modeling predictive of mass transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 535
2.2.2. Mechanisms rejection of heavy metal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536
3. Characteristics of NF membranes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 537
3.1. Surface charge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 537
3.2. Surface morphology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 537
3.3. Permeability and selectivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 538
3.4. Hydrophilicity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 539
4. NF membrane development . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 539
4.1. IP process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 540
4.1.1. Surface charge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 540
4.1.2. Pore size and structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 541
4.1.3. Polymer hybridization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 543
4.2. Nanofiller materials. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 545
4.2.1. Inorganic nanofillers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546
4.2.2. Organic nanofillers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
4.2.3. Organic/inorganic hybrids nanofillers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
4.2.4. Effects of nanoparticles aggregation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
4.3. Grafting process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
4.4. Physical grafting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
4.4.1. UV/photo-grafting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
4.4.2. Electron Beam (EB) irradiation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552
4.4.3. Plasma treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552
4.4.4. Microwave . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 553
4.5. Chemical grafting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 554
4.5.1. Free radicals initiators. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 554
4.5.2. Ionic initiators . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 555
5. Challenge and future perspective . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 558
6. Conclusion. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 559
Declaration of Competing Interest . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 559
Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 560
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 560

1. Introduction mainly contribute to water supply pollutants (Mashhadikhan

et al., 2022). Overexposure to these metal ions by humans
Heavy metal ions degrade and contaminate surface and and animals can result in serious diseases (Frazzoli et al.,
groundwater resources. The complete removal of these ions 2022). According to different health organization agencies,
from water supplies through modern treatment processes is there is a maximum contamination limit (MCL) of heavy
crucial to suppress the harmful effects of these ions on metal ions in drinking water (see Table 1) (Eaves et al., 2022;
human health (Imdad and Dohare, 2022). Heavy metals are Awang et al., 2022). Furthermore, drinking water con-
defined as elements with an atomic weight ranging from 63.5 taminated with heavy metal ions above the MCL value can be
to 200.6 amu and a specific gravity greater than 5.0 harmful to the kidneys, liver, skin, heart, stomach, nervous,
(Eskandari et al., 2020). Lead, and cadmium are two heavy and reproductive systems (Famurewa et al., 2022). Moreover,
metal pollutants that are often found in industrial waste- as listed in Table 1, they may create serious medical condi-
water (Razzak et al., 2022). The productions of vehicle bat- tions like high blood pressure, cardiovascular effects, da-
teries, paints, fertilizers, pigments, and other similar goods mage to the immune system, psychological disorders, and
are among the current manufacturing processes which diarrhea, etc. The traditional methods for treating water
 532

Table 1 – MCL of heavy metal ions in drinking water reported by different health organization agencies, their common sources, and possible disease effects on the human body
due to heavy metal contamination in water.
Metals USEPA BIS BSI WHO Common Sources Negative impact above the acceptable limit
(mg/l) (mg/l) (mg/l) (mg/l)

Pb 0.015 0.01 0.01 0.05 Recycled PVC, paints, and PVC pipes in sanitation, batteries, agriculture, Decreased kidney function, increased blood pressure,
jewelry, and lunch boxes. cardiovascular effects, and reproductive problems
As 0.01 0.01 0.05 0.05 Pesticides, oxidation of pyrite (FeS) and arsenic pyrite (FeAsS), Arsenic- Disorders of the skin, blood, liver, and kidneys
based preservatives on wooden utility poles, fertilizers, and dumping
untreated effluents
Cd 0.005 0.003 0.003 0.005 Photoconductors and photovoltaic cells, pigments, photographic and Damage to the immune system, psychological disorders,
engraving process, electroplated parts, batteries, plastics, synthetic rubber, and diarrhea
and paints
Hg 0.002 0.006 0.001 0.001 Municipal solid waste incineration, combustion of coal, and volcanic Damage to the nervous system, kidneys, and
emissions gastrointestinal tract
Ni NM 0.07 0.02 0.1 Volcanic activity, forest fires, resulting from the weathering of rocks, Birth effects, respiratory failure, heart disorders, and lung
insoluble particles, and wind-blown dust cancer
Cr 0.1 0.05 0.05 0.05 Tanning, chrome plating industries, and leather industry Liver and kidney damage, stomach ulcers, respiratory
problems, and skin rashes
Cu 1.3 2 1.5 1.5 Photovoltaic cells, tanning, and fertilizers Anemia and liver damage
Fe 0.3 NM 0.3 0.3 Waste incinerators, metal factories, and power plants. fertilizers and Stomach problems, nausea, damage to the heart, pancreas,
agriculture runoff. and liver.
Mn 0.05 NM 0.3 0.08 Weathering of rock and soil, landfill leaching, mining, and industrial Problems with motor skills, attention, and memory.
discharges
Chemical Engineering Research and Design 189 (2023) 530–571

Zn 5 NM 15 5 Cosmetics, pigments, and soldering Vomiting, nausea, diarrhea, dizziness, and fevers
Al 0.05–0.2 NM 0.2 0.05 Rock and soil Arthritic pain, skin rashes, diarrhea, vomiting, mouth
ulcers, and skin ulcers
 Chemical Engineering Research and Design 189 (2023) 530–571 533

Table 2 – Utilizing CNF for heavy metals filtration.

Membrane Removal Ref.
(producer) efficiency %

NF 90 Ni2+: 99.2 (Basaran

(Filmtec/DOW) Cr6+: 96.5 et al., 2016)
NF 270 Cu2+: 100 (Al-Rashdi
(Filmtec/DOW) Pb2+: 60 et al., 2013)
Desal HL (Desal/ UO2(CO3)22-: ∼ 93 (Raff and
GE/Suez) UO2(CO3)34-: ∼ 95 Wilken, 1999)
Desal 5DK (Desal/ Co2+: 95 (Ferreira Esmi
GE/Suez) Ni2+: > 95 et al., 2013)
Fig. 1 – Pressure-driven membrane processes for water Zn2+: 80–90 (Fersi Bennani and
treatment technologies, display the particles caught by each M’hiri, 2015)
procedure as well as the pore diameters of the membranes Desal DL (Desal/ Cu2+: > 98 (López et al., 2019)
utilized. GE/Suez) Zn2+: > 98
TFC SR2 (Koch UO2(CO3)22-: 90 (Schulte-Herbrüggen
membrane) et al., 2016)
resources contaminated with heavy metal ions are chemical MPS 34 (Koch Cr+3: 97 (Piedra et al., 2015)
precipitation, ion exchange, flotation, and electrochemical membrane)
treatment (Saleh et al., 2021; Gul and Nasreen, 2018; Altaf AFC 30 (PCI Pb2+: 84 (Bouranene
et al., 2021). However, each of these approaches has its own Membrane) et al., 2008)
RO 9100340361 Zn2+: 94.9 (Torma and
set of restrictions. For example, in the chemical precipitation
(Zenon) Cséfalvay, 2018)
approach, a huge amount of sludge and hazardous fumes are
UTC 60 (Toray) Co2+: 90.5 (Meschke
formed and this technique is only suitable for removing the Cu2+: 91.3 et al., 2018)
high concentration of heavy metals (Tahir et al., 2019; Zn2+: 96.7
Benassi et al., 2019). The drawback of removing heavy metals
ion with the ion-exchange process is high resin cost, low
efficacy (60–90%), and difficulties with spent resin regenera- rejection of divalent ions, higher flux, lower operating pres-
tion (Nazaripour et al., 2021; Nekouei et al., 2019). sure, and reduced energy usage. These characteristics in-
Currently, the water purification process via membrane- dicate NF as a promising and new technology that may be
based technology is the most capable and scalable method extensively employed to remove colors, heavy metals, sus-
for eliminating heavy metal ions from polluted water (Xiang pended particles, raw materials, oil and grease, and other
et al., 2022). Common membrane materials include ceramic, auxiliary chemicals from drinking water and industrial ef-
polymeric, stainless steel, and hybrid substances (Guerra and fluents (Fang et al., 2022; Han et al., 2018). The separation
Pellegrino, 2013). Due to their excellent selectivity rates and performances in terms of selectivity and permeability as well
relative ease of operation and surface feature change, poly- as the mechanical and chemical stability of NF membranes
meric membranes are the most preferred (Adeola and have been improved by altering their structure, composition,
Nomngongo, 2022). This review focuses on polymeric mem- and morphology. As a result of its high-water permeability
branes as the foundation of NF membranes for heavy metal and heavy metals removal rate, as well as its relatively strong
rejection. Fig. 1 schematically illustrates various forms of chemical and mechanical stabilities, thin film composite
membrane filtration, and their selective permeability to se- (TFC) membrane has been commercially used for industrial
parate certain substances in wastewater. Microfiltration (MF), membrane processes (Lee et al., 2022; Castro-Muñoz et al.,
ultrafiltration (UF), nanofiltration (NF), and reverse osmosis 2021; Ma et al., 2022a).
(RO) are four classifications of these membranes. Among all The currently marketed NF membranes, such as the NF 90
membrane-based techniques, RO and NF are the well-es- (Filmtec/DOW), NF 270 (Filmtec/DOW), Desal HL (Desal/GE/
tablished technologies for water purification and desalina- Suez), TFC SR2 (Koch membrane), MPS 34 (Koch membrane),
tion (Niu et al., 2022; Monachan et al., 2022; Han et al., 2017). and UTC 60 (Toray), are typically created from TFC methods
Like ultrafiltration and reverse osmosis, NF is a separation using the time-consuming and complex IP process (Shao
technique involves the use of the hydrostatic pressure to et al., 2022; Shin et al., 2020; Gholami et al., 2020; Jun et al.,
allow the transportation of molecules across the semi- 2018). Table 2 summarises the uses of commercially available
permeable membranes. Some low molecular weight (MW) NF (CNF) membranes for the elimination of heavy metals.
solutes and the solvent pass through the membrane, TFC NF membranes provide strong rejections to heavy me-
whereas larger molecules are trapped. The molecular weight tals and inorganic salts but have a limited permeability to
of the components that are retained by the membrane, and water. In order to produce an adequate flow, a high working
hence the membrane's pore size, determine the major dis- pressure is required, which enhances energy usage. Ad-
tinction between NF and UF. The molecular weight threshold ditionally, they are unable to separate and extract priceless
for NF membranes is around 400–500 Da, with pore diameters inorganic salts and heavy metals in real wastewater (Kanwal
ranging from 0.5 to 2 nm. Moreover, necessitates working et al., 2023; Magalhães et al., 2020; Abdullah et al., 2019;
pressures in the 10–50 bar range. As a result, NF membranes Mastropietro et al., 2021). Moreover, the accretion of in-
have the ability to retain neutral species with MW 200–300 g/ organic salts in the wastewater would weaken the heavy
mol and to reject inorganic ions via a combination of size metals rejection and produce more severe fouling in addition
exclusion and electrostatic interactions between the ions to resulting in a poor permeation flow due to the increased
and the charged membrane (Cao et al., 2022; Hu et al., 2021a). osmotic pressure (Khan et al., 2021a; Katibi et al., 2021; Chu
In comparison to other membrane technologies, such as RO, et al., 2020). Therefore, modifying the NF membrane can
NF provides a number of benefits, including stronger contribute to energy savings, high efficiency in the removal
534 Chemical Engineering Research and Design 189 (2023) 530–571

Fig. 2 – NF's contents are investigated in this review.

of heavy metals, and increased resistance of membranes below acceptable limits. The NF membranes for heavy me-
towards fouling and scaling. The incorporation of nanofillers tals separation are the focus of this review. The content and
in the design of these membranes improves their structural arrangement of the topics for this review are summarised
strength and chemical resistance, increases their durability, in Fig. 2.
allows for greater tolerance of impurities, and makes
cleaning the membranes much easier (Bano et al., 2015; Lari 2. NF membrane overview
et al., 2022; Wu et al., 2022a).
The selective separation of heavy metal ion contaminants 2.1. Historical development
may be significantly reduced by undesirable defects between
polymer matrix and fillers, agglomeration of nanomaterials, Depending on the application, NF was initially created as a
even though nanomaterials, especially inorganic fillers, poor spin-off of RO and UF therefore, it was referred to as open
dispersion of nanomaterials into the membrane structure or RO or tight UF. The invention of the Loeb–Sourirajan (L–S)
on the membrane surface, and create outstanding permea- anisotropic or asymmetric cellulose acetate (CA) mem-
tion pathways with active sites to adsorb pollutants (Yu branes for seawater desalination in the late 1950 s was the
et al., 2021; Damiri et al., 2022). Numerous attempts have backbone of the NF membranes development and most of
been undertaken to enhance adhesion between organic and the pressure-driven membranes in the early 1960 s (Singh,
inorganic phases and permit uniform dispersion of nano- 2014). These membranes laid the groundwork for the crea-
materials in the polymer matrix (Liu et al., 2022a; Imtiaz tion of current membranes in the RO and UF sectors. A few
et al., 2022; Ali et al., 2022; Liu et al., 2022b; Yaqoob et al., years later, an asymmetric UF was technologically sup-
2023). Incorporating a nanomaterial with a high potential for ported via RO composites having a submicron coating on a
trapping heavy metal ions in water resources presents sig- selective layer (Michaels, 1990). The progress of RO and UF
nificant hurdles. In addition, the concept of NF membrane technology has resulted in the emergence of a new dis-
modification and membrane adsorption to effectively re- cipline known as NF. Starting in 1960, this research and
move trace amounts of pollutants, such as cationic heavy development endeavor lasted only roughly 15 years. By the
metals, needs additional research and evaluation. In this early 1970 s, a range of CA asymmetric (or anisotropic)
field, several critical reviews have been made to discuss the membranes covering the complete spectrum, from RO
various approaches used to overcome these difficulties. The through NF to UF, were also available (Linder and Kedem,
goal of this article is to offer an in-depth analysis of the de- 2021). When trying to enhance the economics of water
velopment of NF membranes based on nanotechnology. Its treatment and other industrial purposes, the drawbacks of
focus is on describing the most cutting-edge methods for CA as a membrane material became instantly clear (Liu
creating and modifying NF membranes. Additionally, dif- et al., 2021a). These limitations hampered attempts to in-
ferent methods for preparing organic and inorganic nano- troduce NF into other industries and constrained the
materials that are incorporated into membranes and their number of applications that could be used. One attempt to
functionalization on membranes are explored. These address this issue was the creation of integrally skinned
methods are essential knowledge for creating highly effec- asymmetric (ISA) membranes using materials other than
tive devices. In addition, the design of membrane archi- CA, such as polysulfone (PSU), polyethersulfones (PES),
tectures is discussed to preserve the high capacity of the polyamides (PA), chlorinated polyvinyl chloride (PVC), and
membrane to adsorb contaminants and keep the water flux polyvinylidene fluoride (PVDF) (Zhu et al., 2020). Although
 Chemical Engineering Research and Design 189 (2023) 530–571 535

Fig. 3 – The historical evolution of NF membrane mechanisms during the last few decades (Linder and Kedem, 2021; Lau
et al., 2015; Lu and Elimelech, 2021; Wang and Lin, 2021).

this approach could be used to produce open NF mem- 2.2. Proposed rejection mechanism NF membrane
branes, it was not able to achieve the selectivity/flux com-
bination needed for many applications (Alenazi et al., 2017; 2.2.1. Modeling predictive of mass transport
Qian et al., 2021). A significant development in NF was the Over the last two decades, research on the ability to forecast
identification of noncellulosic composites based on the IP of membrane performance has grown. Due to the extended
UF supports with a submicron selective barrier. Composite Nernst-Planck equation's capacity to offer information re-
membranes were created for the first time in the 1970 s, but levant to features of both the membrane and the process
they were not widely accessible until the latter half of the stream, it has supplanted empirical black box models based on
1980 s (Shen et al., 2022a). The creation of NF ceramic and irreversible thermodynamics as the preferred method
inorganic membranes was another option that came later throughout this time period (Levenstein et al., 1996; Tsuru
(Goh and Ismail, 2018). et al., 1991). The primary goal of such models is to realistically
The majority of NF membranes are composed of three represent the membrane process to improve the fit between
TFC layers. The support layer, which is the top layer, offers observable variables and controllable model parameters. It is
minimal resistance to mass transportation. The second important to keep in mind that the fundamental restriction of
layer serves as a MF or UF membrane in support of the first NF modeling is the need for distinctive model parameters,
layer. The support layer's third active layer controls the such as membrane charge and pore radius, that are not easily
charge, hydrophilicity, and other surface features of the measurable at the near-atomic length scales encountered. Any
membrane. Having a hydrophilic surface is essential be- macroscopic continuous explanation of ion transport and
cause it prevents membrane fouling. Polyvinyl alcohol (PVA) partitioning would likely face a difficult test as a result of the
and regenerated cellulose are two of the most popular hy- exceedingly complicated nano-scale processes involved in
drophilic materials used to make NF membranes in the neutral solute and charged electrolyte separations via NF
2000 s (Bandehali et al., 2021). Since it allows for the selec- membranes. The lack of precise information on the physical
tion of the most appropriate polymers for a given purpose, structure and electrical characteristics of actual NF mem-
using other synthetic polymers for the construction of NF branes and process streams has further hindered the creation
membranes garnered a lot of interest in the 2010 s (Oatley- of rigorous physical descriptions such as molecular dynamics
Radcliffe et al., 2017). However, there are drawbacks to simulations. Thus, the advancements in modeling have pro-
membrane technology, including a high initial investment ceeded in tandem with the enhancements in measuring
cost and membrane fouling. Further treatment procedures methods used for the characterization of NF membranes and
are required because some pollutants, such as heavy metals process streams, since only then will the suitability of model
or the precipitation of insoluble salts, may still be present in parameters be able to be checked.
the retentate (Qasem et al., 2021). As a result, numerous Schlogl (Schlögl, 1966) suggested the application of ex-
methods like UV radiation, plasma and chemical treatment, tended Nernst-Planck equation to describe the transport of
grafting, additive blending, adsorbed coatings, and cross- electrolytes in RO via ion-exchange membranes, and this
linking are frequently used to modify the NF membrane model is now widely accepted as the best available option.
surface. For instance, to increase the hydrophilicity of PA The equation is especially helpful for NF since it takes into
surfaces, cross-linking with hydroxyl compounds is used. account transport pathways and uses actual, quantifiable
Additionally, cross-linking boosts membrane stability and membrane characteristics to determine the necessary
lowers molecular cut-off (Farahbakhsh et al., 2021). The changeable fitting parameters.
positively charged NF membrane for heavy metal removal
ci ki, d Di, dµ
created by the IP approach has drawn a lot of interest re- ji = + ki, c ci V
cently. Numerous studies have found that adding nano- RT dx (1)

particles, creating interlayers and surfactants can improve

where Ki,c and Ki,d are hindrance factors to allow for con-
the permeation flux of NF membranes (Fallahnejad et al.,
vection and diffusion within a restricted region, ji is the ionic
2022). Fig. 3 provides a review of their historical evolution.
flux, c is the concentration, V is the solvent velocity, and
NF-based procedures have matured and the technology's
these variables all interact to create the system. This equa-
efficacy has risen over the past few decades as a result of
tion may be adjusted to get the complete extended
developments in NF membranes and process optimization.
Nernst–Planck equation.
536 Chemical Engineering Research and Design 189 (2023) 530–571

dci ci Di, p d i ci Di, p dp ci Di, p d (PTM), incorporates charge fluctuation through adsorption
ji = DI, P Vsi zi F + Ki, c ci V
dx i dx RT dx RT dx isotherms, the values of which were calculated in advance
(2) using measurements of the tangential streaming potential.
This model is similar to the more rigorous (and complicated)
Eq. (2) controls the movement of an ion in solution and
Space Charge Model (SCM) first presented by Gross and Os-
represents the whole extended Nernst-Planck equation. To
terle (Gross and Osterle, 1968), which accounts for a radial
explain how an ion moves through a membrane pore-like
distribution of concentration and electric potential inside the
that in NF and loose RO membranes, a new equation has
nanopores. Instead of being in the radial direction, the
been developed. Solute concentrations on the feed side (ci(0))
charge fluctuation in this instance is in the axial direction.
and permeate side (ci(Δx)) of the membrane must be de-
The authors concluded that Freundlich adsorption isotherms
termined to solve the transport equation. The equilibrium
were a viable way to determine the charge densities within
relationship between an ion's entry and departure from such
the pores and that the membrane charge evolution with
a pore is as follows:
concentration could be properly determined using streaming
i ci zi F W potential measurements. To measure the tangential
0
= i exp D exp
RT kB T streaming potential over the membrane's surface, as pre-
i Ci (3)
viously mentioned, charge densities within a nanopore have
The first two terms on the right-hand side of Eq. (3) are the very little physical importance, and ion adsorption inside a
standard, widely recognized formulas for steric and Donnan nanopore is simply impossible to quantify. Due to these
effects, respectively (Donnan, 1995). Separation due to di- factors, the methods used would have to be questioned if
electric exclusion is represented by the third component on there was no trustworthy measurement or other means of
the right-hand side of Eq. (3). The recent study summarises verifying the charge density within the nanopore.
the discussions that have taken place over the nature of this The transport of an unlimited number of ions and dis-
impact (Zhang et al., 2020a; Du et al., 2022). solved substances through the NF membrane may be mod-
There are other variants on this fundamental modeling eled using an extension of the Nernst-Planck equation. But,
topic, but they all have roots in the Nernst-Planck equation almost all modeling efforts up to this point have focused on
and differ mostly in how they solve it, the degree to which very dilute and idealized solutions, generally consisting of
they simplify it, or the number of factors they include. For just 2, 3, or even 4 ions at most. More work has to be put into
instance, Bowen et al (Bowen et al., 1997). initially suggested modeling systems of actual industrial consequence if accu-
the Donnan-Steric-Pore-Model (DSPM), from which the rate modeling of concentrated multi-component electrolyte
aforementioned model was derived. By taking into account a solutions realistic of industrial processes is to become com-
Hagen-Poiseuille flow pattern through the nanopore, the NF monplace. With regards to highly concentrated multi-com-
model given here is more rigorously derived from the ex- ponent separations of industrial consequence, Oatley-
tended Nernst-Planck equation. By including the Born model Radcliffe et al (Oatley-Radcliffe et al., 2014). have examined
in the equilibrium partitioning formula Eq. (3), the model also and analyzed the existing modeling methodologies. As this
accounts for the phenomenon of dielectric exclusion by ion research showed, there is now a lack of understanding of the
solvation. Vezzani and Bandini were the first to include the physical characteristics and physicochemical processes
simplest explanation of dielectric exclusion by image forces within nanopores, and it also showed that there are some
phenomena (for slit-like pores) into NF models (Vezzani and major gaps in the academic approach to modeling these
Bandini, 2002). The DSPM & DE model was simply an ex- complicated separations. Particularly, there is a paucity of
pansion of the original DSPM by including a description of knowledge about activity coefficients, the ordering of finite
dielectric exclusion by image forces obtained from the ideas water layers at the solid-liquid interface, and basic physical
of Yaroshchuk (Yaroshchuk, 2000). Szymczyk and Fievet features. Determining the intricate interconnections and
(Szymczyk and Fievet, 2005) made further updates to this physical phenomena in such systems, such as membrane
model to create the Steric Electric and Dielectric (SEDE) charge and particle-particle-membrane interactions, re-
model. This included not only the mathematically intensive quires the development of new methodologies for NF models
explanation of image forces for cylindrical pores but also ion to be effective in the accurate ab initio prediction of NF
solvation through the Born term. When Saliha et al (Saliha process performance.
et al., 2009). examined the SEDE model's capacity to explain
the separation of multi-ionic solutions (3 and 4 ions) by NF, 2.2.2. Mechanisms rejection of heavy metal
they found that the model could not adequately reflect the Depending on the type of membrane and the impurities, NF
experimental solute rejections when the two dielectric ex- membranes can be utilized in various ways to treat waste-
clusion mechanisms were included. But when just one di- water contaminated with heavy metal ions. Physical sieving
electric process, either ion solvation or image forces, was separation of colloids and large molecules. Nevertheless,
included, the model performed well. This finding indicates electrostatic repulsion and diffusion by surface charges are
that just one of the dielectric processes is most likely visible the principal mechanisms for the rejection of pollutants with
in NF membranes, but that both models provide computed low molecular weight. The following are typical rejection
values for the phenomenon that is of the same order of mechanisms for NF membranes:
magnitude. Therefore, regardless of whether the mechanism
is essentially more suitable, any model might be used to re- i. Surface wetting through the creation of hydrogen bonds
present dielectric exclusion. between the membrane and water molecules enhances
By assuming that the membrane charge density varies the passage of water and the entrapment of pollutants
throughout the pore's length, Deon et al (Déon et al., 2011). through the membrane (Nawaz et al., 2021).
explored a new way to simulate the charge density of ii. Electrostatic repulsion or adsorption of pollutants via
membranes. This model, dubbed the Pore Transport Model membranes with micro-porosity and heterogeneous
 Chemical Engineering Research and Design 189 (2023) 530–571 537

properties as predicted by the Donnan equilibrium model excess of counterions in the surrounding solution is neu-
(Xu et al., 2006). tralized. In neutral or alkaline settings, NF membranes are
iii. Dissolving the solute and solvents in a selected layer of normally negatively charged, while in extremely acidic si-
homogeneous and dense NF membrane, followed by tuations, positively charged. The NF membrane's surface
diffusion transfer across the membrane (Cheng charge is useful for the selective interception of multivalent
et al., 2014). ions. Since the polymer backbone (which typically contains
iv. Identifying the transportation by partitioning between carboxylic acid and sulfonic acid) has a set negative charge,
bulk and pore fluids in a dense membrane that is punc- CNF membranes tend to be negatively charged (Nafi and
tured by pores (Suhalim et al., 2022). Taseidifar, 2022; Jeon et al., 2008; Tanninen et al., 2004).
v. Presenting metal-complexing ligand on the surface of the Due to the Donnan effect and steric hindrance, negatively
NF membrane to collect the pollutant and improve se- charged NF membranes exhibit better retention for divalent/
paration performance (Mokhter et al., 2017). multivalent anions with the same charge as the membrane
vi. Modifying the membrane's surface by incorporating a surface (Azizi et al., 2022). Heavy metal cation retention is
nanostructured TFC to absorb heavy metals (Salehi poor in CNF membranes. For instance, the typical rejection
et al., 2022). rates for PbCl2, MnCl2, CuCl2, and CdCl2, for the Dow NF270
membrane were reported to be 12, 60, 68, and 90%, respec-
Typically, membranes with small contact angles are uti- tively (pressure: 4 bar; pH: 5, 1000 ppm) (Al-Rashdi et al.,
lized to treat wastewater. The metal oxides are introduced 2013). When the pH of the feed solution is lower than the IEP
into the membrane to reduce the contact angle and raise the of the membrane, heavier metal cation rejection is possible.
surface charge (Lu et al., 2022). Normally, these metal oxides A greater charge density improves selectivity, and an NF
consist of titania, zirconia, and other transition metal oxides. membrane with a positively charged surface can retain more
These hydrophilic substances can also regulate and fix the divalent/multivalent cations due to electrostatic repulsion
course of coagulant water during phase inversion (Da et al., (Wang et al., 2022a).
2016). Additionally, gold can be incorporated into the mem- Currently, three key methods for creating positively
brane to render its surface non-reactive (Zhou et al., 2022). charged NF membranes have been developed: IP, phase in-
The rejection of solutes by NF membranes is influenced by version, and surface modification (such as surface deposi-
various aspects. In accordance with the solution-diffusion tion, surface grafting, and surface cross-linking) (Yadav et al.,
process, solute rejection decreases at a fixed flow as solute 2022). Creating positively charged composite membranes
concentration or temperature rises due to an increase in the through IP and surface modification often requires the use of
diffusion coefficient. Increasing the operating pressure (OP) harmful or carcinogenic chemicals and many preparation
increases the water flux, whereas increasing the feed solute stages (Noremylia et al., 2022). An alternative is integrally ISA
concentration increases the solute flux (Shefer et al., 2022). In membranes, which can be created utilizing a straightforward
addition, the pH of the feed solution affects both the surface cross-linking approach and a simpler phase inversion
charge and solute charge of the membrane (Hailemariam methodology (Asadi Tashvigh et al., 2019). By adding qua-
et al., 2022). The membrane's surface-active sites are de- ternary amine or nitrogen groups to the membrane's surface
protonated and induce a negative charge density at neutral and interior pores, it is possible to positively charge the ISA
pH. Therefore, the greater rejection of metal ions at neutral membrane (Nozad et al., 2022). It is generally known that a
pH compared to acidic pH can be attributed not only to the base, such as an amine or a hydroxide (KOH, NaOH), can be
presence of attraction electrostatic interactions between the used to open an imide ring (Hajipour and Rafiee, 2009). The
metal cations and negatively charged functional groups on imide ring is first hydrolyzed into a carbonyl group during
the membrane surface but also to the formation of heavy this amination chemistry, and then it combines with the
metal ions complexes with the existing functional groups in modifier's nucleophilic amino group to generate one amide
the interlayer of the membrane structure. group. The membrane has a hydrophilic surface and a posi-
tive charge due to the unreacted free amines of the modifiers.
3. Characteristics of NF membranes While this is going on, the backbone chains of imide-based
polymers can be cross-linked by di- or multivalent amines,
3.1. Surface charge forming a dense active layer and boosting mechanical
strength and chemical resistance. Polymers with imide
The origin of a membrane charge is linked to the fact that groups, such as polyimide, poly(ether-imide), and poly-
membranes can pick up an electric charge in several dif- amide-imide have been utilized in the production of posi-
ferent ways when they come into contact with an aqueous tively charged NF membranes (Ma et al., 2021).
electrolyte solution. A few examples of potential mechan-
isms include the separation of functional groups, the ad-
sorption of polyelectrolytes, the adsorption of ions from 3.2. Surface morphology
solutions, charged macromolecules on surfaces and ionic
surfactants, and so on (Zhang et al., 2020a; DuChanois et al., Membrane fouling and anti-fouling performance are greatly
2019; Teixeira et al., 2005; Dickhout et al., 2019). Depending influenced by the membrane's surface coating and mor-
on the situation, this charging mechanism may take place on phology during heavy metal removal (Pakizeh et al., 2020).
the internal pore surface of the membrane as well as the Fig. 4 illustrates the roughness, waviness, lay, and flows of a
external membrane surface. Because the system must surface topographic pattern, which is repetitive or random
maintain electroneutrality, which affects the distribution of departures from the normal surface (American Society of
ions, surface charges have an impact on how ions are dis- Mechanical Engineers, 2003). Manufacturing processes, vi-
tributed in a solution. Due to the formation of an electrical brations, stresses, work deflections, and the interior struc-
double layer, as a result, the surface becomes charged and an ture of the material may all contribute to the imperfections.
538 Chemical Engineering Research and Design 189 (2023) 530–571

cycles allows for exact atomic-scale adjustment of the thin

film's thickness while it is being deposited (Yasmeen et al.,
2022; Adhikari et al., 2018). Surface hydrophilicity was in-
troduced to the hydrophobic polypropylene (PP) membranes
by Hyde et al (Hyde et al., 2010). and Waldman et al
(Waldman et al., 2018). via ALD of alumina. The TFC-PA
membranes fabricated by Nikkola et al (Nikkola et al., 2014).
were treated with a similar method to improve their hydro-
philicity and, by extension, their anti-fouling ability. Fur-
thermore, low-temperature plasma discharges provide
homogenous surface treatments that are controllable and
flexible, leading to minimizing damage and a wide variety of
conceivable surface functionality (Ataeefard et al., 2008). By
Fig. 4 – A material's typical top surface displays wavy adjusting the plasma's intensity and exposure time, surface
topography and roughness qualities may be fine-tuned to meet a variety of needs (Kim
Adopted from (American Society of Mechanical et al., 2011), as detailed in the subsequent sections of this
Engineers, 2003)). approach.

3.3. Permeability and selectivity

One of the outstanding problems is the impact of surface
roughness on the flow. It was discovered by Elimelech et al. The selectivity of the NF membranes, which is mostly con-
that the commercial TFC membrane they employed fouled trolled by Donnan effects and pore size distribution, directly
more quickly than the CA membrane (Elimelech et al., 1997). determines the energy consumption and advantages of NF
They reasoned that the rougher TFC membrane surface must processes. Fig. 5 gives a thorough summary of current
have caused the observed effects. The relationship between methods for enhancing NF membrane selectivity. The se-
the membrane flow and the surface was shown by Hirose lective properties of NF membranes are mostly determined
et al (Hirose et al., 1996). Increases in surface roughness were by their charge interactions and steric resistance. Therefore,
shown to improve flow because more surface area was made a narrow pore-size distribution may be the key to achieving
accessible for membrane transfer. Additionally., Vrijenhoek high solute-selective separation efficiency (Fig. 5a). Increased
et al. demonstrated conclusively that, for some NF mem- selectivity, especially for charged solutes, can be achieved by
branes, fouling is strongly correlated with surface roughness manipulating membrane surface charge because of the di-
(Vrijenhoek et al., 2001). This was explained by the fact that electric exclusion and the Donnan effect (Fig. 5b). Ad-
colloidal particles preferentially collect in the valleys of the ditionally, since the membrane pore diameters will become
rough membrane surface, as a result of the enhanced inter- smaller as foulants build up over time, the selectivity of NF
actions between them brought about by an increase in sur- membranes will be indirectly decreased by inevitable mem-
face roughness. As a consequence, valleys get obstructed and brane fouling during operation (Fig. 5c). Feng et al. discovered
fouling intensifies on the surface of the rougher membrane that the influence of heavy metals on membrane fouling
(Zhang and Jiang, 2019). Nonetheless, opposite outcomes are could be divided into two categories (Feng et al., 2013). Heavy
also observed for organic particles (Yan et al., 2006; Li et al., metals alter sludge by changing the sludge's properties,
2006). Adhesive forces (interaction between organic particles which plays a significant role in membrane fouling. Con-
and the membrane surface, etc.) are likely critical factors in versely, heavy metals could play a causal role in inorganic
fouling (Huisman et al., 2000). Furthermore, during the be- fouling (Jamil et al., 2018). On the other hand, heavy metals
ginning of the fouling process, particles are brought into di- could also be a direct cause of inorganic fouling (Shirazi et al.,
rect contact with the membrane surface, and it is the 2010). The fouling of membranes by compounds of heavy
interaction between the organic particles and the membrane metals may sometimes be permanent, making restoration
surface that ultimately determines how much fouling will impossible. Cleaning using acids (like citric acid) is common
occur. In contrast, following the creation of the gel layer, the to get rid of inorganic foulants (Agnihotri et al., 2020). Nu-
contact between organic particles becomes increasingly sig- merous attempts have been committed to constructing NF
nificant. Therefore, the impact of surface roughness on the membranes with uniform pore diameters or altering the
overall performance of membranes is, at best, debatable. In hydrophilicity or charges on/in the selective layer to improve
addition, the impact of surface roughness on the deposition membrane selectivity, with some success in minimizing
of smaller molecules remains unclear. It seems intuitive that membrane fouling (Mkpuma et al., 2022). Improvement in
a smoother surface will exhibit less adsorption to organic membrane permeance without sacrificing ion/molecule re-
molecules, and that a rougher, more heterogeneous surface jection can also be seen as a result of increased NF mem-
would be more effective at adsorption due to its increased brane selectivity (i.e. increasing separation selectivity
surface area (Rana and Matsuura, 2010). between water and solutes). Adding nanofillers to the
Chemical surface modification is performed to reduce polymer matrix is another method for increasing the per-
surface roughness because chemicals in the liquid phase meance of NF membranes (Fig. 5d). Through the creation of
may more effectively enter pores and provide a smoother interfacial gaps and their intrinsic nanopores, these nano-
surface (Nemani et al., 2018). Atomic layer deposition (ALD) is fillers offer new molecular transport channels. Covalent or-
another technique for managing roughness; it is a self-lim- ganic frameworks (COFs) and metal-organic frameworks
iting surface reaction process that creates uniform thin (MOFs) are promising materials to enhance membrane se-
coatings with an atomic-scale-controllable thickness and lectivity because of their beneficial properties, such as their
flawless intactness (Lee et al., 2020). The total number of ALD extremely high surface area, strong thermochemical
 Chemical Engineering Research and Design 189 (2023) 530–571 539

Fig. 5 – Techniques for improving the selectivity of NF membranes while manufacturing the membrane. By altering the pore
size, adjusting the charge distribution, making an anti-fouling modification, or adding nanofillers to the polymer matrix
during membrane manufacture, selectivity can be increased.

stability, controllable pore structure, and functionalized pore hydrophilic surfaces. The performance of a membrane is
walls. By carefully combining their ligands or by post-func- influenced by crucial properties such as wettability, pore
tionalization, MOFs (or COFs) can manage their pore size and size, and surface energy. The wettability of a solid surface is
shape in addition to their chemical design versatility. These influenced by its shape and chemical composition. The ad-
materials' cavities can also be customized for particular ap- vantages of the various coating processes used in the lit-
plications, and they can encourage beneficial interactions erature for superhydrophobic and superoleophilic (SHSO)
with polymers (Guo et al., 2022). surfaces are compiled in Table 3 (Priyadarshini et al., 2019;
Mahajan and Sidhu, 2018; Chakraborty et al., 2018; Liew et al.,
3.4. Hydrophilicity 2020). Coated layer properties and their process are described
and include characteristics like coating layer homogeneity,
The membrane's hydrophilicity is assessed using the water controllability of coating thickness and functional groups,
contact angle. A membrane's permeability and antifouling potentials in building hierarchical micro- and nano-rough-
properties can be enhanced by raising its hydrophilicity. ness, coating precision, simplicity, cost-effectiveness, pro-
Although most solids are naturally rough, this roughness is cessing speed, versatility in handling complicated
typically insufficient to keep the material's surface in a super geometries and different materials, large-scale application
hydrophilicity state. Only a few materials have been studied, potential, and coating process repeatability.
despite the fact that any natural or artificial substance could In recent years, coatings with switchable wetting prop-
theoretically be made into a super hydrophilic surface erties have attracted the attention of numerous research
through chemical processing and mechanical roughening, or groups. In some coatings, a transition between super-
broken down into sub-microscopic particles and then de- hydrophobic and super hydrophilic states was established.
posited to form a super hydrophilic coating. Two inorganic This has been accomplished for films created using the sol-
substances that are widely employed for their photoinduced gel technique (Gu et al., 2021). Graft polymerization is a
self-cleaning capabilities are zinc oxide (ZnO) and titanium practical substitute for boosting the hydrophilicity of poly-
oxide (TiO2) (Rafique et al., 2020). SiO2 is a material that has meric membranes and enhancing antifouling resistance
been extensively researched due to its hydrophilicity and low (Pinem et al., 2019). It tethers hydrophilic polymer chains to
cost. Because of functional groups including carboxyl, car- the membrane surface. This method has the benefit of al-
bonyl, hydroxyl, and epoxy on the nanosheet surface, GO lowing for high water flux and long-term hydrophilicity
nanosheets are hydrophilic. Although polymers are attrac- maintenance.
tive building blocks for super hydrophilic coatings, their
surfaces typically need to be oxidized. The hydrophilicity of 4. NF membrane development
polymer surfaces can be increased by a variety of processes
that modify surface chemistry, including X-ray or ion surface The foundation of NF membrane technology development
irradiation, electron beam, plasma, and microwave treat- depends on having better filtering technologies to remove
ment. Surface roughness must be affected by the treatment, inorganic and organic contaminants from solution in a li-
or the chemical treatment must be applied concurrently with quid. Significant advancement in NF membrane performance
surface roughening, for the polymer to become super hy- can be achieved using technologies such as phase inversion,
drophilic. Some of the most frequently used coating techni- UV/photo grating, electron beam irradiation, plasma treat-
ques for modifying the wetting of the surface include sol-gel, ment, layer-by-layer, microwave therapy, etc (Yang et al.,
dip coating, layer-by-layer assembly, thermal, electro- 2019a). All of these techniques are targeted at improving
deposition, electrospinning, femtosecond laser irradiation, rejection propensity, membrane selectivity, and fouling re-
ion beam irradiation, plasma irradiation, spin coating, spray sistance (Sutariya and Karan, 2022). Despite the rapid growth
coating, and chemical vapor deposition (CVD). Utilizing low of NF applications in a variety of industries, there are still
surface energy materials, including roughness, or combining some limitations. The important benefits of NF membrane
the two are standard methods for producing super distinguished by Feng et al. are decreased membrane fouling,
540 Chemical Engineering Research and Design 189 (2023) 530–571

high separation and rejection efficiency, improved mem-

(Mahalingam et al., 2020)

(Vatanpour et al., 2022a)

(HMTShirazi et al., 2022)

brane lifetime, and chemical resistance (Feng et al., 2022).

(Sreekumar et al., 2022)

(Feng and Yong, 2020)

(Khajouei et al., 2017)
Several researchers have used cutting-edge membrane fab-

(Wang et al., 2022b)

(Wang et al., 2020a)

(Wang et al., 2022c)
(Wang et al., 2018)
(Deng et al., 2020)

(Qing et al., 2020)

rication and modification approaches namely IP and grafting
(Tan et al., 2021)
Ref.

polymerization to create membranes with significantly re-

duced fouling propensity including organic solutes, inorganic
solutes, colloids, and biological solids (Goh et al., 2022; Jin
et al., 2022). Typically comprised phase inversion followed by
IP is used to make TFC membranes (Zong et al., 2022) which
can be further developed via incorporation with additives
nanoparticles, resulting in thin-film nanocomposite (TFN)
Repeatable

(Xie et al., 2022). Therefore, the IP method, coating of a thin

protective layer on the membrane, surface modification of
polymer membranes with nanoparticles, and the grafting
✓
✓

✓
✓
✓
✓

✓
×
×
×

×
×
process are the primary techniques used for the develop-
ment of NF membranes with low biofouling properties, high
Flexible

heavy metals rejection, and permeability; these are dis-

cussed in subsequent sections.
✓
✓
✓
✓

✓
✓
×
×
×
×

×
×
Process

4.1. IP process
Affordable

Two different categories of IP essential design concepts are

schematically presented in Fig. 6. One technique for surface
✓

✓
✓
✓

✓
✓
×

×
×
×

×
×

coating is the molecular layer-by-layer approach (Fig. 6a),

which includes dipping a substrate alternately into two
Fast

monomer solutions (such as m-phenylenediamine (MPD) in

✓

✓
✓

✓
×
×
×

×
×
×

water and trimethyl chloride (TMC) in hexane) and then

washing with the appropriate solvents (water and hexane).
The dip-coating process is repeated several times to control
Simple

the layer thickness and improve the membrane quality,

✓
✓
✓

✓
✓

producing a thin, defect-free film made of PA multilayers.

×
×

×
×
×

The majority of available CNF membranes are TFC

membranes created by the IP of triacyl halide and amines
Precise

soaked in organic solvents and aqueous solutions respec-

tively. Due to the simplicity of production, membranes are
✓
✓
✓

✓
×
×
×
×
×
×

×
×
×

typically in flat sheet or tubular shapes (Qian et al., 2021;

Wang et al., 2022a). Compared to flat sheet and tubular
Table 3 – properties of the various surface modification coating methods.

Hierarchical

membranes, hollow fiber membranes have a greater ratio of

surface area to volume and greater packing density (Junaidi
et al., 2020). While IP in flat sheets is relatively straightfor-
✓
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✓
✓
✓
✓
✓

✓
✓
✓

ward, achieving similar results in hollow fibers presents a

×
×

×
Coating

greater challenge. When any of the stages are performed

incorrectly, the outcome may be flawed or impossible to re-
Controllable

plicate (Mohammadifakhr et al., 2020; Sewerin et al., 2021).

There are currently no practical approaches for carrying out
IP on hollow fiber membranes on a large scale (Gao
✓

✓
✓
×
×

×
×

et al., 2020).
Sacrificial interlayers can act as a fine-tuned support layer
to boost the IP features which its creation process is shown in
Uniform

Fig. 6b. Initially, a sacrificial layer is applied to a substrate

(upper panel), then, a PA layer on top of a tailored substrate is
✓

✓
×

×
×
×
×
×
×

×
×

formed (middle panel) and finally, by dissolving in the sol-

vent the sacrificial layer is removed (lower panel).
Femtosecond Laser Irradiation
Coating Application Method

4.1.1. Surface charge

Layer by Layer Assembly

The thin layer on the surface of the membranes is the con-

Ion Beam Irradiation

sequence of the copolymerization and reactivity of two re-

Plasma Irradiation
Electrodeposition
Electrospinning

active monomers (Fig. 6a). Due to the availability of

Spray Coating
Spin Coating

reactants, this reaction is self-inhibiting, and a film layer

Dip Coating

with a few tens of nanometers can be produced. This thin

Thermal

Grafting
Sol-Gel

active layer controls the total permeability, solute retention,

CVD

and overall efficiency of the membranes. In IP, a reaction

product is formed when two reactive monomers (often
 Chemical Engineering Research and Design 189 (2023) 530–571 541

Fig. 6 – IP developing methods for high-performance TFC membranes with (a) surface coating techniques and (b) sacrifice
interlayer (Goh and Ismail, 2018; Cai et al., 2020; Eslami et al., 2020; Wang et al., 2021a).

amine and acyl chloride) dissolved in two different im- post-modification techniques to enhance the surface charge
miscible solvents interact with one another at their interface. of TFC NF membranes by graft polymerization, plasma-in-
The most commonly used monomer in the organic phase duced polymerization, ion implantation, and surface coating,
is TMC, which has three acyl chloride groups. Some TMC which will be explained in the next parts. Although the po-
compounds have acyl chloride groups that could change into sitively charged NF membrane may efficiently reject the
carboxyl groups during or after the IP process. Some TMC multivalent cations, the membrane fouling issue must also
molecules may come into touch with an aqueous solution be considered. Membrane fouling may be aggravated by the
during the IP process due to molecular diffusion caused by a electrostatic attraction between the positively charged
concentration gradient. When the membrane was sub- membrane and the negatively charged foulants because
merged in water following the IP procedure, some remaining many water pollutants, including humic acid, silica (SiO2),
acyl chloride groups could change into carboxyl groups. In polysaccharides, and bacteria, are negatively charged and
neutral solution conditions, the carboxyl groups produced by may coexist with heavy metals in water (Hansima et al.,
either of the two methods might render the resultant 2021). Furthermore, significant barriers to the commercia-
membrane electronegative, which is detrimental to heavy lized manufacture and deployment of these membranes in-
metal removal due to electrostatic attraction (Jiang et al., clude their difficult fabrication process and high
2020). In order to increase the ability of the NF membrane to manufacturing costs. In surface coating techniques, sig-
remove heavy metals, it is reasonable to reduce the mem- nificant parameters that affect NF membrane functioning
brane's electronegativity or even make it positively charged. include pore size, interfacial reaction temperature, polymer
Several researchers have investigated different monomers hybridization, and creation of surface charges which are re-
with the same functionality as the PA monomers (including viewed below.
amine or acyl chloride) to acquire the optimal performance
and attributes of membranes, such as making the surface of 4.1.2. Pore size and structure
the NF membrane positively charged to effectively reject Decreasing the pore size of the NF membrane is another
multivalent cations. For instance, polyethylenimine, poly- technical method for enhancing its capacity to reject heavy
allylamine, ethylenediamine, and chitosan are alternate metals. The pore size of a TFC-NF membrane can be affected
amine groups that researchers have utilized to make the by the monomer concentration, monomer temperature, and
membrane more positive. 1,3-benzene disulfonyl chloride, type of monomer solution. Due to its significant size exclu-
2,4,6- trichloro- 1,3,5- triazine, and 4-(dimethylamino) ben- sion effect, the MPD-based NF membrane was able to suc-
zaldehyde that has been employed in the IP process of TFC cessfully reject all multivalent cations; nevertheless, this
NF membranes are further options for creating the surface resulted in limited water permeability. Because of their loose
positive (Wu et al., 2014; Moslehi, 2022; Wang et al., 2019; structure and negatively charged PA layer, which is a result
Zhao et al., 2022a; Wu et al., 2022b; Kumar et al., 2014). of the hydrolysis of acyl chloride groups in TMC, most PIP-
Table 4 sunmarizes the findings of other investigations on based NF membranes exhibit insufficient rejection of diva-
the use of different monomers to MPD or PIP and TMC for lent cations while having increased water permeability. The
positive surface TFC NF membranes. It is also common to use majority of the literature uses TMC concentrations that range
542 Chemical Engineering Research and Design 189 (2023) 530–571

Table 4 – Recent studies on new monomers for positive surface TFC NF membranes in IP method.
Monomer in the water phase Monomer in the organic phase Zeta potential OP (bar) Permeability Ref.
in pH 7 (mV) (L m-2h-1)

+ 11 8 24.5 (Wu et al., 2014)

+ 15 8 74 (Moslehi, 2022)

+8 5 34.1 (Wang
et al., 2019)

+ 11.8 2 20.3 (Zhao et al.,

2022a)

+ 28 8 80 (Wu et al., 2022b)

+ 27 2 60 (Kumar
et al., 2014)

from 0.1 to 0.15 w/v % (Almijbilee et al., 2020; Thummar et al., monomer and extremely reduce the TMC concentration. This
2022; Park et al., 2021; Tajuddin et al., 2022; Kumar et al., may result in high water flux and a constructive effect in
2022; Xie et al., 2012). The amount of TMC present in the removing heavy metals.
organic phase may have a significant impact on molecular Recently, Tian et al (Tian et al., 2020a). researched a TFC
diffusion, the amount of leftover monomer, and the structure NF membrane with appropriate water permeability and high
and charge characteristics of the PA layer. To overcome this heavy metal removal that was manufactured by reducing the
obstacle, it is possible to simultaneously modify the PA layer TMC concentration to an extremely low amount. They found
structure and charge property when using PIP as an aqueous that the optimum physicochemical parameters of the PA
 Chemical Engineering Research and Design 189 (2023) 530–571 543

Fig. 7 – (a) Schematic for the fabrication of TFC NF membranes using the temperature-assisted IP technique. (b) Images
captured by SEM of TFC NF membranes manufactured between − 15 and + 50 °C
Adopted from (Cheng et al., 2021).

layers incorporated in the NF membrane (NF-0.03) were de- made at a high interface temperature is better suited for
termined to be 0.03 w/v % TMC and 0.6 w/v % PIP with a pore removing heavy metals. For Mn2+, Cu2+ and Cd2+, respec-
radius of 0.305 nm. In addition, this membrane's PA layer had tively, rejections of 97.9%, 93.9%, and 86.7% were shown with
a reasonable thickness of 50 nm and a weak negative charge an optimized membrane sample at 50 °C temperature of oil
of the isoelectric point (IEP) = 5.1. All of these characteristics phase solution. Since the IP reaction released heat, the re-
contributed to exceptional removal effectiveness of almost action temperature could be raised to cause greater disrup-
98% against Cu2+, Zn2+, and Ni2+, and > 92.7% against Cd2+, tion of the reaction interface. The high temperature would
while maintaining a high pure water permeability of 14.6 L/ encourage the evaporation of the organic solution due to the
m2 h-1 bar-1. high volatility, which would further increase the interface
Another method to control the diffusion rate of the PIP instability. As a result, the reaction contact grew more un-
monomers is the solution temperature. The PIP monomers stable, which caused the morphology to take the appearance
contribute to a faster IP reaction rate, which results in a PA of irregular wrinkles. The degassing of the dissolved gases
layer that is thinner and more permeable to water. It is im- was also accelerated by the increased heat release. The
portant to investigate the function of the simultaneous lowered negative charge, fewer surface flaws, and con-
constrained diffusion for the PIP and TMC monomers in the stricted pore size with increased temperature are responsible
structure and functionality of the TFC NF membranes given for the improved separation efficiency for heavy metals of
the differences in the transport behavior during the IP reac- the NF membranes.
tion. The diffusion of PIP monomers in the organic solution Changing the materials used in IP method is one of the
predominates the creation of the PA film because the IP re- hopeful alterations that make the membranes more efficient.
action occurs close to the organic-phase side. Lower diffu- The surface roughness, controlling the pore size, crosslinking
sivity into the organic phase is produced by decreasing the density, separation efficiency, chemical structure, and hy-
temperature of the organic solvent, which also causes an drophilicity of membranes are only some of the physico-
increase in surface tension and viscosity (Wang et al., 2021b). chemical qualities that these monomers have been shown to
A lower rate of TMC transfer toward the reaction interface significantly contribute to in recent research (Zhao et al.,
will also result from the decreased temperature. As an out- 2022b; Li et al., 2019, 2021). Due to the incorporation of new
come, IP can concurrently restrict the diffusion rate of the PIP materials, more advantageous functional groups are emer-
and TMC monomers by lowering the temperature of the or- ging, such as carboxylic and amine groups, which can control
ganic phase. the speed of the polymerization process and improves the
The modified IP procedure suggested by Cheng et al., in membrane characteristics. Examples of new monomers
which the TFC NF membranes were created by regulating the without having amine groups that can interact with TMC
temperature of oil-phase solutions (−15, 5, 20, 35, and 50 °C), during the IP technique are shown in the table below.
is illustrated in Fig. 7 (Cheng et al., 2021). The corresponding (Table 5).
SEM images of the TFC NF membrane surface are provided in
this figure. Here, by precisely controlling the interfacial re- 4.1.3. Polymer hybridization
action temperature during the IP process, the morphologies Antifouling performance, solute selectivity, and water per-
and chemical structures of the TFC-NF membranes were meability of NF membrane can be further improved by in-
accurately controlled. The compositions of the resulting PA troducing the Hyperbranched polymers (HBPs) to the PIP
membranes were significantly altered by the temperature- solution which the structural modification and mass transfer
assisted IP technique. The NF membranes with high inter- mechanism are explained below. HBPs are a large "family" of
facial temperatures showed consistent coffee-ring-like sur- molecules with distinct three-dimensional (3D) architectures
face morphologies. According to reports, the NF membrane and several functional groups. Numerous HBPs, such as
 544

Table 5 – Recent studies on new monomers without amine group in IP method for fabricating TFC NF membranes.
Type of Monomers Permeability (L m-2h- 1bar-1) Pore size (nm) Ref.

β-cyclodextrin 103.9 0.6–0.9 (Liu et al., 2021a)

5,5,6′,6′-tetrahydroxy-3,3,3′,3′-tetramethyl spirobisindane 9.9 0.47–1.3 (Tang et al., 2021)

3-((3,4-dihydroxyphenethyl)amino)propane-1-sulfonic acid 10.36 1 (Ding et al., 2020)

(2 S,3 R,4 S,5 S,6 R)− 6-(hydroxymethyl)tetrahydro-2 H-pyran-2,3,4,5-tetraol 4.5 0.48 (Li et al., 2016)

ammonium(4-hydroxy-3,5-dimethoxyphenyl)methanesulfonate 210 0.65 (Zhou et al., 2018)

Chemical Engineering Research and Design 189 (2023) 530–571

4,4′-((1,4-phenylenebis(methylene))bis(azanediyl))dibenzenesulfonic acid 18 0.47 (Yao et al., 2018)

 Chemical Engineering Research and Design 189 (2023) 530–571 545

Fig. 8 – The schematic of construction and mass transfer for the TFC NF membrane via HPE intervened IP
Adopted from (Tian et al., 2022).

hyperbranched polyglycerol (HPG) and Hyperbranched and the hydrogen bonding interaction between PIP and HPE.
polyester (HPE), have been used to improve the performance Consequently, the HPE-modified TFC NF membrane pro-
of membranes. HPE has a distinctive inner chamber structure duced a perfect, smooth, and thin selective layer. In the in-
and several primary hydroxyl groups at the molecule's ter- terim, HPE can be anchored into the selective layer due to a
minus. Reportedly, HPE containing different quantities of reaction between TMC and the primary hydroxyl group on its
hydroxyl groups was used directly as monomers to build the surface. By increasing the concentration of hydroxyl and
selective layer with TMC/glutaraldehyde (GA)/Terephthaloyl carboxyl groups in the selective layer, the hydrophilicity,
Chloride (TPC) (Qiu et al., 2018; Wei et al., 2013). Due to the electronegativity, and antifouling properties of the mem-
considerable impact of HPE's spatial steric hindrance, all of brane are improved. In addition, the addition of HPE with a
the resultant membrane samples had a relatively loose 3D spherical structure into the reaction solution may result
structure. These membranes can therefore only be used to in the formation of interfacial gaps between the HPE mole-
extract dyes and not metal ions. cules and the PA matrix, which may work similarly to in-
Considering the unique molecular structure of HPE, it can termolecular voids. This would cause an increase in the
be deduced that once HPE is introduced into the PIP solution interchain distance between amide molecules. Furthermore,
(aqueous phase), the steric hindrance effect of HPE and the the HPE molecule's double-branched ring shape generates an
hydrogen bonding interaction between PIP and HPE will re- intramolecular vacuum. Both intermolecular and in-
duce the diffusion rate of PIP monomer into the liquid-liquid tramolecular gaps in the HPE-modified TFC NF membrane
interface reaction zone. Then, it is anticipated that a re- can operate as channels for the rapid passage of water mo-
stricted IP technique will be developed that can reduce the lecules. Subsequently, the permeability of the HPE-modified
thickness of the selective layer. The principal hydroxyl group TFC NF membrane to pure water was dramatically increased.
on the surface of the HPE molecule could react with TMC, From the other aspect, it is anticipated that the polar func-
allowing HPE to be anchored within the active selective layer. tional end groups of HPE will interact strongly and precisely
One thing that might speed up the migration of water mo- with heavy metal ions, making them excellent candidates for
lecules through the selective layer is the interior nanopore binding these ions. This new class of dendritic polymers of-
and the hydrophilic hydroxyl groups on the surface of HPE fers novel strategies for developing nanoscale chelating
molecules. On the other hand, the inclusion of hydrophilic agents for environmental applications (Zheng et al., 2015).
hydroxyl groups is anticipated to improve the antifouling The sorption behavior of several generations of nitrogen-
properties of TFC NF membranes. Balancing the "trade-off" cored HPE toward certain heavy metal ions has been docu-
between water permeability and solute selectivity improves mented by other sources (Asaad et al., 2013; Liu and Wang,
antifouling performance. The HPE modification mechanism 2007; Yu et al., 2022a).
based on the physicochemical and structural alterations of
the selective layer and the separation performance of various 4.2. Nanofiller materials
TFC NF membranes was proposed by Tian et al. and depicted
in Fig. 8 (Tian et al., 2022). Material selection for membrane modification is not a hap-
The inclusion of HPE with abundant primary hydroxyl hazard process; rather, it is based on the material's defined
groups and a regular two-branched circular structure modi- attributes, which are derived from its structural character-
fies the diffusion behavior of PIP in contrast to the un- istics as well as its chemical and physical nature. Material
controlled polymerization reaction between PIP and TMC in permeability and selectivity, heat resistance, mechanical
the conventional IP method. HPE is uniformly disseminated robustness, chemical resistivity, and economic feasibility are
in the aqueous phase owing to its large free volume, absence important factors for material selection. The materials used
of molecular entanglement, and high ductility (Peydayesh to modify the NF membrane for heavy metals removal is
et al., 2019). As a result, the diffusion rate of the PIP monomer classified in Fig. 9. The pre-synthesized fillers are added to
is drastically slow due to the steric hindrance effect of HPE the organic phase (TMC) or aqueous phase (MPD) to produce
546 Chemical Engineering Research and Design 189 (2023) 530–571

Fig. 9 – The classes of different materials to develop NF membrane for heavy metals rejection (Rao et al., 2017; Zhang et al.,
2017; Soyekwo et al., 2019; Subramaniam et al., 2019).

a mixed matrix structure within the PA layer. Different na- membranes are among the most extensively used semi-
nostructures, including organic, inorganic, and hybrid, can conductor nanomembranes due to their affordability, extra-
be utilized as nanofiller to increase the water permeance and ordinary ability to increase hydrophilicity, ease of
biofouling resistance of the PA layer. All these innovative production, increase in thermal and mechanical stability,
nanomaterials can be incorporated into membrane manu- and improvement in fouling resistance (Dutt et al., 2020). In
facture to achieve the objective of significantly enhancing the study of Kamari et al., it is reported that wastewater-
the NF membrane and other types of membranes. For the borne heavy metals like Pb2+, Cu2+, and Cd2+ ions were re-
fabrication of NF membranes, a range of metal and metal covered using a NF membrane with SiO2 NPs integrated
oxide nanoparticles, including zeolite, silica, titanium di- (Kamari and Shahbazi, 2021). Currently, the integration of
oxide (TiO2), and silver nanoparticles (AgNPs), have been layer-stacked molybdenum disulfide (MoS2) membranes with
introduced into the polymeric matrix. In terms of flow and advanced oxidation process (Chen et al., 2019), photocatalytic
rejection, mechanical stability, and anti-fouling qualities, and adsorption technologies (Zhang et al., 2020b; Zhao et al.,
this combination can improve membrane performance (Baig 2020) have been reported to improve membrane perfor-
et al., 2022; Yu et al., 2022b; Bandehali et al., 2019, 2020a). mance, reduce membrane fouling, and/or increase the re-
moval efficiencies of pollutants. The combination of various
4.2.1. Inorganic nanofillers water treatment techniques enables the effective removal of
Extensive research has been conducted on ultrafine and impurities while conserving energy and reducing costs. Non-
highly dispersed metal-based nanoparticles to remove metal corrosive, non-toxic, thermally stable, and environmentally
pollutants from wastewater. For instance, AgNPs have the safe, ZnO, MgO, TiO2, and Al2O3 are used for the removal of
potential to act as an acceptor for Hg(II) by converting it to Hg, Pb, Cu, Cd, Co, As, and Ni. The capacity of these nano-
zero-valent mercury and producing Ag-Hg amalgam (Zhang particles to adsorb metals was dramatically higher than that
et al., 2022a). It has been demonstrated that immobilizing of any of the other nanoparticles studied (Zhang et al., 2020c).
aluminum, copper, zinc, and iron, on the top surface, gives Another interesting inorganic material recently proposed
membranes anti-fouling and antibacterial qualities as an active nanofiller in membrane technology is GO.
(Vatanpour et al., 2022b). Another inorganic material used as Incorporating GO into membranes has several benefits, in-
a nanofiller is cobalt ferrite, which is regarded as one of the cluding (i) the abundance of hydrophilic functional groups
best magnetic ferrites. This material's wide applicability is (such as carboxyl, hydroxyl, and epoxy groups), (ii) the
due to its high specific surface area, chemical inertness, and polymer matrix's high compatibility, (iii) the planar struc-
high mechanical hardness. In order to effectively remove ture, which enables the GO to be horizontally aligned to
heavy metals, spinel ferrite nanoparticles must be mono- produce an ultrathin polymer-GO layer, and (iv) producing
disperse, meaning that their very small diameters are dis- mixed matrix membranes' surface charge and (v) improve-
tributed across the whole sample (Jayalakshmi et al., 2022). ment of mechanical and antifouling capacities (Wang et al.,
These nanoparticles of cobalt ferrite display magnetic ac- 2020b). When producing mixed matrix membranes with GO
tivity, which facilitates separation subsequent treatment. present, it can either be included in the polymer matrix or
Magnetic separation offers safer and more environmentally employed as a distinct layer directly on the membrane sur-
friendly disposal due to its capacity to process large volumes face (membrane surface modification) (Bassyouni et al.,
of wastewater in a short amount of time without developing 2019). GO can be functionalized with various modifiers, such
secondary contaminants (Mehta et al., 2015). In addition, NF as HBPs, linear polymers, ethylenediamine, and alkoxysilane
membranes can be fabricated using semiconducting mate- groups, to improve membrane performance. The hydrolyzed
rials such as silicon and its constituents. Silicon-modified NF polymethyl methacrylate grafted on GO mixed matrix
 Chemical Engineering Research and Design 189 (2023) 530–571 547

membranes made of PES exhibit excellent performance in The production of defects is attributed to the limited mis-
the separation of heavy metal ions and is a useful additive to cibility between the inorganic nanofillers and polymeric
enhance the permeability and antifouling properties of na- matrix, which prevents their aggregation in the selective
nocomposite membranes (Mahmoudian et al., 2018). layer, or to the blockage of the IP reaction, which leads to the
formation of fewer crosslinked PA areas. It has long been a
4.2.2. Organic nanofillers problem for all sorts of dense membranes with hetero-
Currently, research is being conducted on the concept of geneous matrix structures (Ng et al., 2021).
adsorbing polyelectrolyte (POE) chelating polymers onto NF As stated previously, the nonuniform distribution of na-
membranes for the removal of heavy metals. Certain poly- nomaterials in polymeric nanocomposite membranes is the
mers, such as poly (acrylic acid-co-maleic acid), poly (acrylic greatest obstacle posed by both the blending and phase in-
acid), and poly (dimethylamine-co-epichlorohydrin-co-ethy- version steps. It is induced by the aggregation of nano-
lenediamine), were chosen due to the following factors: The particles in the polymeric nanocomposite dope solution and
factors are (i) the negatively charged functional groups on the their partial incorporation in the membrane matrix during
polymers can enhance the adsorption of the polymers onto the phase inversion procedure (Zahid et al., 2018). Nano-
the oppositely charged membrane; (ii) the induced negatively particle aggregation causes the creation of non-selective
charged functional groups from these polymers can change gaps at the interface between the polymer and nanoparticles,
the membrane surface charge, making it more negatively which drastically lowers the rejection rate. Altering nano-
charged at high pH; (iii) the adsorption of POE, such as per- particles or using new membrane manufacturing methods
oxyacetic acid (PAA), has an antifouling function; (iv) che- might improve separation efficiency. Dong et al (Dong et al.,
lating polymers are able to absorb heavy metal ions, (v) the 2016). described a unique method for fabricating TFN-NF
POE coating may decrease the membrane pore size and en- membranes. In situ production of a PSU support containing
hance the rejection; and (vi) the adsorbed coating is simple zeolite nanoparticles was followed by IP to generate a PA
and can be customized according to different applications layer. The larger loading and more consistent dispersion of
(Shrestha et al., 2021; Gao et al., 2014). nanoparticles in the PA layer of the new TFN membrane led
One of the most common environmentally friendly nat- to better water permeability. Novel modified mesoporous
ural biopolymers utilized in membranes is CS. A lot of people SiO2 nanoparticles (MSiO2-NPs)/PA TFN membranes were
are interested in it since it is hydrophilic, inexpensive, has a fabricated by Wu et al (Wu et al., 2013). via IP method with
high perm selectivity for water, and possesses amino-hy- TMC and PIP. (MSiO2-NPs) were added to the PIP aqueous
droxyl functional groups on the CS chain that can act as phase after being functionalized with amino groups. As a
coordination sites. Additionally, CS's effectiveness as a result, during IP, there would be a reaction between (MSiO2-
membrane is significantly influenced by its ability to carry NPs) and TMC, leading to a covalent link between (MSiO2-
positive and negative surface charges in acidic and basic NPs) and the active layer of the TFN membrane. The pure
environments, respectively (Bakshi et al., 2020). Recent stu- water flow of the (MSiO2-NPs)/PA TFN membrane can be in-
dies have concentrated on the utilization of membranes with creased to a maximum of 32.4 L/m2 h by injecting a suitable
CS and multi-walled carbon nanotubes integrated to achieve concentration of (MSiO2-NPs) into the aqueous phase 0.03 wt
specific aims in membrane treatment (Ahmad et al., 2022). To %, which is almost 1.5 times higher than that of TFC mem-
improve the membrane's ability to reject heavy metal ions brane. Therefore, amino functionalization of the NPs' sur-
(Pb+2, Co+2, Ni+2, Cd+2, and Cu+2) at different pH levels, car- faces is used to enhance the interfacial molecular interaction
boxylic acid functionalized multi-walled carbon nanotubes between the PA matrix and the distributed (Rajaeian
were added to the CS matrix as a selective layer on top of et al., 2013).
PSU. This allowed the rejection of nearly 99% for all of them Another strategy is developed to modernize the blending
at pH = 10 (Ganji et al., 2022). procedure by including precursors of the desired nanoma-
terials into the polymeric dope solution, rather than the na-
4.2.3. Organic/inorganic hybrids nanofillers nomaterials themselves. To perform this improved blending
Metal-organic frameworks (MOFs) are 1D, 2D, or 3D nano- process, the precursors for the desired nanomaterials must
crystalline structures consisting of organic molecules with a be soluble in the polymeric dope solution and capable of
porous structure and metal ions or ion clusters (Zheng et al., reacting with water in the coagulation bath to form nano-
2022a). MOFs can be formed by combining metallic and or- materials on the membrane surface. Bismuth oxyhalides,
ganic linkers, specifically benzenetricarboxylate and benze- such as bismuth oxychloride (BiOCl), could be suitable can-
nedicarboxylate, using chemical or physical processes. didates for this new technique since this class of materials
Integration of MOFs on a polymer matrix has been described can be produced by a water-triggered precipitation process,
for the removal of heavy metals utilizing the NF membrane which mirrors the phase inversion procedure for the pro-
(Gnanasekaran et al., 2019). Due to an increase in porosity duction of PVDF membranes (Deng et al., 2018, 2019). Due to
and hydrophilicity, TFN membranes made by embedding their excellent chemical and optical stability, superior cor-
MOFs on polyimide substrate exhibit higher permeability rosion resistance, low cost, and nontoxicity, bismuth oxy-
(Zhao et al., 2021). halides have also been widely researched as heavy metal
absorbents, photocatalysts, and electrochemical deioniza-
4.2.4. Effects of nanoparticles aggregation tion electrodes for water treatment (Deng et al., 2017; Wang
Although there has been some reported improvement in et al., 2014). The water-triggered precipitation of the nano-
water permeance and fouling resistance due to the addition materials (which resembles phase inversion) is integrated
of filler materials, practical implementations of such com- into the PVDF phase inversion in Fig. 10, which was taken
posite membranes continue to be limited by several issues. from the study work of Deng et al (Deng and Li, 2021). To
The most important reason is the unavoidable creation of generate PVDF- BiOCl nanocomposite membranes without
defects at the interface between fillers and the PA matrix. nanoparticle aggregation difficulties, N-Methylpyrrolidone
548 Chemical Engineering Research and Design 189 (2023) 530–571

Fig. 10 – A plausible mechanism of the modified blending-phase inversion technique for producing PVDF-BiOCl
nanocomposite membranes (a). Top surface SEM images of PVDF, and PVDF-0.2BiOCl (b). Composite membranes have
substantially smaller pore size and surface porosity compared to plain membranes because the BiOCl blocks some holes and
reduces pore size.
(Adopted from (Deng and Li, 2021)).

(NMP), Ethylene Glycol (EG), Potassium Chloride (KCl), and Bi Surface grafting has benefits over traditional physical
(NO3)3 were dissolved in the PVDF dope solution to promote methods of modification, including high control of localized
the simultaneous precipitation of PVDF and hydrophilic grafting onto the target surface, simplicity of modification,
BiOCl. This nanocomposite membrane showed an adsorption minimal graft delamination, and substantially higher che-
capacity that was three times higher than that of a standard mical stability (Ghasemlou et al., 2021). As a result of the
membrane when measured against Cr (VI). Table 6 sum- grafting technique, the pore structure could undergo en-
marises the effects of organic, inorganic, and hybrid nano- largement or contraction. Therefore, parametric analyses of
fillers on the NF membrane and how well they remove heavy the grafting technique on various NF membranes are es-
metals. sential. Monomer grafting onto NF membranes has the fol-
Since nitrogen has a strong affinity for Pb2+, Cd2+, Ni2+, lowing benefits. (i) Introducing sufficient charged groups to
and Cr2+ ions atoms, its high concentration in GO-PAMAM produce electrostatic repulsion from the membrane surface,
provided favorable conditions for attracting those ions, (ii) reducing the contact of undesirable solutes and particles
leading to a higher heavy metals rejection corresponding to with the surface, and (iii) increasing the hydrophilicity for
GO-PAMAM/PES membrane with 100% rejection of those ions enhanced surface-water interaction are all ways to improve
(Al-Gamal and Saleh, 2022). The increased rejection rate seen membrane performance. In NF membrane technology, these
was caused in part by the double layer of co-ion-repelling techniques can help reduce fouling.
adsorbed ions. The possible use of phytic acid (C6H18O24P6), Several reviews addressed the grafting procedures from a
Tannin (C76H52O46), and saponin (C58H94O27) in the NF different point of view (Zhou et al., 2015; Sculean et al., 2008;
membrane have not been documented anywhere, according Basheer et al., 2020; Zainol Abidin et al., 2022; Miller et al.,
to our analysis of the nanofiller materials described above. As 2017). In this part, a multi-aspect review of grafting techni-
harmless organic macromolecules, phytic acid, Tannin, and ques that leads to improvement of hydrophilicity and se-
saponin are readily extracted from cereal grains, seeds, and paration performance is carried out. The choice of grafting
plant-derived products. They contain hydroxyl groups and procedure in NF membrane is determined by the preferred
phosphate carboxyl groups (Fig. 11), which gives them con- chemical structure and membrane system characteristics.
siderable negative charges and the ability to form complexes There are numerous ways to begin graft copolymerization,
with a variety of metal ions, including Zn2+, Cu2+, Cd2+, Ni2+, including chemical and physical treatments. UV/photo-
and Pb2+. Therefore, not only may they increase perme- grafting, electron beam (EB) irradiation, plasma, and micro-
ability, but they can also trap heavy metals that pass through wave therapy are subcategories of physical activators. The
the membrane through complexation. initiators of chemical grafting are free radicals and oxidants.
Fig. 12 demonstrates the classification of the grafting tech-
4.3. Grafting process nique for membrane surface treatment along with a sche-
matic representation of the manufacturing process for each
Grafting is a well-known method for changing the surface of subclass. Using immersion and photo-grafting techniques,
organic substrates. Grafting is a technique where monomers water-soluble and weakly acidic monomers such acrylic acid,
are modified onto a polymer chain through covalent bonding. methacrylate derivatives, cardo polyether ketone, and N-
 Chemical Engineering Research and Design 189 (2023) 530–571 549

Table 6 – Organic, inorganic, and hybrid nanofillers' impacts on NF membrane heavy metal removal.
Nanomembrane material Separation layer Types of PWF Removal Ref.
membrane (L/m2.h) efficiency (%)

Inorganic Ni-bentonite Flat sheet 58.8 Zn2+: 98.62 (Dadari et al., 2022a)
Nanomembranes nanoparticles/PES Cu2+: 97.88
Pb2+: 97.03
GO- PAMAM/PES Flat sheet 61.52 Pb2+: 100 (Al-Gamal and Saleh, 2022)
Cr3+: 100
Cd2+: 100
Ni2+: 100
Cu/PEI Flat sheet 11 Ni2+: 96.5 (Roy et al., 2021)
Cd2+: 98
Pb2+: 99
Zn2+: 98.5
As3+: 95
Cr2+: 99
NiAl /PES Flat sheet 78.34 Pb2+: 99.27 (Dadari et al., 2022b)
Zn2+: 99.15
Fe2+: 98.91
Cu2+: 98.58
ZnO/PEI Flat sheet 42.4 Pb2+: 59 (Bandehali et al., 2020b)
Cu2+: 67
Carbon nanotube/PES Flat sheet 80.5 Zn2+: 96.7 (Peydayesh et al., 2020)
Mg2+: 95.01
Cd2+: 92.4
Cu2+: 91.9
Ni2+: 90.7
Pb2+: 90.5
MoS2/ PES Flat sheet 220 Hg2+: 86 (Sreeramareddygari
Cr2+: 90 et al., 2021)
Pb2+: 95
GO-COOH / PPSU Flat sheet 27 Zn2+: 88 (Shukla et al., 2018)
Pb2+: 80
GO-MnO2/SPES Flat sheet 129.7 Cu2+: 81 (Ibrahim et al., 2022)
Zn2+: 64
Ni2+: 67
CoFe2O4/CuO/PES Flat sheet 34.5 Cu2+: 98 (Zareei and Hosseini, 2019)
Ni2+: 92
Pb2+: 88
ZnO/PEES Flat sheet 103.8 As3+: 85 (Maheswari et al., 2022)
As5+: 98
Organic/Inorganic Hybrids SiO2-[AMIm]PF6/PES Flat sheet 46.98 Cu2+: 97 (Shen et al., 2022b)
Ni2+: 95
Cd2+: 78
Zn2+: 90
Ti3C2TX-EDA Flat sheet 60 Cd2+: 98 (Jang et al., 2022)
Zn2+: 99
Pb2+: 93
Cu2+: 98
Mn2+: 99
Ni2+: 95
GO/PPD/PVC Flat sheet 0.9 Cd2+: 84 (Khan et al., 2021b)
Zn2+: 87
Cu2+: 85
Ni2+: 88
Co2+: 90
Fe3O4-SiO2-NH2/PES Flat sheet 59 Cd2+: 93 (Kamari and Shahbazi, 2020)
ZnAl-LDH NCM/ Flat sheet 95 Pb2+: 98 (Azad and Mohsennia, 2020)
PVB-PAN Cd2+: 88
Fe3O4-PDA/PES Flat sheet Pb2+: 99 (Zhang et al., 2020d)
Cd2+: 90
Ag+: 98
CurSBA-15/PES Flat sheet 42.5 Zn2+: 99 (Moradi et al., 2022)
Ni2+: 98
Pb2+: 97
Organic Nanomembranes PAA/PEI Hollow fiber 10.5 Pb2+: 99 (Gao et al., 2014)
Cu2+: 99
Ni2+: 99
Cd2+: 98
Zn2+: 98
(continued on next page)
550 Chemical Engineering Research and Design 189 (2023) 530–571

– Table 6 (Continued)
Nanomembrane material Separation layer Types of PWF Removal Ref.
membrane (L/m2.h) efficiency (%)

H-KIT-6/PSF-PVP Flat sheet 30.2 As3+: 99.8 (Gholami et al., 2022)

Hg2+: 99
CNFs-co-Cs/PES Flat sheet 13.58 Cu2+: 98 (Hosseini et al., 2021)
Cr3+: 97
Pb2+: 97
TTTP/PES Flat sheet 40.21 Cu2+: 98 (Moradi et al., 2020a)
Pb2+: 97
CS/TGIC Flat sheet 47.88 Cu2+: 99 (Yang et al., 2021)
Fe3+: 97
Zn2+: 96
CS-MPD-TMC/PSF Hollow fiber 29.7 As5+: 73 (Mondal and Raval, 2022)
PMO-PPD/PES Flat sheet 33.7 Pb2+: 93 (Mehrjo et al., 2021)
PEC NPs/PSU Flat sheet 36.8 Cu2+: 95 (Ye et al., 2019)
Zn2+: 98
B-Cur/PES Flat sheet 140.45 Fe2+: 99.8 (Moradi et al., 2020b)
Cu2+: 98.7
pb2+: 99.6
Mn2+: 99.3
Zn2+: 99.1
Ni2+: 99.5

Fig. 11 – The chemical structure of phytic acid, Tannin, and saponin as a potential nanofiller for heavy metal removal.

vinylpyrrolidone have been chosen to graft onto polymeric et al., 2019). Importantly, the distribution of grafted chains is
membranes like polyvinylidene fluoride and poly- restricted to the surface. In the majority of instances, UV
ethersulfone. Compared to pristine polymeric membranes, light is applied in the presence of a photosensitizer or pho-
the produced membranes demonstrated superior antifouling toinitiator to perform surface graft polymerization. A pos-
characteristics and selective separation (Tran et al., 2020; sible method for enhancing the membrane's surface
Han et al., 2019; Liu et al., 2021b; Fan et al., 2020). Also, hydrophilicity and anti-fouling resistance is the physical
membranes that are sensitive to temperature, light, and pH grafting of hydrophilic polymer chains (Shen et al., 2020).
were prepared using the grafting method and molecular Grafting-to, -from, and -through are three physical UV/photo
imprinted (Liu et al., 2019; Li et al., 2018; Mamah et al., 2021). grafting techniques for surface alteration. The grafting-to or
Besides, grafting techniques could be used to change UF polymer grafting approach, as depicted in Fig. 12a(i), con-
membranes into NF ones. A NF membrane with smaller nects prefabricated polymer chains to the substrate surface
pores and more ions rejection was produced by UV-initiated by covalent bonding without the use of a polymerization
polyacrylic acid grafting on the PSU-UF membrane (Qiu et al., step. Condensation reactions often occur between terminal
2007; Homayoonfal et al., 2010). An increase in hydrophilicity functional groups of polymer chains and appropriate reactive
enabled by UV-initiated graft polymerization of AA on the sites formed randomly on the substrate surface. Due to the
PES membrane has led to a flux recovery of around 44% steric effects of the bulky grafted polymeric chains, the
(Rahimpour, 2011). grafting-to technique typically yields polymer brushes with
low surface density (Wang et al., 2022b). Since the polymeric
4.4. Physical grafting grafting can be finished in a single step, grafting-to is a
straightforward grafting procedure.
4.4.1. UV/photo-grafting As shown in Fig. 12a(ii), grafting-from or graft poly-
UV irradiation-induced surface graft polymerization offers merization is a process in which monomers gradually extend
various benefits, including a rapid reaction rate, low pro- from the grafting sites on the substrate backbone to generate
cessing costs, simple equipment, and industrialization (Dong side chains of various lengths. To aid in the formation of a
 Chemical Engineering Research and Design 189 (2023) 530–571 551

Fig. 12 – Schematic diagram of an experimental process for physical grafting includes (a) UV/ photo grafting (b) electron
beam (EB) irradiation, (c) plasma, (d) microwave therapy, and chemical grafting including (e) free radicals initiators and (f)
ionic initiators (Suresh et al., 2021; Morshed et al., 2020; Bhattacharya and Misra, 2004; Kochkodan and Sharma, 2012).

high-density polymer sheet, monomers are injected into the heterogeneous or homogeneous branch addition (Pavlinec
surface starting locations during the grafting procedure et al., 2019). The physical characteristics of the grafted co-
(Wang et al., 2022c). The polydispersity of the polymer sheet polymer are impacted by changes in graft distribution. Any
can be raised by producing homopolymers through grafting established polymerization technique can be used to do the
(Yang et al., 2019b). The grafting-from technique is ad- grafting-from approach. The grafting-from approach, out of
vantageous for managing the thickness of the grafting layer the three grafting methods, enables the greatest degree of
since the monomer concentration may grow over time. surface feature customization for a liquid separation mem-
However, this tactic makes it challenging to control the re- brane (Suresh et al., 2021). In an experiment involving the
sponsive material's final chain length. Another method for UV/photo grafting process, phthalocyanine (Pc) derivatives
producing well-defined side chains is grafting-through, as and hyperbranched poly(amidoamine) (HPAMAM) were cre-
shown in Fig. 12a(iii). Frequently, a macromonomer functio- ated before being modified with maleimide groups. Following
nalized with acrylate radicals and a lower molecular weight that, these two monomers joined with a polytetra-
monomer will copolymerize. The number of grafted chains is fluoroethylene (PTFE) membrane that had been furan group-
influenced by their copolymerization activity and the ratio of modified by a Diels-Alder (DA) process utilizing UV light
monomer to macromonomer molar concentrations. The (200 W, max = 254 nm) and hydrazine vapor, as depicted in
molecular weight ratio of the monomer to the macro- Fig. 13. The alteration of the PTFE membrane's surface
monomer and their copolymerization activity determine morphology, as depicted in the FESEM image inset, was in-
how many chains are grafted (Tian et al., 2020b). During the duced by the membrane's modification. The morphologies of
reaction, the ratio of monomer to macromonomer shifts, the PTFE membrane surface during the amine and furan
causing random branch positioning and the creation of graft modifications did not differ significantly from the pristine
copolymers with various branch counts. Based on the re- PTFE surface. Therefore, neither the UV/hydrazine treatment
activity ratio of the macromolecular terminal functional nor the furan alteration had an impact on the membrane's
group to the monomer, this approach allows for either pore structure. However, a thick polymer layer partially
552 Chemical Engineering Research and Design 189 (2023) 530–571

Fig. 13 – Diagram illustrating the HPAMAM/Pc PTFE membrane preparation technique.

Inset: FE-SEM images of pristine PTFE membrane (a), aminated PTFE membrane (b), furan-modified PTFE membrane (c), and
HPAMAM/Pc PTFE membrane (d) (Adopted from (Byun et al., 2019)).

covered the surface pore structure that HPAMAM and Pc's DA substance determines penetration since electrons are not
bonds had altered. The HPAMAM/Pc-modified membrane limited by optical clarity. When a polymer and a prepolymer
was reported to exclude up to 97.1% of the Pb(II) ions and are exposed to the beam at the same time, grafting happens
remove roughly 77.6% of the Cr(VI) ions following this (Fig. 12b (iv)). The prepolymer can attach to and polymerize
treatment (Byun et al., 2019). at these reaction sites because the accelerated electrons
break the polymer's bonds. The production of NF membranes
4.4.2. Electron Beam (EB) irradiation using high-energy EB irradiation has not received much at-
EB irradiation at high energies is a straightforward and effi- tention in research. Xu et al. published one of the successful
cient approach for penetrating the polymer layer. During the studies done to remove Cr(VI) from an aqueous solution by
irradiation procedure, the effective creation of active sites on membrane alteration by electron beam radiation-induced
the polymer was feasible without the addition of any parti- technique (Xu et al., 2014). It was demonstrated that the
cular additives. The process of EB irradiation is depicted in grafted membranes showed no major morphological
Fig. 12b, where the crosslinking reaction that produces a 3D changes in relation to the substrate, indicating that the
network reduces the membrane pore size. Cross-linking is physical structure of the membrane was not adversely
the chemical process that joins linear or branched polymer harmed during the EB radiation-induced graft polymeriza-
chains into a network (Fig. 12b(i)). Using an electron beam to tion. The FESEM images in Fig. 14 that are supplied clearly
crosslink polymers breaks bonds within the polymer, which show these findings.
can then rejoin with adjacent chains to produce a net-like
structure. No additional chemistry is required for EB cross- 4.4.3. Plasma treatment
linking, which is advantageous for both rapid processing and Adding polar groups to a surface through plasma treatment
controlled applications. By covalently connecting polymer is yet another efficient method of increasing its hydro-
chains instead of relying primarily on mechanical entangle- philicity and wettability. It is useful because it affects only
ment, properties such as heat resistance, solvent resistance, the physical and chemical properties of the polymeric sur-
tensile strength, and shrinkage can be improved (Zheng face while leaving the bulk qualities unaffected. Plasma
et al., 2021). Cross-linking frequently makes it possible to treatment can modify the surface energy of polymers, hence
downscale a film without sacrificing performance. Pressure- modifying their wettability and polarity. Plasma surface
sensitive adhesives can be cross-linked to adjust the tacki- modification permits fine control of process parameters such
ness. When subjected to an electron beam, not all polymer as plasma working gas, flow rate, and vacuum, resulting in a
materials crosslink; some polymers deteriorate by a process surface with a high degree of homogeneity. Plasma treat-
known as chain scission (Dissanayake et al., 2021). The beam ment can be utilized for surface cleaning, crosslinking, acti-
ruptures internal polymer links similarly to cross-linking, but vation, etching, or a combination of these (Ma et al., 2022b).
these ruptures continue during chain scission (Fig. 12b (ii)). Plasma irradiation produces production of free radicals,
Chain scission and cross-linking are polymer-based proce- which can be used to attach active species such as mono-
dures. Additionally, prepolymers such as monomers and mers to a surface to tailor it for a particular application.
oligomers can be polymerized by using an electron beam Plasma irradiation can be used to clean, activate, and/or etch
(Fig. 12b (iii)). Cross-linking commonly occurs as a result of a surface (metal, ceramics, glass, or plastics) and plasma
the polymer chains that are formed during the reaction, polymerization can be used to coat the surface. Conse-
creating tough coatings, inks, and adhesives with minimal quently, the impacts of plasma on the surface of a polymer
migration and little to no odor. Similar to other EB processes, can be categorized as shown in Fig. 12c. Surface modification
polymerization happens in milliseconds and is initiated of polymers utilizing non-polymer forming plasma gases
without the aid of a solvent or initiator. The density of the such as He, Ar, N2, or O2 is a regularly employed technique
 Chemical Engineering Research and Design 189 (2023) 530–571 553

Fig. 14 – FESEM micrographs of PSf substrate (a), grafted membrane with DG of 2.67 mmol/m2 (NF2) (b), and grafted
membrane with DG of 4.68 mmol/m2 (NF3) (c).
Cross-sectional photographs reveal that the grafted membrane's physical properties are identical to those of the substrate
(Adopted from (Xu et al., 2014)).

Fig. 15 – Diagram of the apparatus utilized for plasma grafting

Adopted from (Alemán et al., 2018).

for changing the surface properties of polymers. These pro- whole volume, which causes it to heat up quickly and uni-
cesses generate free radicals on the surface, which then react formly. Microwave technology has been used commercially
with excited species in plasma gases. Thus, interactions with for polymerization, foam processing, and vulcanization of
N2, O2, or inert gases produce oxygen functionality such as rubbers (Ariff et al., 2020). Irradiation has a major effect on
hydroxyls, carbonyls, and, in rare instances, carboxylic altering the morphology, outer membrane layer, and mem-
groups. Déon et al. presented the example of membrane brane flow. In addition to the thermal effect, microwave ir-
surface modification by plasma polymerization of positive radiation is heavily influenced by wave effects. Regardless of
allylamine to address the inadequacies of commercial the irradiation power, increasing the irradiation period led to
membranes; their plasma grafting apparatus is represented an increase in penetration rate followed by a reduction in
in Fig. 15 (Alemán et al., 2018). It was established that this flux. This process may be considered a unique membrane
method permits a permanent alteration of the membrane photo modification technique. Microwave energy is non-io-
surface. It was discovered that the change had only a little nizing, which distinguishes it from other forms of ionizing
impact on the membrane's hydraulic permeability, resulting radiation. In other respects, the molecular structure of the
in permeation fluxes similar to those attained with virgin polymer being heated is unaffected by this type of radiation.
membranes. Although a complete reversal of the membrane The effect of the microwave irradiation period and its effect
charge's sign is not always the case, a notable increase in on the membrane surface is described below. In the first 10 s
rejection for divalent cations was shown, and this led to a of microwave irradiation, the heat action of the radiation-
considerable improvement in separation selectivity with induced excessive surface compression decreased the
monovalent cations. roughness characteristics. Rougher surfaces produced by
The removal of heavy metals (which are typically multi- longer irradiation times exhibit a higher penetration rate (Hu
valent cations) from saline solutions seems to be a very et al., 2021b). This is most likely caused by the wave char-
promising application for this method of membrane mod- acteristics of microwave radiation. Microwave heating can be
ification. Unfortunately, due to the strong exclusion me- produced by both dielectric polarisation and conduction.
chanism at the pore entry, the method is not effective Microwave energy waves alternately rise and fall above a
enough to remove divalent cations from solutions selectively horizontal baseline. The baseline half cycle has negative
containing divalent anions. characteristics, and the baseline half cycle above the baseline
has equally favorable characteristics. Because molecules in-
4.4.4. Microwave clude both positive and negative particles, they act like tiny
There has been a rise in interest in microwave irradiation in magnets. The negative molecular particles are drawn to and
organic synthesis due to the significant acceleration of some try to align themselves with this positive field of energy as
reactions compared to conventional processes carried out in the positive half cycle of the microwave penetrates the ma-
a regular microwave oven (Sun et al., 2021). An object may terial. Then, the converse happens when the microwave
directly and uniformly absorb microwave radiation over its energy alternates to the negative half cycle (the negative
554 Chemical Engineering Research and Design 189 (2023) 530–571

Fig. 16 – Diagram and potential responses of IP and diethylenetriamine (DETA) assisted microwave grafting
Adopted from (Huang et al., 2021).

particles are repelled and the positive particles are attracted). indicating its potential utility in heavy metal removal (see
Microwave ovens operate at a frequency of 2450 million cy- Fig. 16). By introducing more amine groups, the alteration
cles per second. The material's molecules experience ex- resulted in the formation of a positively charged layer on top
treme friction as a result of this rapid oscillation. The of the negatively charged PA layer, leading to an increase in
porosity and number of pores on the membrane surface hydrophilicity and IEP.
likely increase as a result of the very high oscillation of
polymer functional groups over a longer period (60 s). This is 4.5. Chemical grafting
consistent with the rejection (flow) diminishing (growing) as
irradiation power is increased. We hypothesize that during 4.5.1. Free radicals initiators
short (10 s) and intermediate (60 s) irradiation times, the Radical graft polymerization is an appealing technique for
conduction effect of irradiation and dielectric polarisation modifying surfaces. Using processes such as ion beam,
and tiny magnets (wave characteristics) are responsible for plasma, and -irradiation, the main radical can be produced
the production of low and high porosity in the membrane either directly or via electron transfer from a free radical
surface, respectively. The very high thermal effect of irra- initiator. The latter can be produced by the hemolytic
diation produces further compression of the thin layer at breakdown of chemicals such as photoinitiations or peroxide
longer durations (> 60 s) due to coalescence and polymer using heat or light, or by a redox process involving an ap-
chain combination. In consequence, extending the irradia- propriate oxidant and reductant. In the work of He et al (He
tion time improves the thermal effect. At the moderate time, et al., 2018)., a 2-methacryloyloxyethyl phosphorylcholine
however, the wave effect of irradiation predominates over (MPC) and 2-aminoethyl methacrylate hydrochloride (AEMA)
the heat effect (which causes pores to be compressed more), co-polymer, [AEMA-co-MPC], was devised and produced by a
resulting in a large number of small pores. Due to the higher single-step free-radical polymerization to effectively remove
thermal effect, longer irradiation times (> 60 s) provide an the As and Se. Fig. 17 shows their suggested method for
extremely thick surface (Zhang et al., 2020e). Huang et al creating the zwitterionic copolymer [AEMA-co-MPC] by uti-
(Huang et al., 2021). utilized microwave-assisted grafting of lizing AIBN as an initiator in modified free radical poly-
membranes to create dual-charged NF membranes that dis- merization between MPC and AEMA monomers. Fig. 17 also
played extraordinary resistance to a variety of heavy metals, shows the related FESEM images of 50 wt% [AEMA-co-MPC].

Fig. 17 – Schematic illustration of the synthesized zwitterionic copolymer AEMA-co-MPC (left). The surface and cross-
sectional morphology of co-polymer modified TFC membranes containing 50 wt% (right)
Adopted from (He et al., 2018).
 Chemical Engineering Research and Design 189 (2023) 530–571 555

Fig. 18 – Diagrammatic representation of a straightforward membrane procedure for DP-TFC using the DPC membrane and
PEI surface grafting under activation of intermediate CMPI
Adopted from (Qi et al., 2019).

The TFC membranes produced from PIP solutions containing covalent bonding with surface carboxylic groups, they cre-
50 wt% [AEMA-co-MPC] have excellent surface embossment ated the NF membranes using 2-chloro-1-methyl iodopyr-
that resembles nodules. This behavior is most likely caused idine (CMPI) as an active agent. Their intended approach is
by the higher molecular volume and slower diffusion rate of shown in Fig. 18. Their creation demonstrates that the pro-
[AEMA-co-MPC]. It inhibits the IP reaction and delays the duced membranes have an effective removal rate for
transport of PIP molecules from the aqueous phase to the harmful heavy metal ions (CrCl3: 98.0%, NiCl2: 95.8%, and
organic phase because of steric hindrance. Due to their re- CuCl2: 96%).
duced pore sizes and improved hydrophilicity, the co- In Table 7, two surface modification methods IP and
polymer modified TFC membranes demonstrate greater pure grafting that have been used by various researchers to en-
water permeability and rejections for both pollutants than hance the performance of NF membranes in the removal of
the unmodified TFC membrane. The produced TFC mem- heavy metals are listed. Investigations have been done into
brane with 50% [AEMA-co-MPC] exhibited the highest water how the active layer, surface charge, and selectivity affect
permeability of 8.5 LMH/bar and the most astounding rejec- the extraction of heavy metals from wastewater. In addition
tions of 99.8%, 99.1%, and 98.2% against HAsO42-, SeO42- and to the Donnan exclusion and size effect, their principal
SeO32- respectively. function is the production of metal complexes, and the use of
adsorptive polymers throughout the NF process seeks to in-
crease the effectiveness of heavy metal removal by compo-
4.5.2. Ionic initiators sition or adsorption. Certain scientists utilize a reagent to
It is also possible for grafting to take place at the ionic level. alter the surface charge of the NF membrane, making it po-
For this purpose, you can use a variety of different initiators, sitively charged and having hydroxyl groups, which are es-
such as alkali metal suspensions in a Lewis base liquid, or- sential for increasing membrane permeability.
ganometallic compounds, or sodium naphthalene. From the data in the table, we can conclude that the re-
Carbonium ions are formed all along the polymer chain jections of metal cations are significantly improved by using
when alkyl aluminum (R3Al) and the polymer backbone in its PEI, PIP, or PAMAM cross-linked NF membranes, but their
halide form (ACl) react. The reaction proceeds through a utility is limited by the lower penetration flow. Other studies
cationic mechanism as shown below: attempted to improve heavy metal removal via complexation
or adsorption during the NF process by adding metal com-
plexes or adsorptive polymers in addition to Donnan exclu-
sion and the size effect (Zhang et al., 2021a). There are still
some problems with chelating polymer membranes that
.
need to be addressed. Low selectivity, inability to be recycled
An anionic process can also be used to carry out grafting.
and increased fouling are a few examples (Zhang et al.,
The following chemical process is what happens when so-
2021b). Furthermore, the problem of low ion selectivity
dium-ammonia or the methoxide of alkali metals combines
caused by the pore heterogeneity of TFC-PA membranes can
with the monomer to create the graft copolymer (PO-Na+).
be addressed by manipulating the IP process to make the
original membrane more compact and fault-free (Wu et al.,
2021). On the other hand, secondary amide groups on the
surface of most of the membranes would be oxidized in the
. presence of active chlorine, resulting in substantial perfor-
The surface properties of NF membranes were reported to mance deterioration and shortened service life. By grafting a
be altered by Qi et al. utilizing a surface ionic initiators protective layer with a positive charge onto the surface of the
grafting technique (Qi et al., 2019). In order to graft a cationic PA top layer, exceptional chlorine resistance can be obtained.
macromolecule polymer onto the membrane surface via However, due to chemical cross-linking and chain transfer in
556 Chemical Engineering Research and Design 189 (2023) 530–571

Table 7 – Summary of various NF membrane surface modifications highlighting essential characteristics and filtration
performance.
Substrate / Active Working principle WCA Fabrication & OP (bar) Feed Rejection (%) Permeance Ref.
layer (Types of / (Membrane (◦) modification solution (Lm- 2h-
1
membrane) Charged) Method bar- 1)

PES-TMC /PIP- DETA Donnan effect / 43–44 IP 5 2000 ppm 17 (He

(Flat sheet) (Positive) NiSO4 94.8 et al., 2018)
ZnSO4 94.5
CuSO4 95.9
Cu(NO3)2 89
Pb(NO3)2 85.1
PSF/PEI-PA (Flat Complexation 31–33 IP 5 500 ppm 8.86 (Zhang et al.,
sheet) sites with metal Cd(NO3)2 100 2021a)
ions / (Negative) NiCl2 99.91
CuSO4 100
Pb(NO3)2 99.99
P84/PEI (Flat sheet) Donnan 62–65 IP 8 10 ppm 6 (Zheng et al.,
electrostatic Cu(NO3)2 100 2022b)
repulsion & Size ZnCl2 67
exclusion / Ni(NO3)2 66
(Positive) PbCl2 78
Kevlar/ TMC- TEA Donnan 70–73 IP 6 1000 ppm 13.6 (Zhang et al.,
(Flat sheet) electrostatic ZnCl2 97.4 2022a)
repulsion & Size Cd(NO3)2 97
exclusion / CuCl2 97.9
(Positive) Ni(NO3)2 97.7
PbCl2 91.7
Kevlar/PEI-TMC-THPC Donnan 50–53 Grafting 6 1000 ppm 11.6 (Zhang et al.,
(Flat sheet) electrostatic ZnCl2 96.3 2022b)
repulsion & Size Cd(NO3)2 95.8
exclusion / CuCl2 95.9
(Positive) Ni2(NO3)2 96
PbCl2 90
PES/PIP-TMC (Flat Size exclusion & 39.5 IP 4 1000 ppm 6.4 (Zhang et al.,
sheet) ions selectivity / CoCl2 98.2 2021b)
(Negative) NiCl2 98.9
CuCl2 94.5
PSF/Pa-Tp/ PIP-TMC pore size NR IP 5 2000 ppm 8.66 (Jiang
(Hollow fiber) distribution / Cr2(SO4)3 65.4 et al., 2021)
(Negative) CuSO4 64.3
ZnSO4 91.7
MnSO4 91.0
PES/PIP-TMC/CTAB Donnan 20–25 IP 3.5 500 ppm 21.5 (Xu
(Flat sheet) electrostatic ZnSO4 98 et al., 2022)
repulsion & Size NiSO4 98
exclusion / Cu(NO3)2 98
(Positive) Pb(NO3)2 85
PAN/TMC-PEI (Flat Donnan 45–50 IP NR 1000 ppm 31.5 (Wang et al.,
sheet) electrostatic NiCl2 95 2022d)
repulsion & Size ZnCl2 93
exclusion / CuCl2 93
(Positive) PbCl2 80
PVDF-SMA/GR-T-CH3I Donnan 97.3 IP & Grafting 1 1000 ppm 27.9 (Yang
(Hollow fiber) electrostatic in 0 s NiSO4 99.4 et al., 2022)
repulsion & Size 0 CuSO4 99.6
exclusion / in Cr2(SO4)3 99.9
(Positive) 180 s
PSF/PIP-TMC-BIBB- Donnan 35–37 IP & Grafting 6 1000 ppm 14 (Wu
DMC (Flat sheet) electrostatic CuCl2 93.5 et al., 2021)
repulsion & ZnCl2 96.8
hindrance effect /
(Positive)
PES/ PAMAM Donnan 50–55 IP & Grafting 10 200 ppm 3.6 (Zhu
dendrimer electrostatic CdCl2 99.13 et al., 2015)
(Hollow fiber) repulsion & Size Pb(NO3)2 99.67
exclusion / CuSO4 99.61
(Positive)
PES/PEI-BTC (Flat Donnan exclusion 71.87 IP 10 1000 ppm 15.68 (Li et al., 2022)
sheet) / (Positive) MnCl2 98.78
ZnCl2 98.32
NiCl2 97.74
(continued on next page)
 Chemical Engineering Research and Design 189 (2023) 530–571 557

– Table 7 (Continued)
Substrate / Active Working principle WCA Fabrication & OP (bar) Feed Rejection (%) Permeance Ref.
layer (Types of / (Membrane (◦) modification solution (Lm- 2h-
1
membrane) Charged) Method bar- 1)

CuCl2 95.67
CdCl2 90.49
P84/PEI (Flat sheet) Donnan 60–65 IP 4 250 ppm 10.8 (Zheng et al.,
electrostatic PbCl2 99.0 2022c)
repulsion & the Ni(NO3)2 96.7
steric hindrance / ZnCl2 96.2
(Positive) Cu(NO3)2 99.8
PVDF-SMA-GTA/PAA- Donnan NR Grafting NR 100 ppm 29.6 (Song
EDS-NHS electrostatic CuSO4 94.2 et al., 2022)
(Hollow fiber) repulsion & the
steric hindrance /
(Negative positive
dual-charged)
PI/PEI-TMC-ANPI (Flat Donnan 37.7 IP & Grafting 6 1000 ppm 7.33 (Bai
sheet) electrostatic CuCl2 98.1 et al., 2022)
repulsion & Size NiCl2 98
exclusion /
(Positive)
PSF/COOH-TiO2-TMC Donnan effect / 49.4 IP 10 2000 ppm 8 (Karki and
(Flat sheet) (Negative) CuSO4 86.89 Ingole, 2022)
HgCl2 77.01
Pb(NO3)2 83.42
PES-PVP/TTP (Flat Donnan effect / 32.1 Grafting 4 100 ppm 17.5 (Moradi
sheet) (Negative) Cu(NO3)2 95.3 et al., 2021)
Pb(NO3)2 96.1
PES/graphen oxide/ Donnan effect / 33.3 Grafting 5 20 ppm 7.16 (Abdi
metformin (Flat (Negative) Cu(NO3)2 92 et al., 2018)
sheet)
PVDF/APTES Donnan effect / 58.5 Grafting 5.5 5 ppm 0.763 (Zeng
functionalized (Negative) Cu(NO3)2 47.9 et al., 2016)
halloysite (Flat Cd(NO3)2 44.2
sheet)
PSF/PIP PA layer (Flat Donnan effect / 50.9 IP 15 617 ppm 7.33 (Pino
sheet) (Negative) Cu(NO3)2 71.8 et al., 2018)
PES/Ag- PIP PA layer Donnan effect / 45 IP & Grafting 5 100 ppm 8 (Bera
modified PEI (Flat (Positive) Cd(NO3)2 97 et al., 2018)
sheet)
P84/ PEI/ glutaldehyde Donnan effect / – IP 5 1000 ppm 14.8 (Gao
(Hollow fiber) (Positive) CdCl2 94 et al., 2016)
PES/ Donnan effect / – IP 5 200 ppm 1.66 (Zhu
polybenzimidazole (Negative) Cd(NO3)2 70 et al., 2014)
(Hollow fiber) Pb(NO3)2 93
PAN/TiO2 (Flat sheet) Donnan effect / 59.98 IP 10 50 ppm 7.68 (Hosseini
(Negative) NiSO4 88.1 et al., 2017)
CNF (NF270)/ Adsorption & Size 14.5 Grafting 3 5 ppm 13.9 (Liu
halloysite exclusion / CuSO4 74.3 et al., 2020)
nanotubes (Flat (Negative) Ni(NO3)2 70.1
sheet)
HPEI-(GO-like CNM) Donnan effect & 60 IP 1 1000 ppm 12 (Tofighy and
(Flat sheet) Size exclusion / CuCl2 92.6 Mohammadi,
(Positive) NiCl2 92.3 2020)
ZnCl2 95.6
PbCl2 90.5
CdCl2 94.1
PES/PEI-TMC Donnan effect & – IP 1 1000 ppm 5.14 (Gao
(Hollow fiber) Size exclusion / NiCl2 98 et al., 2020)
(Positive) ZnCl2 93
CuSO4 93
558 Chemical Engineering Research and Design 189 (2023) 530–571

Fig. 19 – The performance of the NF membrane which extracted from Tables 6 and 7 for (a) Cu2+, (b) Zn2+, (c) Ni2+, and (d) Pb2+
using membranes with positive and negative surface charges.

free radical polymerization, the unregulated thickness and certain technical issues, though, and they must be fixed. It
density of PA membranes' surface modification layers would has been discovered that surface engineering (functionali-
rise, drastically reducing their water permeability (Zhu zation) using organic polymers and functional groups like
et al., 2015). -OH, -COOH, and -NH2 increases the stability and adsorption
Fig. 19 shows the performance of NF membrane in Tables capacity of heavy metals. When used as a cross-linker or
6 and 7 for Cu2+, Zn2+, Ni2+, and Pb2+ based on membranes grafting agent, PEG, PDA, PAA, PAMAM, EDA, and other
with positively and negatively charged surfaces. As shown, substances create membrane porosities and adsorption sites.
the positive surface membrane has greater permeance than As the size, porosity, and surface area increase, so does the
the negative surface membrane. Negatively charged mem- adsorption of pollutants. These membranes have a range of
branes are less effective in removing heavy metals because 77–99% elimination effectiveness. However, the fundamental
of the Donnan effect, which causes them to reject multi- issues with polymeric membranes have been resolved along
valent anions more strongly than multivalent cations (Wu with enhanced removal efficiencies of up to 100% by cleverly
et al., 2016). Thus, it is advantageous to create a positively using organic, inorganic, and hybrid nanofillers. Although
charged NF membrane for the elimination of heavy metal the creation of highly efficient NF membranes for water
ions. Also, the high surface charge density of the membranes treatment has shown that the use of organic, inorganic, and
makes them susceptible to fouling by counterions and sus- hybrid nanofillers as an addition to the host membrane
pended colloids during filtering. Heavy metals may be effi- matrix is very beneficial, they may also be the cause of the
ciently removed from water using NF membranes that following adverse effects:
include a separation layer comprised of a negatively charged
upper layer and a positively charged underlayer. This is a • The presence of nanoparticles can impede the flow of
positive point to reduce membrane fouling as well as the water.
removal of heavy metal ions. • Inadequate interaction between polymer and nano-
particles may result in the creation of flaws and non-se-
lective pores, lowering the selectivity.
5. Challenge and future perspective
• The antifouling abilities of membranes may be diminished
if biofilms form on their surface.
Enhancing the rejection capacity of NF is receiving more
• The polymer chain packing may be reduced if nano-
focus, which has been made possible in large part by the particles are present in the matrix of the polymer.
multiple benefits of tailored nanomaterials, such as their
• Low separation performance will result from nanoparticle
high adsorption capacity, selectivity, and quick removal ki- deposition and agglomeration on the membrane surface
netics of heavy metals in water and wastewater. There are
 Chemical Engineering Research and Design 189 (2023) 530–571 559

or inside the membrane due to poor nanoparticle disper- capability of the novel techniques of NF membrane fabri-
sion in the polymer matrix. cation and nanofiller materials listed in Tables 6 and 7. It is
important to note that the separation efficiency of mem-
By maximizing the number of variables involved in the brane processes is dependent on both operating environ-
production of NF membranes, it is a significant task to re- ment and membrane properties.
solve the aforementioned issues. The potential ability of NF
polymeric membranes to separate various heavy metal ions, The investigations are currently limited to the laboratory
such as Cd2+, Hg2+, Pb2+, Ni2+, Cu2+, Al2+, Co2+, Zn2+, Mn2+, and stage, thus more thorough studies at the scale of the entire
Cr4+ from water resources is typically considered to be en- industry are required. Additionally, the most crucial element
hanced by proper systematic membrane synthesis, surface for industrial applications is the cost of the materials, which
modification via IP and grafting, and addition of nanofillers to is higher in the case of coating nanomaterials that can be
their structure. Given the present global need for clean water corrected by recycling agricultural waste to create carbon-
scarcity, this review has provided a clear understanding of based nanomaterials or using a variety of accessible, low-
the advantages of incorporating nanofiller onto NF polymeric cost local natural materials. Other issues include the destiny
membranes for the separation and removal of a wide spec- of NF membranes and their potential for reuse. Researchers
trum of heavy metal ions. The research community is likely are currently concerned about the proposed nanofillers'
to continue looking for new hybrid materials that could not toxicity. In this direction, it is important to place a focus on
only overcome the shortcomings (such as permeation and using biopolymers and green chemistry to create nanoma-
retention rates) of NF polymeric membranes but also physi- terials. So, in terms of removal effectiveness, selectivity,
cochemical properties (such as mechanical, chemical, and toxicity, separation, and reusability, a nanocomposite of
thermal stability). This is based on the current findings of tailored metal oxides with organic, inorganic, or biomaterials
this review, as well as the current developments works, and may offer a superior option.
efforts in developing new NF membrane material. To sum up,
the following suggestions are provided for new researchers
planning their research to increase the effectiveness of NF 6. Conclusion
membranes for the removal of heavy metals:
As, Cd, Cr, Cu, Ni, Zn, Pb, Hg, and Ag are the most dangerous
• The first step for researchers is to pinpoint candidate heavy metals that can be detected in wastewater. Many ex-
polymers with high enough removal efficiencies. This al- periments were carried out by researchers to remove heavy
lows for the planning and direction of additional research metals from water using conventional water treatment
based on the primary barrier and weakness of pure techniques. Although many techniques, including RO, NF,
polymers. UF, MF, electrochemical, and adsorptions, have been estab-
• When discussing the incorporation of nanomaterials into lished, there is no definitive review that addresses the
polymers, it is essential to note that such inorganic phases modification of the NF membrane to remove heavy metals.
must be embedded intelligently, taking into account two This review article offers information about NF membranes,
crucial factors: 1) the physicochemical properties of the preparations, advancements, benefits, drawbacks, and ap-
nanomaterials (stability, porosity, morphology, etc.), and plications. The most crucial finding is that NF membranes
ii) their metal uptake mechanisms related to the removal might be a fascinating area of research. To overcome those
of heavy metals (adsorption, sieving, size-exclusion, etc.). obstacles or constraints, however, so that these membranes
Such fundamental analysis will yield substantial im- can have an impact on the wastewater treatment proce-
provements in less time and with fewer resources, i.e., dures, there are still a lot of things to be done. It was dis-
minimal filler loading may enhance the characteristics of covered that by carefully integrating organic, inorganic, and
polymer membranes through synergistic effects. hybrid nanofillers into polymer membranes, high percentage
• The resulting separation efficiency in membranes is sig- of the heavy metals could be removed. Out of all the NF
nificantly influenced by the membrane preparation pro- membranes that have been introduced, the B-Cur/PES, GO-
cesses. Even though the majority of the field's PAMAM/PES, and Ti3C2TX/EDA composite-based membranes
advancements have been attributed to the characteristics that use organic, inorganic, and hybrid nanofillers to modify
of nanomaterials, it is important to note that the in- the NF membrane have higher potential than the others
vestigation of novel methods for fabricating membranes, because they, respectively, chelate heavy metals in poly-
along with the advancement of current ones, will enable electrolytes, have a wealth of hydrophilic functional groups,
the tailoring of membranes that are significantly im- and combine metallic and organic linkers. Most of the para-
proved. meters, including water permeability, fouling, reusability,
• Although many studies have demonstrated the effective- toxicity, and stability, depend on the synthesis methods and
ness of membranes in separating heavy metal ions, there materials used to create this membrane, and fine-tuning the
is currently a dearth of evidence demonstrating the sus- membrane building elements is a procedure that will likely
tainability of these systems over the long term. Extending become more common in the future.
membrane testing will help chemical engineers better
comprehend membranes' potential for practical applica-
tions. Declaration of Competing Interest
• To summarise, it is advised for new scientists to in-
vestigate the applicability of such new materials and The authors declare that they have no known competing fi-
methods to NF membrane processes for the removal of nancial interests or personal relationships that could have
heavy metal ions based on the pertinent insights and appeared to influence the work reported in this paper.
560 Chemical Engineering Research and Design 189 (2023) 530–571

Acknowledgements Surface Texture: Surface Roughness, Waviness and Lay. Amer

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