LDHs

Science of the Total Environment 912 (2024) 169160
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Science of the Total Environment

journal homepage: www.elsevier.com/locate/scitotenv
Review
Progress in layered double hydroxides (LDHs): Synthesis and application in

adsorption, catalysis and photoreduction
Ahmad Farhan a, Aman Khalid a, Nimra Maqsood b, Sidra Iftekhar c,
Hafiz Muhammad Adeel Sharif d, Fei Qi e, Mika Sillanpää f, g, h, Muhammad Bilal Asif i, *
a
Department of Chemistry, University of Agriculture Faisalabad, Faisalabad, Pakistan
b
Department of Chemistry, University of Science and Technology, Hefei, China
c
Department of Applied Physics, University of Eastern Finland, Kuopio, Finland
d
Research Center for Eco-Environmental Engineering, Dongguan University of Technology, Dongguan, China
e
Beijing Key Lab for Source Control Technology of Water Pollution, College of Environmental Science and Engineering, Beijing Forestry University, Beijing, China
f
Department of Chemical Engineering, School of Mining, Metallurgy and Chemical Engineering, University of Johannesburg, Doornfontein, South Africa
g
Sustainability Cluster, School of Advanced Engineering, UPES, Bidholi, Dehradun, Uttarakhand, India
h
Department of Civil Engineering, University Centre for Research & Development, Chandigarh University, Gharuan, Mohali, Punjab, India
i
Advanced Membranes and Porous Materials Center (AMPMC), Physical Sciences and Engineering (PSE), King Abdullah University of Science and Technology (KAUST),
Thuwal, Saudi Arabia
H I G H L I G H T S G R A P H I C A L A B S T R A C T
• Layered double hydroxides (LDHs) show

promise in environmental remediation.
• Functionalisation of LDHs improves
their adsorption, catalytic and cyclic
performance.
• Removal mechanisms include adsorp
tion, electrostatic interaction, complex
ation, and degradation.
• LDH application in catalysis should be
preferred over non-destructive adsorp
tion process.
• Challenges faced by LDH-based com
posites for scale-up are highlighted and
discussed.
A R T I C L E I N F O A B S T R A C T
Editor: Huu Hao Ngo Layered double hydroxides (LDHs), also known as anionic clays, have attracted significant attention in energy
and environmental applications due to their exceptional physicochemical properties. These materials possess a
Keywords: unique structure with surface hydroxyl groups, tunable properties, and high stability, making them highly
LDHs desirable. In this review, the synthesis and functionalization of LDHs have been explored including co-
Heterogenous catalysis precipitation and hydrothermal methods. Furthermore, extensive research on LDH application in toxic
Water treatment
* Corresponding author.
E-mail address: muhammad.asif@kaust.edu.sa (M.B. Asif).
https://doi.org/10.1016/j.scitotenv.2023.169160
Received 30 September 2023; Received in revised form 23 November 2023; Accepted 5 December 2023
Available online 10 December 2023
0048-9697/© 2023 Elsevier B.V. All rights reserved.
A. Farhan et al. Science of the Total Environment 912 (2024) 169160
Toxicity pollutant removal has shown that modifying or functionalizing LDHs using materials such as activated carbon,
Heavy metals polymers, and inorganics is crucial for achieving efficient pollutant adsorption, improved cyclic performance, as
Removal mechanisms well as effective catalytic oxidation of organics and photoreduction. This study offers a comprehensive overview
of the progress made in the field of LDHs and LDH-based composites for water and wastewater treatment. It
critically discusses and explains both direct and indirect synthesis and modification techniques, highlighting
their advantages and disadvantages. Additionally, this review critically discusses and explains the potential of
LDH-based composites as absorbents. Importantly, it focuses on the capability of LDH and LDH-based composites
in heterogeneous catalysis, including the Fenton reaction, Fenton-like reactions, photocatalysis, and photore
duction, for the removal of organic dyes, organic micropollutants, and heavy metals. The mechanisms involved
in pollutant removal, such as adsorption, electrostatic interaction, complexation, and degradation, are thor
oughly explained. Finally, this study outlines future research directions in the field.
1. Introduction focused on synthetic and functionalization of LDHs, as well as adsorp

tion or catalytic processes. This necessitates a review article that
Water is a vital resource that underpins all human activities. Each comprehensively and critically evaluate LDH for the remediation of
day, vast amounts of wastewater are generated in households, com toxic pollutants. Herein, structure and synthesis methods of LDH-based
mercial establishments, and agricultural operations due to the ever- nanocomposites and their use as adsorbents and heterogenous catalyst
increasing human population. Unfortunately, despite this surge in are analysed. Various approaches and ideas for enhancing the efficiency
wastewater production, the availability of freshwater remains insuffi of the LDH-based adsorbents and catalysts have been discussed,
cient to satisfy the needs of rapidly expanding population. Conse including changing the support material and functionalization. Impor
quently, intense competition and inequitable distribution of the limited tantly, LDH regeneration to maintain their efficiency after repeated
freshwater resources persist among various sectors (Bozorg-Haddad cycles has been explored. Finally, future research directions are outlined
et al., 2020; Salehi, 2022). It is to be noted that industries consume vast to scale-up LDH in water and wastewater treatment.
amounts of water to meet their needs, but this practice also leads to
environmental pollution. The wastewater they release into lakes, 2. Structure of layered double hydroxide
streams, and rivers is heavily contaminated with toxic pollutants such as
heavy metals and organic dyes (Cheng et al., 2022; Farhan et al., 2023a). Layered double hydroxides (LDHs) are basically 2D anionic lamellar
Industrial wastewater negatively impact different environmental sys structures composed of metal hydroxide octahedral units, resembling
tems viz. terrestrial and aquatic ecosystems. Some common heavy brucite-like layers (Fig. 1). LDHs, also known as anionic clays, exhibit
metals found in wastewater, such as Cd2+, Pb2+, and Hg2+, are non- high ion exchange capacity, a large surface area, a porous structure, and
biodegradable, and pose significant risks (Farhan et al., 2023c; notable thermal stability (Han et al., 2023). These layered materials
Mathew et al., 2016). Additionally, organic dyes in the environment are have garnered significant attention across various fields, including
both carcinogenic and mutagenic, and the discharge of untreated dye adsorption, catalysis, photocatalysis, electrochemistry, biomedical
containing wastewater puts all the aquatic ecosystem at risk. Therefore, research, magnetization, and polymerization (Ahmed and Mohamed,
it is crucial to confront this issue by implementing effective methods for 2023; Dong et al., 2022; Karim et al., 2022; Mohapatra and Parida,
the treatment of wastewater before it is released into water bodies 2016; Rohit et al., 2021). LDHs are represented by the following general
(Ahmed and Mohamed, 2023; Asif et al., 2020; Chen et al., 2021b; chemical formula: [M(II)1− x M(III)x (OH)2]x+ (An− )x/n mH2O. In this
Farhan et al., 2023b). formula, M(II) and M(III) indicate divalent and trivalent metal cations.
Layered double hydroxide (LDH), which is a two-dimensional (2D) The divalent metal and trivalent cations that can be used in LDHs syn
clay-like material, has increasingly been investigated as an adsorbant or thesis are Mg2+, Ca2+, Ni2+, Cu2+, Zn2+, Al3+, Fe3+, Cr3+, Ga3+, and
a heterogenous catalyst for environmental remediation including the Mn3+. Additionally, the term A indicates the interlayer inorganic or
removal of heavy metals and organic dyes from complex water matrices. organic anion and x indicates the molar ratio (He et al., 2023b).
The discovery of hydrotalcite, a natural form of LDH, can be traced back Sometimes divalent and trivalent metals can be substituted by mono
to 1842. In 1942, the first LDHs were developed, along with the intro valent and tetravalent metals. One of the interesting features of LDH is
duction of the concept of double sheet synthesis (Feitknecht and Gerber, their tailored properties by just changing the metal composition and
1942). LDHs have gained significant attention due to their unique type. LDHs, serving as an emerging type of metal-to-metal charge-
frameworks and features, prompting thorough investigations of their transfer framework, have recently been used as heterogenous catalyst in
potential applications in energy and environmental applications. The processes like water electrolysis, nitrogen fixation, and reduction of
distinctive properties of LDHs, such as interlayer space, interchangeable carbon dioxide because of their readily tunable metal cation composi
guest anions, and large specific surface areas, facilitate the effective tion (Ning et al., 2021). Furthermore, the dispersion of active substances
removal of a wide range of pollutants, making LDH applicable to various within the laminate not only serves to modify the LDH band structure,
environmental conservation efforts (Dong et al., 2022). To date, various thus improving the utilization of sunlight, but also leads to the creation
synthesis methods have been employed for preparing LDH-based of unsaturated defective sites, thereby enhancing catalytic efficiency (Li
nanocomposites, each yielding unique structural features and proper et al., 2020a).
ties (Zhao et al., 2023b). Extensive research efforts have been devoted to
use the LDHs in the removal of heavy metals (Bi et al., 2022; Ling et al., 3. Synthesis and functionalization of layered double hydroxide
2023) and organic dyes (Ahmad et al., 2023; Mallakpour et al., 2023) via
adsorption (Gao et al., 2023; Santamaría et al., 2023; Whittaker et al., Several synthetic methods such as co-precipitation, hydrothermal,
2023), as well as catalytic oxidation or reduction (Bian et al., 2021; Li and sol-gel have been studied and reported for LDH development (Karim
et al., 2023a; Vasseghian et al., 2023). et al., 2022; Mittal, 2021). Pure LDHs may lack functional groups and
This state-of-the-art review examines the current progress of LDH for structural components, limiting their activity and efficacy in environ
different environmental applications, particularly adsorption and mental applications. In this context, functionalized LDHs have been
catalysis. Several excellent review articles have been published in recent developed by including new functional groups or structural components
years (Ahmed and Mohamed, 2023; Dong et al., 2022; Karim et al., to address these shortcomings. In order to create and produce new,
2022; Mohapatra and Parida, 2016; Rohit et al., 2021), which have been highly functioning LDHs-based nanocomposites, modifications to LDHs
2
have been recommended. In this section, several routes to LDH synthesis rapid dissolution of hydroxide precipitates, leading to the formation of
have been critically reviewed and their implications in environmental well-defined crystalline structure. Additionally, incorporating the hy
application are elucidated. For the ease of readers, this section firstly drothermal process into other synthesis methods enhances their effec
discusses direct synthesis of LDH followed by indirect synthesis tiveness, resulting in larger particles with improved purity and
techniques. crystallinity. The synthesis conditions, including the temperature and
duration of the hydrothermal treatment, play a crucial role in deter
3.1. Direct synthesis of LDHs mining the crystallinity of LDHs. In cases where low-affinity foreign
organo-anions need to be incorporated into the interlayers, the hydro
3.1.1. Co-precipitation method thermal method is particularly suitable. It is to be noted that the hy
The most widely used method for synthesizing LDHs is co- drothermal technique is highly regarded for its fundamental chemical
precipitation, which involves combining solutions of di, tri and tetra reactions and straightforward operation, making it a lucrative technol
valent metal salts in water followed by addition of an alkaline solution ogy. This process involves mixing metal salts and precipitating agents in
and raising the pH, which leads to the co-precipitation of LDH. However, an autoclave containing a solvent, followed by subjecting the solution to
this approach may result in the incorporation of counterproductive thermal treatment at a specific temperature (above 100 ◦ C). Pre
hydroxide ions within the interlayer or on the outer layer of LDH cipitators such as sodium hydroxide, sodium carbonate, ammonia, urea,
(Auerbach et al., 2004; Evans and Duan, 2006). The incorporation of and methanol are commonly used in this method. Previously, Zhang
carbonate ions within the layers, resulting from the dissolution of et al. (2022) successfully utilized the hydrothermal method to fabricate
ambient CO2 in the solution, poses the most challenging aspect of LDH CaAl-LDH. They dissolved calcium nitrate tetrahydrate and aluminum
synthesis. To mitigate this, the reaction must take place under inert nitrate nonahydrate in a sodium nitrate solution, which was then placed
conditions, such as N2. Experimental conditions can selectively facilitate in an autoclave reactor for 36 h at 100 ◦ C. After centrifugation, the
the insertion of interlamellar anions. Key parameters include the tem mixture was dried at 60 ◦ C to obtain CaAl-LDH for the removal of Cu(II)
perature of the reactor, concentration of the alkaline solution, pH of the and Cd(II) (Zhang et al., 2022). In another study, Tian et al. (2020)
reaction media, flow rate of the reactants, concentration of the metallic demonstrated the efficacy of a one-pot hydrothermal method for syn
salt solutions, and the age of the precipitate (Gu et al., 2015). The co- thesizing NiFe-LDH by combining iron nitrate hexahydrate, nickel ni
precipitation method offers several advantages, including high yield, trate hexahydrate, and urea. The solution was subsequently placed in an
one-step synthesis, crystalline LDHs, and high overall purity. A summary autoclave and treated at 120 ◦ C for 10 h to obtain the corresponding
of direct synthetic routes to LDH is presented in Table 1. LDH (Tian et al., 2020). Similarly, Abbasi et al. (2021) reported the
In 2017, Abdellaoui et al. (2017) successfully synthesized MgAl-LDH fabrication of MnFe-LDH/ polyethersulfone (PES) composite membrane.
by utilizing nitrate as the interlayer anion by gradually adding NaOH to The PES membrane was introduced into solution containing 1:1 Mn2+/
a 2:1 Mg:Al solution under N2 to prevent carbonate contamination Fe3+ to achieve a grass-like structured MnFe-LDH/PES composite
(Abdellaoui et al., 2017). In 2020, Shi et al. (2020) synthesized various membrane. The mixture underwent treatment at 90 ◦ C for 25 h, followed
LDHs by combining ZnCl2 or MnCl2 or MgCl2 with FeCl3 in different by multiple washes with water and drying for 6 h at 60 ◦ C (Abbasi et al.,
molar ratios of 1:1, 2:1, 3:1, 4:1, and 5:1 (Shi et al., 2020). Bessaha et al. 2021).
(2017) achieved the synthesis of ZnAl-LDH by carefully adding Na2CO3 In this method, urea is used as an agent for precipitation, facilitating
and NaOH drop by drop to metal salt aqueous solutions. They success homogeneous precipitation and control over crystallite dimensions and
fully produced ZnAl-LDH with varying cationic fractions (3,1 and 4,1) size, which significantly improves the crystallinity of the product.
while keeping the pH level consistently at 7.5 (Bessaha et al., 2017). In Additionally, the gradual decomposition of urea produces an alkaline
order to eliminate any residual intercalated chloride ions, produced LDH pH necessary for LDH precipitation, along with lamellar hydroxyls and
was centrifuged, rinsed in deionized water, and dried for 12 h at 100 ◦ C interlayer carbonate anions. In the urea hydrolysis method, urea, and a
(Mittal, 2021) (Fig. 2). solution of precursor salts (e.g., chlorides, hydroxides, nitrates, or sul
fates) are often combined in an autoclave reactor. The mixture is then
3.1.2. Hydrothermal method heated to the appropriate temperature for a specific duration. The
This method is a widely used technique in the synthesis of LDHs. It resulting precipitates are collected through filtration, thoroughly
has been extensively studied and proven to be efficient in promoting the washed with water, and left to dry overnight. This approach offers the
Fig. 1. A schematic representation of LDH structure (Gao et al., 2014).
3
Table 1
Direct synthesis of LDH using Co-precipitation, hydrothermal, microwave irradiation, urea-assisted hydrolysis, and sol-gel methods.
LDH Precursors Molar Ratio Synthesis Operating conditions pH Application Toxic pollutants Ref.
method
ZnCr-LDH Zn(OH)2 2:1 Co- Slurry heated at 90 ◦ C for 6 h 6 Adsorption Pyrophosphate (Fu et al.,
Cr(OH)3 precipitation and then separated by 2021)
centrifugation. The
precipitates were filtered,
dried overnight.
S-MgA-LDH Mg 0.17:0.03:0.12 Co- Mixture was heated at 90 ◦ C 9.5–10.5 Adsorption Anionic dyes (Grover et al.,
(NO3)2⋅6H2O precipitation for 24 h. Final product was 2022)
Al(NO3)3⋅9H2O washed, and then dried at
Starch 50 ◦ C for 24 h.
ZnAlCe-LDH Zn(NO3)2 NA Co- Nitrogen atmosphere was 10 Anti-corrosive (Liu et al.,
Al(NO3)3 precipitation used. Slurry was aged for 18 coating 2015)
Ce(NO3)3 h at 65 ◦ C. Final product was
washed and dried for 12 h at
60 ◦ C.
Fe@MgAl- FeCl3⋅6H2O NA Co- Slurry was aged for 1 h. Final 11 Adsorption 4-Nonylphenol, 4- (Zhou et al.,
LDH Mg(NO3)2 precipitation product was then washed, octylphenol, and 2017)
Al(NO3)3⋅9H2O and dried at 50 ◦ C. Bisphenol A
CuZnAl-LDH Cu(NO3)2 13.86:77.94:30.6 Co- Precipitates were dried at 8 CO oxidation (Gonçalves
Zn(NO3)2 precipitation 80 ◦ C. et al., 2023)
Al(NO3)3
ZnAl-LDH γ-Al2O3 NA Urea The precursor was mixed NA Substrate (Liu et al.,
Zn(NO3)2⋅6H2O hydrolysis with urea. By increasing modifier 2014)
Urea temperature, urea
hydrolyzed into CO2 and
NH3
MgCoAl- Co(NO3)2⋅6H2O 1:3 Urea Mixture was heated for 24 h 7 Catalyst support (Chagas
LDH Al(NO3)2⋅9H2O hydrolysis at 120 ◦ C. Final product was et al., 2015)
NiCoAl- Mg dried at 120 ◦ C for 20 h.
LDH (NO3)2⋅6H2O
Ni(NO3)2⋅6H2O
Urea
MgAl- LDH Mg 2:1 Urea Solutions were kept for 48 h NA Thermal stability (Naseem
MgFeAl- (NO3)2⋅6H2O hydrolysis at 100 ◦ C. Final products et al., 2019)
LDH Al(NO3)3⋅9H2O were dried at 70 ◦ C for 24 h.
MgCoAl- Fe(NO3)3⋅9H2O
LDH Co(NO3)2⋅6H2O
MgCuAl- Cu(NO3)2⋅3H2O
LDH Zn(NO3)2⋅6H2O
MgZnAl- Ni(NO3)2⋅6H2O
LDH
MgNiAl-
LDH
NiMgAl- NiSO4 1:1:1:6 Hydrothermal Mixture was heated at NA Adsorption Congo red (Lei et al.,
LDH MgSO4 180 ◦ C for 6 h. Precipitates Cr(VI) 2017)
Al(NO3)3 were washed and dried at
Urea 80 ◦ C for 12 h.
ZnIn-LDH Zn(NO3)2⋅6H2O 3:1 Microwave The mixture was kept in NA Photocatalysis Methylene blue (Liu et al.,
In irradiation microwave at 150 ◦ C for 2 h. 2020)
(NO3)3⋅4.5H2O Precipitates were
Urea centrifuged, and then dried
at 70 ◦ C for 12 h.
MgAl-LDH Mg 2:1 Hydrothermal The mixture was kept in 10 Adsorption Arsenate and (Jung et al.,
(NO3)2⋅6H2O autoclave and heated for 24 phosphate 2021)
Al(NO3)3⋅9H2O h at 210 ◦ C. The product was
rinsed and dried at 80 ◦ C.
CoAl-LDH Co(NO3)2⋅6H2O 2:1 Hydrothermal The mixture was kept at 10 Catalytic Ranitidine (Asif et al.,
Al(NO3)3⋅9H2O 130 ◦ C for 16 h, and dried at membrane 2022)
60 ◦ C.
ZnNiCr-LDH Zn(NO3)2⋅3H2O (Zn2+Ni2+)/Cr3+ Hydrothermal The mixture was kept in 7 Adsorption Cr(VI) (Guo et al.,
Ni(NO3)2⋅6H2O 3:1 oven and heated at 100 ◦ C 2021)
Cr(NO3)3⋅6H2O for 2 h. The sample was
centrifuged and dried at
80 ◦ C for 12 h.
CaAl-LDH Ca(NO3)2⋅4H2O 0.03:0.008 Hydrothermal The mixture was kept in 11 Adsorption Cd(II) and Ca(II) (Zhang et al.,
Al(NO3)3⋅9H2O autoclave and treated at 2022)
100 ◦ C for 36 h.
NiAl-LDH Ni(acac)2 3:1 Sol-gel Solutions were mixed and 8 Thermal (Saikia et al.,
Al(acac)3 treated at 80 ◦ C for 2 h. degradation 2017)
Mg2− xMx/ Mg NA Sol-gel Gel precursors were dried at 10 NA NA (Valeikiene
Al1 LDH (NO3)2⋅6H2O 105 ◦ C for 24 h. et al., 2020)
(M = Sr, Al(NO3)3⋅9H2O
Ca, Ba) Sr(NO3)2
(continued on next page)
4
Table 1 (continued )
LDH Precursors Molar Ratio Synthesis Operating conditions pH Application Toxic pollutants Ref.
method
Ca(NO3)2⋅4H2O
Ba(NO3)2
MgFe-LDH Mg(NO3)2 Fe NA Sol-gel Gel was filtered and final 9.2 Adsorption Indigo carmine (Ahmed and
(NO3)2 product was dried at 100 ◦ C Mohamed,
Cetrimonium for 1 d. 2017)
bromide
CaAl-LDH Ca(OMe)2 2:1 Sol-gel Gel was stirred at ambient 13 NA NA (Muráth
MgAl-LDH Mg(OEt)2 temperature for 3 days. et al., 2019)
Al(OEt)3 Ageing of gel was performed
at 20 to 60 ◦ C for a week.
Mg3-xMx/ Mg NA Sol-gel Gel was dried at 105 ◦ C for 12 Substitution (Valeikiene
Al1-LDH (NO3)2⋅6H2O 24 h. effect of et al., 2019)
(M: Co, Al(NO3)3⋅9H2O transition metals
Cu, Ni, Zn, Co(NO3)2⋅6H2O
Mn) Cu(NO3)2⋅3H2O
Ni(NO3)2⋅6H2O
Zn(NO3)2⋅6H2O
Mn
(NO3)2⋅4H2O
Fig. 2. A generic route to the synthesis of crystalline LDH.
advantages of controlled particle dimensions, morphology, and the resulting in structural species that act as precursors for the unit cell with
absence of competing anions other than hydroxides (Herrera et al., perforated crystalline structure. The unit cell then grows in various di
2008). Using the urea hydrolysis method, Grover et al. (2022) produced mensions due to the nucleation process influenced by microwave irra
ZnAl-LDH by combining AlCl3, ZnCl2, and urea. The mixture was diation. Utilizing microwave irradiation is highly efficient for
refluxed at 100 ◦ C for 7 h under stirring at 350 rpm using a magnetic manufacturing organic LDH in an appropriate solvent, as it offers
stirrer. After reflux, the contents were stirred at 60 rpm for 4 h. The excellent control and minimal heat loss. Moreover, this approach boasts
resulting LDH was obtained, washed with water and ethanol, and dried a faster reaction time compared to conventional methods such as co-
for 16 h at 60 ◦ C (Grover et al., 2022). Another example is the synthesis precipitation. Liu et al. (2020) prepared ZnIn-LDH using microwave
of MgNiAl-LDH, where MgSO4, Al(NO3)3, NiSO4, and urea were utilized assisted hydrothermal method using different molar ratios of metal ions
in a molar ratio of 1:1:1:6. The mixture was stirred for an hour before (Zn2+/In3+) (Liu et al., 2020). In another study, Qiu et al. (2020) syn
being placed in a stainless-steel autoclave. It was then held at 180 ◦ C for thesized histidine-functionalized graphene quantum dots/Ni-Co LDH by
6 h before cooling to room temperature. After separate centrifugation, microwave irradiation method by mixing Ni/Co salt with urea in ethane-
the product was rinsed five times with ethanol and water, followed by 1,2-diol solvent and then stirred for 24 h. The homogeneous mixture was
drying for 12 h at 80 ◦ C (Lei et al., 2017; Zhou et al., 2017). kept in microwave synthesizer at 190 ◦ C to obtain resultant LDH (Qiu
et al., 2020).
3.1.3. Microwave irradiation
The microwave-assisted approach has been shown to be an accessible 3.1.4. Sol-gel method
and straightforward method for synthesizing LDH as the microwave This method involves the physical components of a reaction, where
radiation can impact kinetics, selectivity, and the nucleation stage. In metallic substrates are commonly used, although acetates and acetyla
this process, an amorphous gel forms in a suitable solution with OH− , cetonates are occasionally employed. The alkoxides are dispersed in an
5
organic solvent, followed by the hydrolysis of the alkoxides, resulting in oxides or layered double oxides (LDO) (Asif et al., 2023). Calcination
the formation of a sol, which then undergoes incomplete condensation enhances the surface area and creates chemically and thermally durable
of the metallic precursor, leading to the creation of a colloidal gel materials with increased active sites (Karim et al., 2022; Mohapatra and
through internal cross-linking. The properties of the resulting solid LDH Parida, 2016). By using de‑carbonated water to minimize CO2− 3
can be modified by adjusting the rate of condensation or hydrolysis of contamination, the resulting calcined LDH can be dissolved in an anionic
the metallic precursors, along with other factors such as pH, tempera solution, leading to the formation of LDH with the desired anion.
ture, and solvent type. The LDH produced using this method exhibits However, factors such as time, calcination temperature, and heating rate
high purity, a large surface area, and specific pore size (Tichit et al., influence the structural recovery of LDH. The “memory effect” refers to
2005). Ahmed and Mohamed (2017) used this technique to prepare the process of restoring the layered structure after thermal degradation,
MgFe-LDH by combining appropriate proportions of ferric and magne as illustrated in Fig. 3. In a previous study, MgAl-Cl-LDH was synthe
sium nitrates and stirring continuously for an hour. After adding cetyl sized using the co-precipitation method, followed by a 5 h heating at
trimethylammonium bromide above the critical micelle concentration 550 ◦ C. After calcination, the resulting LDO was treated with a sodium
(CMC), NaOH was added resulting in formation of brown precipitate, dodecyl sulphate (SDS) solution and stored for 2 d. Subsequently, the
which was agitated allowing the sol to age for 2 d for gel formation. The LDH-SDS suspension was subjected to thorough centrifugation, followed
gel particles were then obtained through filtration, cleaned, and dried at by five rinses to obtain crystalline product (Aşçı, 2017). Regeneration of
100 ◦ C for 1 d (Ahmed and Mohamed, 2017). the baked LDH could be accomplished by mixing it with an SDS solution
Commonly used methods include co-precipitation, hydrothermal in CO2-free deionized water, and the resulting suspension was stirred at
methods, sol-gel methods, and microwave irradiation (Ahmed and room temperature for a day, resulting in the formation of LDH (Mittal,
Mohamed, 2023; Dong et al., 2022; Karim et al., 2022; Mohapatra and 2021).
Parida, 2016; Rohit et al., 2021). These methods have advantages and Hybrids and composites based on LDHs have been created utilizing a
disadvantages. For example, the coprecipitation method is cost- variety of ingredients, such as carbon nanostructures (Mittal, 2021).
effective, rapid, scalable, and involves simple steps and equipment. Using either hard or soft models, LDHs produced through co-
However, it does not provide effective control over the morphology of precipitation can also create grass-like morphologies by combining hy
LDH. In the case of the hydrothermal method, the large-scale synthesis drothermal processes with surfactants. Soft patterning agents are
of LDHs can be conducted with effective control over their crystallinity organic molecules that strongly interact with the inorganic growth on
and morphology, but at the expense of time and energy. The sol-gel them. In this context, SDS is a popular soft templating medium due to its
method allows for the synthesis of nanostructured films and powders structure-directing properties. The amount of SDS used is crucial in
with poor crystallinity over a short synthesis time. On the other hand, determining the morphology. A 0.005 M produces a rose blossom ge
although this could be an energy intensive process, microwave irradia ometry, while a concentration of 0.02 M forms a sphere (Boccalon et al.,
tion is suitable for obtaining crystalline LDHs with high purity. The se 2020; Zhang et al., 2015). As the concentration approaches the CMC, the
lection of the method to be used for LDH synthesis may depend on the size of the petals decreases while the number of petals increases, even
available resources and intended properties of the LDHs. tually leading to their union. This procedure involves dispersing the
reactants thoroughly with ultrasonic vibration for 30–60 min, followed
3.2. Indirect synthesis and regeneration of LDHs by mixing them with clean water at a molar ratio of approximately
1:2:10 (M3+: M2+: Urea). The solution is then heated for 6 h at 200 ◦ C in
When LDH is heated to 400–600 ◦ C in an inert environment, the a 100 mL autoclave. After four rounds of rinsing with ethanol, the final
intercalated water and carbonate ions are lost, resulting in the formation product is dried for 6 h at 80 ◦ C (Almoisheer et al., 2019; Li et al., 2020b;
of a combined metal oxide known as calcined LDH or layered metal Pourfaraj et al., 2017; Shamsayei et al., 2018; Starukh and Levytska,
Fig. 3. A schematic representation of ‘memory effect’ for LDH regeneration. This generic schematic is prepared based on the reported literature.
6
2019; Zhang et al., 2020b; Zong et al., 2018). In a recent study, re approach is highly efficient because it may be completed within a few
searchers dissolved Mg(NO3)2⋅6H2O, Al(NO3)3⋅9H2O, hexamethylene- minutes at ambient temperature. Furthermore, a wide range of
tetramine, and SDS in deionized water to create ultrathin dodecyl- conductive substrates can effectively anchor NiLa-LDH NSAs. This pro
sulfate intercalated MgAl-LDH nanosheets. To encourage crystalliza cess can also be scaled up to accommodate substrates with high surface
tion, the solution was heated to 140 ◦ C for 24 h in autoclave (Lei et al., areas (Jiang et al., 2019).
2020). Similarly, in 2017, researchers used polyvinylidene fluoride Another lab-scale, cost-effective, and efficient synthesis strategy was
(PVDF) nanofibers as a scaffold framework due to their mechanical developed to overcome the time and temperature problems associated
strength, excellent flexibility, and thermal stability. By employing with the co-precipitation method. A practical and exceptionally effective
ethanol, CoSO4⋅7H2O, Al2(SO4)3⋅18H2O, and urea, a PVDF fibrous method for synthesizing ZnAl-LDH with a hierarchical design and fast
membrane can be hydrolyzed to create PVDF@LDH composite fibers for kinetics has recently been reported (Liu et al., 2023). The building
oil and water separation (Lv et al., 2017). blocks or precursors used in the fabrication process included zinc oxide
The use of carbon nanostructures to synthesize LDH composites was and aluminum nitrate. This choice of ingredients helped to minimize the
reported several times. After calcining Zn–Al LDO nanosheets, Zn/Al- production of unwanted by-products. By leveraging the convenience
LDO@C was created by depositing extremely fine amorphous carbon and flexibility of this approach, a ZnAL-LDH with a 3D structure was
on ZnAl assembled double oxide nanosheets. ZnAl-LDH nanosheets with developed with a yield of 200 g per batch. The growth mechanism relies
a large surface area, which is specifically targeted due to abundant primarily on the combined effects of hydrolysis, dissolution, and
active sites, are created by the standard co-precipitation method. On the reconfiguration. Although some unreacted ZnO was present, it was
other hand, multi-walled carbon nanotubes (MWCNTs) have a signifi evident that crystalline ZnAl-LDH was effectively formed within 1 min,
cant specific surface area, excellent mechanical flexibility, and strong indicating an exceptionally rapid synthesis rate. When the reaction time
thermal or chemical stability. Consequently, calcination of LDH creates was increased to 5 min, the ZnO phase ceased to develop, forming a
ZnAl-LDO@C nanohybrids with a significant effective surface area and pristine crystal lattice of ZnAl-LDH. When the reaction time was
outstanding dispersion capability (Li et al., 2020b; Li et al., 2020c). extended to 2 h, there were insignificant alterations in the diffraction
Through electrostatic interaction between the two materials, Long et al. peaks with increasing crystallinity (Liu et al., 2023). Conventional
(2016) created composites consisting of negatively charged oxygenated synthetic approaches to adsorbents typically rely on expensive organic
MWCNTs and positively charged LDHs. After being exposed to HNO3, solvents or complicated preparation methods, thereby restricting their
MWCNT underwent a straightforward co-precipitation process in which practical application. To address this issue, a practical and eco-friendly
metal salts were added (Long et al., 2016). Another study reported the approach to develop MnAl–NO3–LDH was reported, which has the po
synthesis of CuAl-LDH and single walled carbon nanotubes (SWCNTs) tential for scale-up. The raw materials used for the preparation of LDH
using urea hydrolysis method (Almoisheer et al., 2019). By manipu included Ca(OH)2, Ca(NO3)2, and Al(OH)3, resulting in the formation of
lating the self-assembly process, a 3D categorized composite of LDH/ Ca4Al2(OH)12(NO3)24H2O. In contrast to traditional preparation
carbon sphere (CS) were prepared (Lyu et al., 2020). Employing a sol methods, all raw materials are converted into the final product without
vothermal approach using methanol as the source of solvent (as opposed the release of by-products (Zheng et al., 2023). Despite the synthesis of
to water) in an atmosphere of nitrogen, ZnAl-LDH were first prepared. LDH using these emerging methods, future studies should focus on their
The next step involved boiling a glucose solution in an autoclave to reliability and scalability.
create CS. Building a 3D LDH on CS was required in the third step of the
procedure, which started with LDH gel in methanol and was then 4. Application of pure and functionalized LDHs
coupled with a CS-methanol mixture. Finally, a hollow LDH structure
was created via calcination (Lyu et al., 2020). Our literature survey The section focuses on reviewing the progress in the application of
suggests that resultant nanocomposites prepared by combining LDH pure and functionalized LDH for toxic pollutant remediation (Fig. 4).
with other materials such as CNTs, and biochar exhibit exceptional
physicochemical properties including adsorption and catalytic activity. 4.1. LDH-based composites for adsorption
3.3. Other methods of LDH synthesis Adsorption is considered as an established method of water and
wastewater treatment. Adsorption mechanisms by LDH and LDH-based
Some emerging methods for the preparation of LDHs are discussed in composites include hydroxide precipitation, physical adsorption,
this section, including the electrosynthesis method, which is considered chemical bonding, and electrostatic attraction (Gong et al., 2011; Wu
a green, fast, and simple preparation method. For instance, Moradi et al. et al., 2011; Yang et al., 2013; Zhang et al., 2013). Various environ
(2023) developed a binder-free electrosynthesis method to create CoMn- mental factors affect the adsorption of toxic pollutants by LDH-based
LDH, which acted as a precursor to prepare Co–Mn based metal nanocomposites (Fig. 5a), while Fig. 5b shows different mechanisms
–organic frameworks (MOFs). MnCo-LDH nanosheets with a hierarchi of adsorption by LDHs.
cal structure were fabricated on a nickel foam substrate using a 3- The main classifications of dyes used to study the method of
electrode configuration consisting of an aqueous solution containing adsorption for eliminating dyes by LDH are anionic and cationic. LDH
Co(NO3)2⋅6H2O, Mn(NO3)2⋅4H2O, and KNO3, which served as the are regarded as superb contenders for engulfing anionic dyes (Kandisa
working, counter, and reference electrodes, respectively. The electrodes et al., 2016; Reish, 1996). The propensity of LDH to adsorb anionic dyes
were prepared with varying Co:Mn ratios while maintaining a total salt to cationic dyes is similar to that achieved by activated carbon (Abdel
concentration of 0.05 M and a KNO3 concentration of 0.3 M. The syn kader et al., 2011; Zaghouane-Boudiaf et al., 2012; Zhu et al., 2005).
thesis of CoMn-LDHs was conducted using chronoamperometry at a Fig. 6 demonstrates the mechanistic process for adsorption of methyl
fixed potential of − 1.0 V vs. Ag/AgCl for 400 s. Following the deposi orange (MO) happening on MgAl-LDH (nanocrystalline adsorbent)
tion, the electrodes were washed with deionized water and air-dried at modified using glycerol (Yao et al., 2017). Because of the metal ion
ambient temperature (Moradi et al., 2023). In another study, uniformly surface associations with the SO3 cluster along with hydrogen bonding,
structured NiLa-LDH nanosheet arrays (NSA) on a conductive substrate MO was effectively adsorbed by LDH (Sheng et al., 2016a; Sheng et al.,
were prepared using a simple and efficient electrosynthesis technique. 2016b; Wang and Chen, 2015). The presence of MO molecules on the
NiLa-LDH NSAs were formed on the working electrode by reducing an outer layers of adsorbents has been determined by complexation of
aqueous solution of the precursors. This reaction produces OH− ions, surface molecules and interaction with electrostatic forces (Chen et al.,
which facilitate the co-precipitation of Ni2+ and La3+. It is important to 2016; Sun et al., 2016). The adsorption isotherms connect the percent
note that the synthesis of NiLa-LDH NSAs using this electrosynthesis age of pollutants in the solution to the total quantity of solute adsorbed
7
Fig. 4. Applications of LDH-based composites for the removal of toxic pollutants from aqueous solutions.
Fig. 5. (a) Factors influencing the adsorption of toxic pollutants by LDH and LDH-based composites; and (b) a schematic representation of potential adsorption
mechanisms by LDHs.
8
Fig. 6. Mechanism of methyl orange (MO) adsorption by MgAl-LDH.
(eliminated) at equilibrium. The capability of adsorption has been alternative for characterizing and exploring heavy metal elimination by
determined using the isotherms. Solution phases (for example solid-gas LDH. The simulation results show that the anion MoS2− 4 functionalized
and solid-liquid) and processing variables such as starting pH, concen LDH is the most efficient adsorbent in removing heavy metals.
tration, and duration of contact have a significant impact on adsorption Furthermore, the negatively charged functional groups in LDH as well as
efficiency (Ahmed et al., 2012). Different kinetic approaches are tried to functional groups containing oxygen to Hg2+ and Ag+ adsorption are
describe the relationship between the pollutant and the adsorbent. The different (Sellaoui et al., 2020). Co-precipitation was employed to
Langmuir and Freundlich isotherms, which can be utilized on hetero incorporate sulphur, amide, and carboxyl groups into the MgAl-based
geneous as well as homogeneous substrates, are the two formulations LDH surface, and cysteine was intercalated. The major variables
that are most frequently employed (Asgari et al., 2014; Choy et al., 2000; include the production of precipitates in metallic hydroxides or sul
Tan et al., 2016). The Sips isotherm, which combines the Langmuir and phides, and the topological association of massive surface groups.
Freundlich isotherms, is another applicable isothermal paradigm. The Cysteine is a promising intercalation compound that might improve the
Sips hypothesis transforms into isotherms of Langmuir and Freundlich, adsorption efficacy of LDHs. MgAl-Cys-LDH has the potential to be
accordingly, for both elevated and decreased adsorbate amounts (Yao effective for heavy metal removal (Zhang et al., 2020c).
et al., 2017). The Langmuir and Freundlich isotherms also suit the re To address the problem of separating hydrophilic LDHs-based ad
sults of the experiments. Due to the fact that the procedure for adsorp sorbents, several researchers have chosen to include magnetism by
tion can only be limited to the use of dye monolayers. Pseudo-first order incorporating iron oxides into LDHs for the production of magnetic
as well as pseudo-second order kinetic schemes were employed to LDHs (MLDH) (Behbahani et al., 2021; Hassani et al., 2018a; Lu et al.,
explain how the absorbent and adsorbate interact in order to most 2017; Oladipo et al., 2019; Shan et al., 2014). In a recent study, thio
closely match to the findings of the experiments (Jalil et al., 2010; Wang glycolic acid (TGA) was employed as an intercalant to prepare a mag
et al., 2015). netic LDH-based nanocomposite viz. Fe3O4-ZnFe-TGA-LDH to remove
heavy metals including Hg2+ and Pb2+ (Movahhedi et al., 2020). The
4.1.1. Factors affecting heavy metal adsorption specific adsorption of this magnetic nanocomposites revealed that the
Heavy metals have been extensively investigated as the probe pol adsorption potential is either high or weak with no intermediate
lutants for assessing the efficacy of LDHs. According to available studies, adsorption potential (Movahhedi et al., 2020). Shan et al. (2014)
efficient adsorption of heavy metals by LDH-based composites has been examined the adsorption kinetics, isotherms, thermodynamic, and me
achieved (Table 2). Heavy metals have led to the widespread use of LDH chanical properties of Cd2+ during removal magnetic Fe3O4-MgAl-CO3-
for their removal from wastewater and soil. High efficiency has been LDH and MgAl-CO3-LDH. Cd2+ adsorption was endothermic, and
reported (Table 2) in the adsorption of heavy metals onto LDH-based spontaneous. The findings showed that process of adsorption happens on
composites. The MgAl-LDH was tested for the elimination of heavy the surface by the formation of CdCO3 and complexation on the surface
metals such as Pb2+, Cu2+, Ni2+ and Zn2+ (Zhao et al., 2020c). In a one- make up the majority of the magnetic LDH (Shan et al., 2014). In order
pot technique, NiFe-LDH, a micro composite material with intercalated to enhance the adsorbent separation from the water after the adsorption
sulphide ions, was created for selective metal removal. Because sulfonic process, synthesis of magnetic LDHs should be preferred.
acid and sulphide groups are fairly soft Lewis bases, weak Lewis bases Hibino demonstrated that LDHs are attractive adsorbents for anions.
may preferentially adsorb heavy metal ions, in accordance with the This is because lamellar materials, such as LDHs, consist of stacked metal
Lewis acid-base concept (Wang et al., 2019a). Chelating by NiFe-LDH hydroxide layers separated by interlayer voids that are populated by
resulted in metal ion adsorption, and a series of characterization tech anions and water molecules. LDHs can be used as efficient adsorbents for
niques were utilized to elucidate the adsorption mechanisms by linking the removal of anions because of the ease with which interlayer anions
the radioligand couplings to remove heavy metals. This study demon can be exchanged (Hibino, 2018). In a recent study (Kang and Park,
strates how the adsorbent has a high probability of selectively removing 2022), LDHs were recognized as highly sought-after adsorbents because
heavy metals and is a promising material for water treatment (Wang of their programmable properties, which make them useful in a variety
et al., 2019a). Sellaoui et al. (2020) used statistical physics modelling to of applications. LDHs are intriguing because their characteristics can be
explain the effective adsorption of Ag+ and Hg2+ on functionalized LDH tuned by changing the type of metal and interlayer anion. Although
with different intercalated anions such as NO3− , SO2− 2−
4 , CO3 , and MoS4
2−
research has been conducted to improve the properties of LDHs by
(Sellaoui et al., 2020). The probabilistic physical theory comprising two changing their composition, very little research has been conducted to
sites of action built around adsorbate interaction is the most effective investigate anion intercalation techniques that may efficiently create the
9
Table 2
Performance of LDH and LDH-based composites for the adsorption of heavy metals from different water matrices.
Composite Precursors Synthetic LDH Dose Pollutant Pollutant Adsorption Contact Cycles pH Removal Ref.
name method concentration capacity time
NiCo-LDH/ Ni(NO3)2⋅6H2O Green 2.0 mg Hg2+ 250 mg L− 1

530 mg g− 1
120 min – 3, 8 99% (Soltani et al.,
MOF Co(NO3)2⋅6H2O synthesis Ni2+ 439 mg g− 1
2021b)
ZrCl4
ZnAlNi- Zn(NO3)2⋅6H2O Co- 50 mg Ni2+ 100 mg L− 1
223 mg g− 1
120 min 8 7 97% (Feng et al.,
LDH/ Al(NO3)2⋅9H2O precipitation 2020)
MXen NiSO4⋅6H2O
NiCo-LDH/ Ni(NO3)2⋅6H2O in-situ 0.02 g Cd2+ 0.5–250 415 mg g− 1
120 min – 5 – (Soltani et al.,
MOF Co(NO3)2⋅6H2O Pb2+ mg L− 1 301 mg g− 1
2021a)
ZrCl4
ZnAl-GA- AlCl3 Co- 0.05 Cu2+ 50 mg L− 1
190 mg g− 1
2h 6 5 94% (Mahmoud
LDH ZnCl2 precipitation g L− 1 et al., 2020)
Gallic acid (GA)
AlLi-LDH/ LiNO3 Hydrothermal 50 mg Cr6+ 100 mg L− 1
172 mg g− 1
4h 3 4 94% (Manea et al.,
CNTs Al(NO3)3⋅6H2O 2022)
2+ − 1
Fe3O4/ Mg(NO3)2⋅6H2O Hydrothermal 0.03 g Pb 10–300 mg 191 mg g 1h 6 5 – (Behbahani
FeMoS4/ Al(NO3)3⋅9H2O Cd2+ L− 1. 141 mg g− 1
et al., 2021)
MgAl- Zn(NO3)2⋅6H2O Cu2+ 110 mg g− 1
LDH FeCl3⋅6H2O
Na2MoO4⋅2H2O
Thiourea
Ligand/ Fe(NO3)3⋅6H2O Co- 0.025–0.10 Cu2+ 60 mg L− 1
425 mg g− 1
7 7 5 99% (Awes et al.,
MgFe- Mg(NO3)2⋅6H2O precipitation g 2021)
LDH Aminouracil ligand
1
NiFe- Ni(NO3)2⋅6H2O Hydrothermal 0.5 g L− Hg2+ 10 mg L− 1
462 mg g− 1
24 h 5 6 >99% (Wang et al.,
MoS4- Fe(NO3)3⋅9H2O Pb2+ 299 mg g− 1
2019c)
LDH/CF NH4F Cu2+ 128 mg g− 1
Urea
[SnS4]4− / MgSO4 Co- 20 mg Hg2+ 10 mg L− 1
343 mg g− 1 – – 2, 7 99% (Li et al.,
MgFe- Fe2(SO4)3 precipitation As3+ 25 mg L− 1
49 mg g− 1 2021)
LDH SnCl4⋅5H2O
Na2S⋅9H2O
MgAl- Mg(NO3)2⋅6H2O Co- 0.05 g Cu2+, 1.5 mmol L− 1
0.9 mmol 240 min – 6.15, >95% (Zhang et al.,
LDH/SA Al(NO3)3⋅9H2O precipitation Pb2+, 2.5 mmol L− 1
g− 1 5.54, 2021)
Sodium alginate Cd2+ 1.0 mmol L− 1
1.2 mmol 5.48
(SA) g− 1 0.9
mmol g− 1
1
MgAl- Mg(NO3)2⋅6H2O Hydrothermal 0.3 g L− Hg2+, 10 mg L− 1
250 mg g− 1
3h – 5.5 99% (
LDH/ Al(NO3)3⋅9H2O Cu2+, 105 mg g− 1
88% Mombeshora
MPA Cu(NO3)2⋅3H2O Pb2+ 122 mg g− 1
92% et al., 2022)
Mercaptocarboxylic
acid (MPA)
NiFe-LDH/ Ni(NO3)2 Co- 50 mg Pb2+ 1000 mg L− 1
986 mg g− 1
2 min 3 11 >95% (Baruah
N-doped Fe(NO3)3 precipitation Cd2+ 971 mg g− 1
et al., 2019)
GO Graphene oxide
(GO)
ZnAl-LDH Zn(NO3)2⋅6H2O in-situ 20 mg Cr6+ 40 mg L− 1
118 mg g− 1
140 min 5 10.6 >99% (Zheng et al.,
Al(NO3)3⋅9H2O vulcanization 2021)
FeMg- MgCl2⋅6H2O Co- 0.05 g Cu2+ 50–800 mg 85.53 mg 30 min 6 5 100% (Khandaker
LDH/BC FeCl3⋅6H2O precipitation L− 1 g− 1 et al., 2021)
Biochar (BC)
1
MgZnFe- Cu(NO3)2⋅3H2O Co- 0.01 g L− Cu2+ 5–1000 mg 118 mg g− 1
90 min 1 5 >98% (Hussein
LDH Zn(NO3)2⋅6H2O precipitation L− 1 135 mg g− 1
et al., 2023)
MgZnFe- Mg(NO3)2⋅6H2O
LDH/Tz Fe(NO3)3⋅9H2O
3-amino 1-H-1,2,4-
triazole (Tz)
CuMgAl- Cu(NO3)2⋅3H2O Co- 0.25 g Zn2+ 70 mg L− 1
154 mg g− 1
90 min 5 5 95% (Alnasrawi
LDH/ Mg(NO3)2⋅6H2O precipitation et al., 2023)
MMt Al(NO3)3⋅9H2O
Montmorillonite
(MMt)
CaAl-LDH/ Ca(NO3)2 Co- 0.039 g Cu2+ 15 mg L− 1
200 mg g− 1
6.31 – 8 93% (Taheri et al.,
Fe3O4 Al(NO3)3⋅9H2O precipitation Ni2+ 110 mg g− 1
min 83% 2023)
Fe3O4
nanocomposite
1
MgAl- Al2O3 Co- 2 g L− Cr6+ 10–250 mg 178 mg g− 1
180 min 5 2 95% (Li et al.,
LDH/ MgO precipitation L− 1 2023c)
PBC PBC
1
CuMgAl- Cu(NO3)2⋅3H2O Co- 0.02 g L− Cd2+ 50 mg L− 1
175 mg g− 1
120 min 5 5 89% (Alnasrawi
LDH/ Mg(NO3)2⋅6H2O precipitation and
MMt Al(NO3)3⋅9H2O Mohammed,
MMt 2023)
(continued on next page)
10
Table 2 (continued )
Composite Precursors Synthetic LDH Dose Pollutant Pollutant Adsorption Contact Cycles pH Removal Ref.
name method concentration capacity time
CaFe-LDH/ FeCl3⋅6H2O Co- 0.20 g Cd2+ 50 mg L− 1 22 mgg-1 300 min – 6 50–70% (Liang et al.,
CSB CaCl2 precipitation Pb2+ 50 mg L− 1 218 mgg-1 2023)
Corn straw biochar Zn2+ 800 mg L− 1 17 mgg-1 6
(CSB) Cu2+ 50 mg L− 1 8 mg g-1
necessary morphologies of LDHs. Anion exchange in ZnAl-LDHs syn Negarestani et al. (2023) synthesized a novel LDH for the elimination
thesized on a silicon substrate using a posttreatment-based reconstruc of methylene blue and reactive orange 16 dyes from aqueous solution
tion method was assessed. Structural and chemical investigations (Fig. 8). They used sisal fiber (SF) biomaterial because of its distinctive
indicated that calcined ZnAl-LDH underwent reconstruction as a features, including its tensile strength, sustainability, non-toxicity, and
consequence of the anion-exchange process with NaCl. As NaCl con high density. The SF was used as a base/supporting material and
centration increased from 0.15 M to 0.60 M, the rate of anion exchange modified to develop a nanocomposite consisting of SF, polyaniline
and fraction of ZnAl-LDH that underwent rebuilding increased. When (PANI), rhamnolipid (RL), and NiAlLDH To prepare this composite,
the NaCl concentration was increased above 0.90 M, anion exchange aluminum nitrate nonahydrate and nickel nitrate hexahydrate were
decreased. Therefore, the anion composition and shape of ZnAl-LDHs mixed in water with the help of ultrasound vibrations to modify NiAl-
may be modified by controlling the concentration of NaCl present LDH. Urea and SF@PANI were added to the mixture. This reaction
throughout the reconstruction process (Kang and Park, 2022). was conducted for 18 h at 75 ◦ C to produce binary PANI and NiAl-LDHs
In another study, a novel adsorbent CuMgAl-LDH-montmorillonite composites improved by sisal fibers (SF@PANI@LDH). Then this com
(MMt) nanocomposite was prepared for the removal of Cd2+ from posite was washed and dried at 55 ◦ C. This urea hydrolysis approach
pollutant water. The LDH was developed by employing the low- directly affected LDH on SF (SF@LDH) and RL mixture was prepared by
supersaturation co-precipitation approach (Alnasrawi et al., 2023). combining RL with deionized water and mixed it gently for 30 min, or
The effects of different parameters and their influence on sorption of until a cloudy color is observed. The SF@PANI@LDH was then
Cd2+ were studied. Fig. 7(a–f) shows the effect of pH, dose, agitation immersed in the RL mixture for 30 h at room temperature and pressure.
speed, particle size, and initial concentration of the probe metal Cd2+. Fig. 8a–b show SF@PANI@RL@LDH adsorption efficiency at different
The optimized conditions that gave maximum adsorption capacity from pH as well as its reusability. Material was reused for six cycles with
these experiments were as follows: dose = 0.02 g L− 1, pH = 5, Cd con consistent adsorption efficiency. The elimination of methylene blue
centration = 50 ppm. Fig. 7g shows that after five repeated cycles, the accelerated appreciably in alkaline solution. On the other hand, reactive
LDH may be regenerated with a 29.56% efficiency reduction in the orange 16 adsorption was effective in the acidic solution with pH = 3.
adsorption capacity. The results demonstrate that the novel synthesized The methylene blue and reactive orange 16 dyes had the maximum
nanocomposites have great prospects of regeneration, which might adsorption capacity of 24.80 mg g − 1 and 23.98 mg g− 1, respectively at
result in reduced expenses and environmental effects (Alnasrawi and 45 ◦ C. According to Fig. 8(d), mechanisms of dye removal include
Mohammed, 2023). electrostatic force of attraction, H-bonding, and π- π interaction (Neg
arestani et al., 2023). Selected examples of the performance of LDH-
4.1.2. Factors affecting organics adsorption based nanocomposite for dye removal are presented in Table 3.
Layered double hydroxides have been widely used for the removal of The effectiveness and reusability of adsorbents including those based
organic dyes from wastewater. These dyes are harmful for all aquatic life on LDHs largely determine their long-term viability and stability (Sta
as well as terrestrial life, and thus must be removed from industrial wiński et al., 2017; Zubair et al., 2021; Zubair et al., 2017). Adsorbent
wastewater before discharging them to the streams and lakes. LDH- regeneration is the most important factor that governs operating cost.
based nanocomposites have shown remarkable efficiency for the Calcination and chemical methods are the two most often utilized
removal of several dyes (Table 3). Najafi et al. (2022) synthesized NiFe- methods for LDH regeneration. The adsorbents are firstly cleansed with
LDH by employing a combined urea hydrolysis and hydrothermal water before being baked at different temperatures. Chemical treatment
method. Two different adsorption methods sono-sorption and liquid- entails the regeneration of adsorbents using organic solvents and/or
phase sorption were used to remove the congo red dye from aqueous acids. Fig. 9 illustrates both the chemical and thermal processes for
solution. Owing to the formation of microscopic bubbles, intense vi adsorbent regeneration (Stawiński et al., 2017). In a study, NiAl-LDHs
brations, high-velocity microjets, and reduced thickness of diffusion were used to eliminate the Congo red dye (Bharali and Deka, 2017). A
layers, the sono-sorption technology demonstrated effective dye efficacy water-based Na2CO3 solution was employed to assess the capacity of the
(Najafi et al., 2022). In addition, the NiFe-LDH/Au nanocomposite adsorbent for reuse. The chemical restoration approach showed excep
performed significantly better removal of the congo red dye, eliminating tional regeneration potential of 80%, 86%, and 91% during three sub
95% in just 7 min during the sono-sorption process. The efficient sequent cycles. Similarly, ZnAl-LDH/Al(OH)3 composites were
execution of the NiFe-LDH/Au composite can be attributed to the regenerated by combining it with 0.2 M NaOH solution over a duration
increased specific surface area of the adsorbent, improved dispersion of of 2 h. The regenerated nanocomposite showed elimination performance
Au-nanoparticles over the surface of NiFe-LDH, and synergistic in of 74% after five cycles (Guo et al., 2018). Notably, NiFe-LDH (Zubair
teractions between Au and NiFe-LDH (Najafi et al., 2022). The prepa et al., 2018) and ZnAl-LDH (Kumar et al., 2017) have been effectively
ration of magnetic ZnAl-LDH was investigated for the elimination of reused after methylene orange adsorption using 0.1 M NaOH. In
congo red and malachite green dyes (Tang et al., 2023). At room tem vestigations were conducted on the type of dye, environmental factors,
perature, the highest adsorption capacity of malachite green and congo dye concentration, and adsorption capacity. Table 3 also includes the
red by ZnAl-LDH was found to be 850.93 mg g− 1 and 279.09 mg g− 1, reusability of the LDHs reported in literature, showing that the congo
respectively. Adsorption thermodynamics revealed that the adsorption red dye can be successfully removed using a range of LDHs. In a study
of both dyes was instantaneous and endothermic in nature. Further (Lu et al., 2017), compared to the pure MgAl-LDH (520 mg g− 1), the iron
more, M ZnAl-LDH maintained its adsorption ability even after four oxide containing LDH (Fe3O4@MgAl-LDH) exhibited a maximum
cycles. Finally, ZnAl-LDH could be considered a viable adsorbent for adsorption capacity of 813 mg g− 1. Compared to the Fe3O4@MgAl-LDH,
dye-containing wastewater (Tang et al., 2023). pure Fe3O4 could only adsorb at 133.7 mg g− 1,. It is important to note
11
Fig. 7. The impact of experimental conditions on Cd2+ sorption by CuMgAl-LDH-MMt. (a) dose = 0.25 g, initial Cd2+ = 50 ppm, particle size = 194 μm, and rpm =
200, (b) Effect of LDH dose; initial Cd2+ = 50 ppm, pH = 5, particle size = 194 μm and rpm = 200, (c) Effect of agitation speed; initial Cd2+ = 50 ppm, pH = 5,
particle size = 194 μm, and LDH dose = 0.20 g, (d) Effect of LDH particle size; initial Cd2+ = 50 ppm, pH = 5, and LDH dose = 0.20 g (e) Effect of initial Cd2+
concentration; pH = 5, rpm = 150, dose = 0.20 g, and particle size = 87 μm (f) Effect of initial Cd2+ concentration on adsorption, and (g) Cyclic performance of the
LDH. Reproduced from Alnasrawi and Mohammed (2023) under a Creative Commons license.
12
Table 3
Selected performance of LDH and LDH-based composites for the adsorption of organics from water matrices.
Composite name Synthetic method Pollutant Pollutant LDH Capacity Contact pH Reusability Removal Ref.
dose dose time
1 1
ZnAl-gallate-LDH/ Co-precipitation Malachite green 50 mg L− 0.05 g 61 mg g− 3h 8 6 95% (Mahmoud
polystyrene L− 1 et al., 2020)
nanofibers
1
CuAl-LDH/polymer Urea-assisted co- Methylene blue 50 mg L− 1 mg 575 mg 35 min 11 5 – (Ghanbari and
precipitation g− 1 Ghafuri, 2022)
1 1 1
CoZnAl-LDH/ Co-precipitation Methylene blue 30 mg L− 0.4 g L− 170 mgg− 2h 10 4 95% (Sharifi-Bonab
graphene oxide et al., 2020)
− 1
MgAl-LDH/activated Hydrothermal Methylene blue 50 mg L 10–40 816 mg 120 min 9 5 98% (Aldawsari
carbon mg g− 1 et al., 2021)
− 1 1
NiFe-LDH/Au Urea-hydrolyzed Congo red 10 mg L 7 mg 417 mgg− 10 min 4.8 4 95% (Najafi et al.,
hydrothermal 2022)
ZnAl-LDH/polyvinyl Co-precipitation Tartrazine, 25 mg L− 1 20 mg 36 mg g− 1 40 min 2, 7, – 96% (Balayeva et al.,
alcohol Ponceau 4R, 15 mg L− 1 16 mg g− 1 2 2023)
Patent blue V 6 mg L− 1 33 mg g− 1
CoMgAl-Borate-LDH Chemical etching Congo red, 200 mg L− 1 2.50 mg 1493 mg – 4.0 5 87% (Miao et al.,
Methyl orange 150 mg L− 1 3.33 mg g− 1 84% 2021)
990 mg
g− 1
1
MgAl-LDH/Diatoms Co-precipitation Congo Red 50 mg L− 40 mg 306 mg 30 min 7 5 98% (Sriram et al.,
g− 1 2020)
1
CoCu-LDH Ultra-sonication Methyl orange 200 mg L− 0.02 g 1064 mg 75 min 7 5 >99% (Saghir et al.,
and precipitation g− 1 2020)
− 1 − 1
ZIF-67@LDH Co-precipitation Methyl Orange 200 mg L 0.2 g L 663 mg 15–20 6 4 94% (Saghir and
Alizarine Red S g− 1 min 4 98% Xiao, 2021)
893 mg
g− 1
1
SF/polyaniline/bio- Urea hydrolysis Methylene blue 40 mg L− 100 mg 25 mg g− 1 200 min 10 6 >99% (Negarestani
1
surfactant Reactive orange 20 mg L− 24 mg g− 1 3 et al., 2023)
rhamnolipid-LDH 16
ZnAl-LDH/SDS/ Co-precipitation Congo red 1500 mg 1.50 g 1.42 × – 5 7 94% (Zong et al.,
MWCNTs L− 1 L− 1 10− 3 mol 2022)
g− 1
1
NiMgAl-LDH Hydrothermal and Methyl orange 25 mg L− 0.01 g 323 mg 80 min 9 3 93% (Waheed et al.,
Co-precipitation g− 1 2023)
1
Titanate nanotubes/ Hydrothermal Acid rain 1 50 mg L− 0.02 g 124 mg – 2 – – (Zhang et al.,
layered double Methylene Blue g− 1 9 2023)
hydroxides/ Methylene green 322 mg 9
graphene oxide g− 1
526 mg
g− 1
1 1
Magnetic ZnAl-LDH Co-precipitation Congo red 100 mg L− 0.5 g L− 279 mg 6h 6–7 4 – (Tang et al.,
1
Malachite green 200 mg L− g− 1 2023)
850.9 mg
g− 1
1 1
CaCr-LDH/biochar Co-precipitation Congo dye 50 mg L− 0.5 g L− 631 mg 6h 6.85 3 – (Cruz et al.,
g− 1 2023)
that LDH-based hybrids considerably increase their adsorption capacity. issues result in instability, sub-par catalytic efficiency, and increasing
For instance, the congo red dye is effectively removed by CaFe2O4/poly prices. To address these limitations, strategies like heterojunction as
o-phenylenediamine/MgAl-LDH and ZnAl-LDH/Al(OH)3 (Beyki et al., sociation, copolymerization, nano-structural technology, surface defect
2016; Guo et al., 2018), exhibiting comparable sorption capacity of 500 engineering, and elemental doping have been developed (Ashiq et al.,
mg g− 1 and 1574.4 mg g− 1, respectively, with effective removal of above 2022; Hassani et al., 2018b; Niu et al., 2021; Qian et al., 2021; Yu et al.,
95%. A novel TiO2/LDH composite was found to remove nearly 98% of 2021). In this context, The hetero-structures of LDHs have emerged as
congo red using just 0.05 g of the adsorbent (Ma et al., 2017). Our potential catalysts for photocatalysis due to their ease of production,
literature survey showed that LDH could be effective for anionic, ability to facilitate the transport of photo-excited electrons, and control
cationic, and neutral dyes. Importantly, functionating or modification of over electron and hole recombination (Sahoo et al., 2021; Yang et al.,
LDH is recommended to improve adsorption capacity and cyclic 2021). However, LDH materials exhibit inadequate photocatalytic effi
performance. ciency due to aggregation, and temporary electron-hole generation
(Abazari et al., 2020; Mallakpour and Hatami, 2018). To overcome these
4.2. LDH-based composites for heterogenous catalysis limitations, the addition of metallic substances, or metal oxides to LDHs
can enhance their photocatalytic properties. By creating exfoliated
In this section, focus of discussion has mainly been placed on the sheets with improved oxidation capabilities and enhanced photo
application of LDH and LDH-based composites on photocatalysis. The activity, these modifications contribute to enhanced structural proper
main objective of photocatalysis is to develop light-absorbing catalysts. ties and active sites (Abazari et al., 2020). The relationship connecting
However, current photocatalysts face several challenges, such as sig the metal ions M2+ and M3+ in LDHs results in a structural modification,
nificant photo corrosion under UV and sunlight exposure, uncontrolled whereby M3+ functions as a doping agent to increase the photocatalytic
extinction coefficient, limited surface area, narrow bandgap, recombi efficiency depending on visible light (Motlagh et al., 2020; Nayak et al.,
nation of hole and electron pairs, and high material preparation costs 2019). The key advantages of using LDHs for photocatalytic degradation
(Lan et al., 2014; Pourshirband et al., 2021; Wang et al., 2017). These include their extensively hydroxylated stacked structure, which
13
Fig. 8. (a) The effect of solution pH on the removal of methylene blue and reactive orange 16 dyes by SF@PANI@RL@LDH; (b) Cyclic performance of SF@PA
NI@RL@LDH; (c) Preparation of SF@PANI@RL@LDH; and (d) Mechanisms of dye removal by SF@PANI@RL@LDH. Reproduced from Negarestani et al. (2023)
under Creative Commons CC BY license.
enhances adsorption of pollutants and separates charges (Cui et al., assemblies on ZnTi-LDHs facilitate the integration of Ti4+ and Zn2+,
2021; Seftel et al., 2015). Additionally, LDH surface modifications might promoting charge separation and boosting photocatalytic activity (Seftel
enhance the ability to absorb substances with hydrophobic properties et al., 2014). Moreover, the addition of Zn2TiO4 and ZnO layers improve
over their outermost layers, thereby enhancing photocatalytic degra the photocatalytic efficiency of TiO2/ZnAl-LDH composites, owing to
dation (Huang et al., 2013). the enhancement in electrical properties and stability (Hadnadjev-Kostic
et al., 2014). According to a previous study, rhodamine B elimination
4.2.1. Functionalization of LDHs for enhanced photocatalytic performance could be improved by employing BiOCl/NiFe-LDH composite as a pho
The outer layer of LDHs can be coated with different materials to tocatalyst. The TEM images revealed that BiOCl nanoparticles are evenly
increase their surface area without compromising the photocatalytic distributed over the pristine NiFe-LDH sheets, corroborating the XRD
performance (Wang et al., 2019b). A visible-light-driven photocatalyst findings (Ma et al., 2015). Since BiOCl disperses more widely over NiFe-
ZnCr-CO3-LDH, effectively degraded rhodamine G, 4-chloro-2-nitro LDH, electrons may more easily move from the NiFe-LDH conduction
phenol, and rhodamine B through the production of •OH radicals band to the conduction band (CB) of BiOCl. Since the valance band (VB)
(Mohapatra and Parida, 2012). The sunlight irradiation triggers a chain of NiFe-LDH has a more negative potential, the holes created in the
reaction, resulting in the generation of reactive oxygen species by BiOCl VB may be easily transferred. This resulted in a more efficient
forming electron-hole pairs in the oxygen molecules within the LDH separation of electrons and holes. The interaction between the holes and
layers. Different anionic materials were studied to understand their the outer groups on LDHs produced •OH radicals and accelerated the
impact on the photocatalytic function of ZnCr-LDH (Mohapatra and degradation process (Ma et al., 2015). LDHs supplemented with transi
Parida, 2012). Metal-to-metal charge transferring from the oxo-bridged tion metal oxides were investigated for the photocatalytic degradation
connection of Zn-O-Y in ZnCr-LDHs enhances the photocatalytic effi of acidic red 14 dye under visible light. The CeO2/ZnTi-LDH showed
ciency. Incorporating ZnCr-LDHs with tungstate and molybdate showed superior photocatalytic efficiency compared to other metal oxides, due
higher efficiency for rhodamine G decomposition (Mohapatra and Par to the narrowest bandgap, lowest pore volume, and largest surface area
ida, 2012). The photocatalytic efficiency of nanoscale photocatalysts (Xia et al., 2014). Metal-modified LDH hybrids are a focus for improving
can be enhanced by combining LDHs with transition metal oxides that photocatalytic effectiveness due to their plasmon resonance character
have a broader spectrum of absorption. For instance, CeO2 self- istic and ability to prevent charge amplification. Ag/ZnTi-LDH
14
Fig. 9. Regeneration of adsorbents including LDH by thermal treatment (a) and chemical treatment (b).
demonstrated exceptional efficiency in the destruction of rhodamine B, LDH CB. This improved charge separation and resultant degradation
benefiting from plasmon resonance and reduced recombination rates efficiency. Polypyrrole, a conducting polymer with a P-electronic shape
(Zhu et al., 2018). Additionally, Pd(II)/Bi2O3/MgAl-LDH, with a low and high visible light absorption, can be coupled with LDHs. Indeed,
ered bandgap, improved surface area, and advantageous phase trans Mohamed et al. (2018) tested a nanofibrous ZnFeLDH-based catalyst for
formation, exhibited notable photocatalytic properties in the safranin stain removal photocatalysis. The higher surface area and 2.31
degradation of methylene blue (Zhou et al., 2015). eV bandgap of the composite boosted photocatalytic efficiency,
To enhance photocatalytic efficiency, metal-free polymers with completely removing the tested dye in 120 min. The catalyst proved
enhanced stability in structure and absorbance of light, like graphitic durable during three recycling operations with a decline of only 5.79%.
carbon nitride (g-C3N4), may be coupled with LDHs. In-situ crystallized The metal‑oxygen cluster polyoxometalates (POM) have shown excep
g-C3N4/ZnAl-LDH composites vs. pure g-C3N4 and ZnAl-LDH demon tional catalytic characteristics. Photocatalytic break down of methylene
strated synergistic effects on methylene blue photocatalysis (Yuan and blue in water by POM/ZnAlFe-LDH was successful (Xu et al., 2018).
Li, 2017). UV irradiation transports electrons from the g-C3N4 conduc Negatively charged POMs helped cationic dye components adsorbed
tion band (~1.112 eV) to its CB because ZnAl-LDH has more energy onto the top layer of POM/ZnAlFe-LDH. Carbon-based LDH modifica
(+0.55 eV). Electrons in ZnAl-LDH break down to O2 for generating •OH tions may speed charge separation due to their electrical characteristics
radicals, which improves charge separation (Yuan and Li, 2017). Further (Gholami et al., 2020).
research found that the hydrothermally-made catalyst CoAl-LDH/g- In a previous study (Ju et al., 2017), urea was used to create C60-
C3N4/rGO had a higher photocatalytic ability for tetracycline and Congo customized ZnAlTi-LDH nanocomposites. The nanocomposites were
red degradation as compared to pure CoAl-LDH (Jo and Tonda, 2019). then evaluated for the degradation of Bisphenol A under visible light. It
As illustrated in Fig. 10(a) (Jo and Tonda, 2019), the considerable was found that C60 acts as a photosensitizer, transferring irradiation-
interface interaction between LDH, g-C3N4, and rGO increased charge generated electrons to the ZnAlTi-LDH phase, thereby increasing elec
transmission and photocatalytic ability for pollutant degradation. tron density. The nanocomposite holes react with the adsorbed OH− to
Because of their interface connection, g-C3N4 and rGO exhibit strong generate radicals for Bisphenol A degradation (Ju et al., 2017).
electron conduction capacity that helped in collecting electrons from Furthermore, integrating LDHs with graphene enhanced the
15
Fig. 10. (a) Mechanism of photocatalytic degradation by CoAl-LDH/g-C3N4/rGO composite, (b) Process of electrons-holes departure in the ZnCr-LDH/GO com
posite, and (c) Mechanism of phenol removal by CuNiFe-LDHs during Fenton reaction.
photocatalytic capabilities of nanomaterials due to its higher charge intriguing approach in this situation for the removal of organic pollut
carrier mobility and electrical conduction. In another study (Lan et al., ants (Asif et al., 2022; Asif et al., 2023; Ly et al., 2023). To create very
2014), degradation of ofloxacin under visible light using GO/ZnFe-LDHs reactive and stable nanocomposites, LDHs may be used as a catalyst or
was assessed. The creation of heterostructures between ZnFe-SO4-LDHs supporter (Zhang et al., 2014). Increased catalytic activity, and surface
and GO improved the degradation of ofloxacin by facilitating charge area can be achieved by embedding Fenton catalysts within LDHs
differentiation and longevity. Importantly, they discovered that a hybrid (Huang et al., 2018). Because of their stacked structure, inclusion of
ZnCr-LDHs/GO nanocomposite exhibited better degradation of rhoda divalent and trivalent metals is relatively simple. It appears that LDHs
mine B under visible light as compared to pure ZnCr-LDHs (Lan et al., have advantages over other Fenton-like catalysts (Bai et al., 2017;
2014). The ZnCr-LDHs/GO displayed high charge separation, enabling Huang et al., 2018). Owing to the redox-cycle between Fe2+ and Fe3+,
the nanocomposite catalyst to evolve in the visible light spectrum this equilibrium can aid in the regeneration of active sites to maintain
(Fig. 10b). The homogeneous dispersion of ZnCr-LDHs on GO nano catalytic activity. Additionally, the oxygen vacancies produced by the
sheets prevented recombination of photogenerated electron-hole pairs, octagonal geometry of the LDHs are beneficial for Fenton-like reactions
making them more susceptible to breakdown rhodamine B (Lan et al., (Guo et al., 2020; Zhong et al., 2019). The released Fe2+ from LDH-based
2014). Overall, LDH photocatalysts, when combined with other mate catalysts may be effectively used in this anionic interchange in a solution
rials such as graphene, can effectively degrade toxic organic contami of water to carry out homogenous Fenton reactions.
nants, thereby improving wastewater treatment. A highly reactive and effective Fenton-like catalyst for the degradation
of toxic organic pollutant was developed by combining dodecylbenzene
4.2.2. LDH as Fenton and Fenton-like catalyst sulfonate (DBS)-LDHs with carbon dot (Zhang et al., 2014). This com
The typical Fenton reaction has inherent limitations that prevent its posite showed unique geometric features, promoting radical production
widespread application, including reaction in a limited pH range, the within the matrix without the need for external power. The free electrons
generation of iron sludge, as well as the wasteful usage of chemicals from LDHs interacted with H2O2 to generate •OH radicals, while the re
(Nidheesh, 2015; Nidheesh et al., 2013). Heterogeneous Fenton-like action of these radicals with DBS molecules on the outermost layer of
reactions using non-metallic, or transition metals present a highly LDHs produced SO2− 4 . Another Fenton-like catalyst was created by
16
combining biochar with FeAl-LDH for the degradation of phenol (Fan and was unaffected within the range of 4.0 to 6.5, possibly due to the
et al., 2021). The enhanced adsorption capacity and radical yield expe formation of less sensitive precipitates of Cu2+. Notably, Cu ions pre
dited the degradation of phenol. In a study by (Lu et al., 2016), a multi- dominated during their association with H2O2, contributing electrons for
metal Cu-Zn-Fe-LDH material with sulfate was found to be an efficient the production of •OH radicals and exhibiting a faster radical formation
Fenton-like catalyst for the removal of acetaminophen from water sam rate compared to Fe2+ (Wang et al., 2018). Moreover, as shown in Fig. 10c
ples. The addition of Fe and Cu ions triggered a cyclic process that (Karim et al., 2022; Wang et al., 2018), Cu regeneration was supported by
generated •OH radicals, and the catalyst remained active for six cycles. the effective transmission of metal-oxo-metal bonds. LDHs are also
Wang et al. (2018) utilized a multi-metal ternary composite, CuNiFe-LDH, extremely hydrophilic due to the presence of surface hydroxyl groups,
to effectively degrade phenol in the Fenton reaction. The Cu0.5Ni2.5Fe- which favors the catalytic process taking place for phenol degradation.
LDH catalyst demonstrated the highest removal of total organic carbon, For the MnMg/Fe-LDH catalyst, an appreciable increase in methylene
with the Cu/Ni molar ratio significantly influencing the degradation ef blue degradation rate was reported (Gonçalves et al., 2020). The presence
ficiency. The catalyst activity was relatively less sensitive to pH changes of Mn in LDH, which raised the surface area and lowered crystallinity, was
Table 4
Selected examples of LDH and LDH-based composites for the degradation of organics from water.
Composites Precursors Synthetic method Light source Pollutant Pollutant LDH Contact pH Removal Ref.
concentration dose time
1
Al-Li-Th-LDH@CNT Al(NO3)3⋅9H2O Hydrothermal Tungsten Malachite 40 mg L− 10 4h 7 98% (Manea
LiNO3 lamp Green mg et al., 2022)
(NH2)2CO
CNTs
1
ZrCuFe-LDH/rGO Zr(NO3)4⋅5H2O Co-precipitation Tungsten Methylene 10 mg L− 1.0 g 75 min 7 95% (Kumar
Fe(NO3)3⋅9H2O lamp blue L− 1 et al., 2021)
Cu(NO3)2⋅3H2O
Graphene oxide
1
ZnCo- LDH Co(NO3)2⋅6H2O Co-precipitation UV blue- Ponceau 4R 5 mg L− 0.5 g 120 min 6 100% (Abd-Ellatif
Zr(NO3)2⋅6H2O fluorescent L− 1 et al., 2022)
lamps
1
NiAl-LDH/ Al(NO3)3⋅9H2O Co-precipitation – Malachite 20 mg L− 0.75 – 7 89% (Hanifah
Polyoxometalate Ni(NO3)2⋅6H2O Green g et al., 2022)
Polyoxometalate
1
Magnetic LDH- Fe(NO3)3⋅9H2O Co-precipitation Visible light Eriochrome 50 mg L− 0.05 120 min 2 94% (Oladipo
based Ni(NO3)2⋅6H2O + Calcination black T dye g et al., 2019)
CoO–NiFe2O4 Co(NO3)2⋅6H2O method
catalyst
1
CoAl-LDH/g-C3N4/ Co(NO3)2⋅6H2O Hydrothermal Tungsten Congo red 20 mg L− 50 60 min 2 99% (Jo and
rGO Al(NO3)3⋅9H2O halogen lamp mg Tonda,
Graphite powder 2019)
Terephthalic acid
1
MgZnCr-LDH/TiO2 MgCl2 Co-precipitation Xenon lamp Congo Red 100 mg L− 0.5 g 40 min 9.26 98% (Ma et al.,
ZnCl2 L− 1 2017)
CrCl3
1
Nd/ZnAl-LDH Al(NO3)3⋅6H2O Hydrothermal Xenon lamp Congo red 40 mg L− 200 2.5 h – 93% (Wani et al.,
1
Zn(NO3)2⋅6H2O Fast green 20 mg L− mg 3h 85% 2022)
1
Nd(NO3)3⋅6H2O Rose Bengal 32 mg L− 2.2 h 89%
Urea
EDTMPA-Cu-LDH EDTMPA Co-precipitation Xenon lamp Rhodamine B 10 mM 0.3 g 2h 5.85 98% (Zhang
Cu(NO3)2⋅3H2O L− 1 et al.,
2020a)
1
Lys/CoFe-LDH@g- Co(NO3)2⋅6H2O Co-precipitation Visible light Rhodamine B 20 mg L− 50 90 min 98% (He et al.,
C3N4 FeCl3⋅6H2O mg 2023a)
Lysine
1
δ-Fe2O3/MgAl-LDH Al(NO3)3⋅6H2O Impregnation Tungsten Methylene 50 mg L− 0.5 g 240 min 5.9 86% (Kerchich
Mg(NO3)2⋅6H2O lamp blue L− 1 et al., 2021)
Fe(NO3)3⋅9H2O
1
ZnCoFe-LDH ZnCl2 Co-precipitation Visible light Methylene 10 mg L− 0.1 g 180 min 6 74% (Keyikoğlu
CoCl2⋅6H2O irradiation blue L− 1 et al., 2022)
FeCl3⋅6H2O
1
ZnIn-LDH Zn(NO3)2⋅6H2O Microwave Sunlight Methylene 20 mg L− 0.5 g 120 min – 98% (Liu et al.,
In(NO3)3⋅4⋅5H2O hydrothermal irradiation blue L− 1 2020)
1
M3CrCO3-LDH Cr(NO3)3⋅9H2O Co-precipitation Halogen lamp Methylene 5 mg L− 20 g 140 min 9–10 91% (Pan et al.,
M(NO3)2⋅6H2O blue L− 1 2019)
(M: Ni, Cu, Co,
Zn, Mg)
1
ZnCuFeCr-LDH Cr(NO3)3⋅9H2O Plasma assisted Xenon lamp Methyl 20 mg L− 1g 42 min – 97% (Tao et al.,
Zn(NO3)2⋅6H2O preparation orange L− 1 2020)
Cu(NO3)2⋅3H2O
Cr(NO3)3⋅9H2O
1
SnWO4/ZnFe-LDH Zn(NO3)2⋅6H2O Co-precipitation Xenon lamp Methyl 50 mg L− 50 40 min 9 95% (Wang et al.,
Fe(NO3)3⋅9H2O orange mg 2020a)
Na2WO4⋅2H2O
SnCl2⋅2H2O
1
NiCr-LDH/BC NiCl2⋅6H2O Hydrothermal Xenon lamp Methyl 100 mg L− 1 mg 60 min 5 100% (Li et al.,
CrCl3⋅6H2O orange L− 1 2023b)
Biochar (BC)
17
responsible for the improved catalytic activity. By embedding LHDs onto 4.2.3. LDH-based composites for degradation of organics
FeS and Fe3O4 using an in-situ growth method, FeS@LHDs and LDHs coupled with different support materials and composites
Fe3O4@LHDs catalysts were developed for the decomposition of showed excellent dye removal efficiency (Table 4). Previously, re
methoxychlor (Huang et al., 2018). While FeS was in charge of dichlori searchers synthesized ZnCo-LDH using the co-precipitation method. The
nation, Fe3O4 was principally in charge of producing •OH radicals. For the pH was maintained at 10 for the photodegradation of Ponceau 4R dye,
Fenton and Fenton-like catalytic reactions, LDHs can be modified using using a fluorescent lamp as the light source. The optimized dose of LDH
polymer-based, similar to photocatalysis. For instance, Yang et al. was found to be 0.5 g L− 1, and the degradation efficiency reached 100%
(2020a) developed a chitosan-based NiFe-LDH hybrid for facilitating the after 2 h (Abd-Ellatif et al., 2022). In another study, a hybrid material
degradation of phenolic compounds. In summary, pure LDH and their was synthesized using NiCo-LDH for the degradation of red reactive 120
composites could be low-cost and highly reactive catalyst for Fenton and dye. The microspheres of a Ni-based metal-organic framework were
Fenton-like reaction suitable for scale-up. transformed into the layered NiCo-LDH framework. The metal ions (Ni
Fig. 11. (a) Schematic representation of photocatalytic degradation of rose bengal (RB), Congo red (CR), and fast green (FG) dyes using Nd/ZnAl-LDH, (b)
Degradation products of CR after treatment using Nd/ZnAl-LDH, (c and d) LC-MS spectra of RB and CR after photocatalytic degradation using Nd/ZnAl-LDH, and (e)
Degradation products of CR after treatment using Nd/ZnAl-LDH. Reproduced with permission from Wani et al. (2022). Copyright 2021 Chinese Society of
Rare Earths.
18
and Co) efficiently connected the surface hydroxyl groups to perox methods have been investigated for the removal of heavy metals. Zhao
ymonosulfate (PMS), generating •OH and SO4•− radicals that eliminated et al. (2023c) developed models of different LDHs for the removal of
the dye (Deng et al., 2021). In this study, a CoFeNi-LDH/GO mixture was heavy metals using density functional theory (DFT) and molecular dy
used to activate persulfate (PS) for the degradation of the antibiotic namics (MD) simulations. Chemical binding, electrostatic interactions,
gatifloxacin (Deng et al., 2021). The combination of LDH with graphene and isomorphic substitution were the dominant mechanisms for the
oxide (GO) created a catalyst with a laminated structure. Under alkaline removal of five widespread heavy metals: Zn2+, Cu2+, Zn2+, Co2+, Ni2+,
conditions, 100% removal of gatifloxacin was achieved in just 20 min. and Cd2+. Additional insights have been provided on the impact of
However, acidic environments affected the performance of LDH/GO introducing vacancies (such as H or OH vacancies) into the (003) surface
composite and expedited metal leaching. The oxidation-reduction cycles on the removal mechanisms (Zhao et al., 2023c). The removal of heavy
of Fe2+/Fe3+ and Co2+/Co3+ on the catalyst exterior was reported to metals by LDHs primarily follows an electrostatic interaction mecha
achieve degradation of the antibiotic lomefloxacin, utilizing the CoFe- nism, irrespective of the presence or absence of vacancies. Based on the
LDH/PS system. Sulphate radicals played a significant role in the analysis of the energy barrier associated with the rate-determining step,
destruction process within the first 60 min of operation (Ma et al., 2020). it was inferred that the LDHs, specifically the defect-free (003) and
Considering an ultimate performance of 93.2% at a PS dosage of 1 g L− 1, defective (003) surfaces, exhibited an increased tendency for Cd2+
0.2 g L− 1 catalysts, as well as the solution of pH 5, sulphate radicals mineralization. In contrast, LDHs with OH and Ca vacancies were shown
significantly contributed to the destruction within the first 60 min of the to be more favorable for the mineralization of Cu2+. Finally, it was
operation (Karim et al., 2022). observed that the insertion of vacancies can have a significant impact on
Wani et al. (2022) synthesized Nd-doped ZnAl-LDH by using hy the isomorphic substitution of heavy metals, with Ca vacancies showing
drothermal process for photocatalytic degradation of different dyes the most significant effect (Zhao et al., 2023c). In another study, LiAl-
including congo red. The band gap of Nd-doped ZnAl-LDH enables the LDH was prepared to remove Zn2+ and Cu2+ via isomorphic substitu
degradation of congo red, rose bangal, and fast green dyes using visible tion and surface complexation mechanisms. (Zhao et al., 2020b).
light. When light of a certain wavelength falls on the surface of ZnAl- Different operating and environmental factors play vital roles in
LDH, electrons undergo a transition from the VB to the CB, creating water treatment technologies. The presence of defects in environmental
vacancies or holes in the VB. However, in semiconducting composites, catalysts has been extensively investigated and has been found to have
electron-hole pairs recombine rapidly, reducing photocatalytic effec significant effects on the material characteristics and overall efficacy. In
tiveness. The addition of Nd3+ to the ZnAl-LDH matrix improved pho a previous study, the removal of Cr(VI) from MoS2-lignin-derived carbon
tocatalytic efficiency by acting as an electron trap, slowing down (LDC) composites was significantly improved by the introduction of
recombination (Fig. 11). The separated electron-hole pairs combine with defects into the MoS2 layer (Chen et al., 2021a). Similarly, a monolayer-
dissolved oxygen to generate highly reactive OH radicals. The holes in structured MgAl-LDH, which was subsequently calcined at 350 ◦ C for 4
the VB react with H2O, producing more OH radicals. These reactive OH h, showed improved performance (Xiong et al., 2023). This calcination
radicals interact with the dye molecules on the surface of Nd/ZnAl-LDH, process resulted in the formation of a defective monolayer, MgAl-mono-
breaking them down into simpler byproducts. Experimental results 350. Characterization and computational analysis provided insights into
showed significant degradation of congo red, rose bangal, and fast green the properties of the MgAl-mono-350. This material exhibits a signifi
dyes, with reported degradation rates of 93%, 89%, and 85%, respec cant presence of oxygen defects, which play a crucial role in facilitating
tively. Table 5 provides detailed information on various advanced LDH- the stable removal of Cd2+ through an isomorphous substitution process.
based nanocomposites used as photocatalysts for the reduction of heavy As a result, Cd2+ was immobilized on the resulting LDH structure. The
dyes. MgAl-mono-350 material also exhibited exceptional selectivity towards
Cd2+ compared to other commonly detected heavy metals. This study
4.2.4. LDH-based composites for reduction of heavy metals showed the capability of defect-engineered LDH to effectively eliminate
Different types of LDH-based composites have been used for catalytic heavy metals from contaminated water through targeted elimination
reduction of heavy metals (Table 5). Due to their extremely toxic nature, processes (Xiong et al., 2023). In another study, TiO2− x with oxygen
it has become evident to scrutinize this problem of heavy metal pollution vacancies was synthesized using a solvothermal method to remove
using innovative approaches. Photocatalytic reduction of metals has heavy metals. Because U(VI) can be trapped by defective sites, TiO2− x
shown efficiency in recent years (Table 5), which is the reason why displayed exceptional performance in eliminating U(VI) (Song et al.,
scientist are working to synthesize different kind of novel LDH-based 2017). Defect engineering has also been utilized in the development of
composites. Sun et al. (2023) synthesized a Pd-SNS/MgAl-LDH as a high-performance adsorbents to remove heavy metals (Chen et al., 2022;
photocatalyst for the removal of Cr(VI). The photocatalytic efficiency Liu et al., 2024). The adsorption performance of LDH is influenced by
was enhanced by the strong connection between Pd-SnS nanoparticles their size and shape. The effect of particle size on removal was studied
and LDH nanosheets (Sun et al., 2023). Particularly, Pd-SnS/LDH het and found to show a positive correlation between the reduction in the
erojunctions with SnS and Pd contents achieved 99% removal after 40 particle size of MgAl–LDH and its removal capacity (Rojas, 2016).
min under visible light irradiation and exhibited efficient stability Zhao et al. (2023a) developed a unique NiFe-LDH/nitrogen self-
throughout experimental duration. Additionally, the Pd-SnS/LDH pho doped g-C3N4 (NFS/NCN) Z-scheme heterojunction and utilized for
tocatalyst kept its excellent stability after four consecutive cycles with photoreduction of Cr6+ (Fig. 12). To prepare NFS/NCN, NCN and NiFe-
no noticeable decrease in its ability (Sun et al., 2023). In another study, LDH were dissolved in ethanol. Thioacetamide was vigorously agitated
mesoporous MCM-41/ZnCr-LDHs were developed using co-precipitation with the above solution for 30 min at the ambient temperature. The
approach, and obtained high porosity, extensive surface area, excellent mixed suspension was then put into a reaction vessel and held there for
chemical stability, and a lot of surface-OH grafting sites. Under optimal 6 h at 120 ◦ C. After cooling down the precipitates, they were filtered and
conditions, amine-functionalized MCM-41/ZnCr-LDH nanocomposite repeatedly rinsed with ethanol and water. The Z-scheme heterojunction
demonstrated 95% of Cr6+ reduction in 2 h under visible light radiation, technique and the potential photoreduction process were coherent as
which was 1.2 times better than that obtained by unmodified MCM-41/ shown in Fig. 12b. Both NFS and NCN in the NFS/NCN composites may
ZnCr-LDH nanocomposite and 1.5 times better than the pure ZnCr LDH be stimulated by visible light, and similarly, photoinduced electrons (e− )
(Sahoo et al., 2021). and holes (h+) emerged. The photo-generated h+ on the VB of NCN then
LDHs can effectively eliminate heavy metals through interlayer interacted with the photo-generated e− on the CB of NFS, which swiftly
anion exchange, which involves the anchoring of anions, particularly moved to the interface between NFS and NCN. In this current situation, a
metals. Additionally, LDHs may eliminate heavy metals through significant amount of photo-generated h+ and e− were found on the VB
adsorption or isomorphic substitution inside the laminates. Various of NFS and the CB of NCN, respectively. Furthermore, the
19
Table 5
Selected examples of LDH-based composites for catalytic reduction of heavy metals.
Composite Precursors Synthetic method Source of light LDH Pollutant Contact pH Pollutant Efficiency Ref.
dose Concentration time
1
Ag@Ag3PO4/g- Ag3PO4 Electrostatic self- Visible light 0.02 g 20 mg⋅L− 2h 5 Cr6+ 97% (Nayak and
C3N4/NiFe- g-C3N4 assembly + In-situ Parida, 2018)
LDH Ni photoreduction
(NO3)2⋅6H2O
Fe
(NO3)3⋅9H2O
1
CoAl-LDH Al Co-precipitation Solar light 20 mg 10 mg⋅L− 1h 5 Cr6+ 99% (Das, 2021)
NiAl-LDH (NO3)3⋅9H2O
MgAl-LDH Co
(NO3)2⋅6H2O
Ni
(NO3)2⋅6H2O
Mg
(NO3)2⋅6H2O
1
ZnCr-LDH/MCM- Zn(NO3)2 Co-precipitation Visible light 0.02 g 20 mg⋅L− 2h 2 Cr6+ 97% (Sahoo et al.,
41 Cr(NO3)3 2021)
− 1 6+
AgBr@Ag/CoAl- Co Facile precipitation + Visible light 50 mg 50 mg⋅L 120 min 3 Cr 96% (Chen et al.,
LDH (NO3)2⋅6H2O Photo-assisted 2020)
Al reduction
(NO3)3⋅9H2O
AgNO3
NaBr
1
CuPd/MgAl- Mg Hydrothermal Visible light 40 mg 40 mg L− 40 min 5 Cr6+ 98% (Sun and Park,
LDH/g-C3N4 (NO3)2⋅6H2O 2022)
Al
(NO3)3⋅9H2O
NaBH4
CuCl2⋅2H2O
1
BiOI@ZnTi-LDH Bi(NO3)3 Hydrothermal Visible light 0.5 g 50 mgL− – 3 Cr6+ 96.3% (Xiong et al.,
Ethanediol L− 1 2020)
KI
Zn
(NO3)2⋅6H2O
1
ZnAl-LDH Zn Co-precipitation UV light 100 10 mg L− 5h 3.2 Cr6+ 100% (Yuan et al.,
(NO3)2⋅6H2O mg 2017)
Al
(NO3)3⋅9H2O
1
ZnAl-LDH/TiO2 Zn Sol-gel Ultraviolet 100 20 mg L− 150 min 2 Cr6+ 100% (Yang et al.,
(NO3)2⋅6H2O irradiation mg 2019)
Al
(NO3)3⋅9H2O
TiO2
1
ZnTi-LDH/ Zn Co-precipitation Xenon lamp 50 mg 10 mg L− 50 min 3 Cr6+ 100% (Chuaicham
Fe@MT20% (NO3)2⋅6H2O et al., 2021)
TiCl4
Fe
(NO)3⋅9H2O
1
NiAl-LDH Ni Hydrothermal – – 0.02 g L− 120 min – Pb2+ >95% (Wang et al.,
(NO3)2⋅6H2O Ag+ 2020b)
Al Cu2+
(NO3)3⋅9H2O
1
Fe3O4/ZnAl- Zn Sol-gel UV lamp 20 100 mg L− 8h 3 Cr6+ 98% (Yang et al.,
LDH/TiO2 (NO3)2⋅6H2O mg 2020b)
Al L− 1
(NO3)3⋅9H2O
Fe3O4
1
Pd/SnS/MgAl- Mg Hydrothermal Visible light 50 mg 50 mg L− 40 min 7 Cr6+ 99% (Sun et al.,
LDH (NO3)2⋅6H2O 2023)
Al
(NO3)3⋅9H2O
1
NiFe-LDH/OCN Ni Solvothermal Visible light 15 mg 30 mg L− – 7 Cr6+ 94% (Zhao et al.,
(NO3)2⋅6H2O 2022)
Fe
(NO3)3⋅9H2O
OCN
1
NiFe-LDH/NCN Ni Hydrothermal Visible light 15 mg 15 mg L− 90 min 3 Cr6+ 99% (Zhao et al.,
(NO3)2⋅6H2O 2023a)
Fe
(NO3)3⋅9H2O
NCN
1
MnFe-LDH/SiO2 MnCl2⋅4H2O Hydrothermal Mmaster TL-D 1g 25 mg L− 150 min 4 As3+ 98% (Mohapatra
FeCl3⋅6H2O Super lamp L− 1 Cr6+ 95% et al., 2022)
Si(OC2H5)4
20
Fig. 12. (a) Schematic illustration of NFS/NCN, (b) Schematic representation of predicted charge separation and photocatalysis, (c to h) SEM images of the
composites, and (I and j) TEM and HRTEM images of the composites. Reproduced with permission from Zhao et al. (2023a) Copyright 2022 Elsevier.
21
photogenerated e− on the CB of NCN had the capacity to reduce the Cr6+ of 7. The rejection of methylene blue by the ZWLDH-20 membrane was
into Cr3+. Meanwhile, the photo-generated h+ may directly react with 77% at a permeate flux of 180 L m− 2 h− 1 (Zhao et al., 2020a). To provide
the hole scavengers to form CO2 and H2O. As a result, the synthesized long-term advantages using adsorption for the elimination of micro
NFS/NCN composites displayed impressive photocatalytic reduction pollutants from wastewater, it is recommended that the adsorbents be
performance, and Cr6+ could be efficiently removed. Under visible light recycled as much as possible. Recently, the adsorption of the antibiotic
irradiation, the photoreduction of Cr6+ by NFS/NCN composite was ceftriaxone on 2D microspheres of ZnMgFe-LDH was investigated
90.52% (Zhao et al., 2023a). (Mohamed et al., 2023). The ZnMgFe-LDH achieved 99% elimination of
ceftriaxone, with the highest adsorption capacity of 242 mg g− 1 at pH 5.
4.2.5. LDH-based composites for membranes and electrocatalysis The used adsorbent, i.e., the ZnMgFe-LDH/CTX complex, was recycled
Organic micropollutants such as pharmaceuticals, pesticides, and as an electrooxidation catalyst in methanol fuel cells. The electro
industrial chemicals are diverse in nature and pose significant hazards to chemical performance of ZnMgFe-LDH/CTX was nearly ten times higher
human health and environmental ecosystems. Most organic micro than that of ZnMgFe-LDH. Recycling LDH-based adsorbents is an
pollutants are discharged into the environment through industrial ac economical approach (Mohamed et al., 2023). LDH-based membranes
tivities and end up in surface waters (Reddy et al., 2019). Owing to their have versatile applications for the removal of organic contaminants.
resistance to biodegradation, the water quality is severely compromised Establishing interactions between LDH and organic micropollutants is a
(Tegladza et al., 2021). Moreover, these micropollutants can bio crucial aspect in the application of adsorption, while in the case of
accumulate in tissues and climb the food chain. Therefore, it is crucial to photocatalysis, LDH-based catalysts must act as activators (Sajid et al.,
eliminate organic micropollutants from wastewater before its further 2022). In another study, an LDH-based membrane was shown to activate
use (Hassan et al., 2020). In recent years, interface engineering of LDH peroxymonosulfate to generate reactive oxygen species that can elimi
into membranes has received significant attention owing to its efficacy nate a range of organic micropollutants (Asif et al., 2022). Research on
compared to batch systems. LDH-based membranes have been used to LDH-based membranes is still in its inception phase and is expected to
treat diverse organic micropollutants. In a study (Raicopol et al., 2019), gain momentum in the near future because of their scale-up potential.
cellulose acetate (CA)/MgAl-LDH membrane was developed to remove Another emerging approach involves the electrocatalytic degrada
two pharmaceuticals, namely diclofenac and tetracycline via an tion of organic micropollutants. A wide spectrum of organic micro
adsorption mechanism. An increase in the LDH loading rate in the pollutants has been eliminated using electrocatalysis, such as electro-
polymer matrix resulted in a reduction in the pore size. The addition of 4 Fenton and electro-oxidation processes. The heterogeneous electro-
wt% MgAl-LDH led to a substantial enhancement in water flux, reaching Fenton (EF) strategy is highly promising for micropollutant-
529 L m− 2 h− 1, compared to the water flux of the pristine CA membrane, contaminated wastewater treatment. The EF process can produce
which was only 36 L m− 2 h− 1. The LDH layers in the polymer matrix hydrogen peroxide on-site and can function effectively across a range of
were completely exfoliated. Owing to the electrostatic interactions be pH values without producing any metal residue. Nonetheless, the het
tween the positively charged LDH layers and negatively charged diclo erogeneous EF method requires bifunctional cathode electrodes that
fenac, the CA/MgAl-LDH membrane achieved ten-fold better adsorption exhibit exceptional performance in redox reactions and H2O2 break
than the CA membrane. Similar observations were made for tetracycline down. For instance, the electrophoretic deposition approach to deposit
adsorption caused by hydrogen bonding (Raicopol et al., 2019). Simi ZnFeV-LDH on a graphite felt cathode, which served as a heterogeneous
larly, a CoAl-LDH membrane was developed by growing it directly on a electrocatalyst, was explored (Keyikoğlu et al., 2023). The resulting
tubular alumina support. The LDH was calcined to reduce its surface product was referred to as ZnFeV-LDH@GF. The ZnFeV-LDH@GF
energy and roughness. Furthermore, it enhances the permeability of the cathode showed the potential to produce 59.8 ± 5.9 mg L− 1 of H2O2
membrane by eliminating intercalated anions and increasing their within 90 min, while being supplied with a constant supply of O2. The EF
porosity. The uncalcined and calcined LDH-based composite membranes method, utilizing a cathode composed of ZnFeV-LDH@GF, demon
were assessed to evaluate their suitability for dye rejection. The alumina strated an elimination efficacy of approximately 90% for the tested
support membrane exhibited a rejection of only 7% for the Eriochrome pharmaceutical (i.e., ciprofloxacin) at a pH of 7. The apparent reaction
Black T dye. On the other hand, the rejection was above 98% for the rate constant of ZnFeV-LDH@GF-EF is 2.14 times greater than that of the
LDH- and calcined LDH-based membranes. The permeance of the EF process using pristine GF. The application of ZnFeV-LDH coating
calcined LDH-based membrane was 1.8 times higher compared of the resulted in a significant increase in the generation of •OH from 1.74 mM
other tested membranes. The calcined LDH-based membrane main to 3.65 mM. The mechanism of •OH generation is speculated to include a
tained its performance for 110 h during the nanofiltration process, with single-electron transfer from the Fe2+/Fe3+ and V4+/V5+ redox couples
no notable reduction in permeance or rejection efficiency. Notably, the to H2O2. The ZnFeV-LDH@GF cathode maintained 90% removal of the
permeance of the uncalcined LDH-based composite membranes tested pharmaceuticals, even after 10 cycles. Importantly, ZnFeV-
decreased after 10 h. The calcined LDH membrane demonstrated LDH@GF-EF completely eliminated ciprofloxacin from the wastewater
improved stability and permeance in the removal of dyes from waste within 210 min. Moreover, the developed system demonstrated efficacy
water. The results revealed that this calcination strategy is effective for in eliminating several types of micropollutants, such as dyes, pharma
improving the separation efficiency of LDH-based membranes (Huang ceuticals, and pesticides (Keyikoğlu et al., 2023). In another study, the
et al., 2020). electro-oxidation degradation of tetracycline using an FeCo-LDH-based
Membrane-based separations have been combined with photo anode was investigated. It was observed that P-doping aids in the
catalytic degradation through the deposition of a layer of photocatalysts desorption of hydrogen, while the deposition of Cu-nanodots accelerates
onto the surface of the membranes. The integration of membrane-based the splitting of molecules, leading to an increased generation of •OH.
separation and photocatalysis not only improves pollutant removal but Cu/P-FeCo-LDH exhibited exceptional tetracycline degradation across
also reduces the membrane fouling propensity. Therefore, effective all tested pH levels compared with the unmodified FeCo-LDH anode.
membrane-based photocatalysis is an attractive technology for water This is due to the fact that it possessed a reduced energy barrier of 0.6 eV
treatment. The use of NiAl-LDH in conjunction with other materials has for the generation of •OH compared to the pristine FeCo-LDH anode
been reported as a feasible approach to develop a highly effective pho (Feng et al., 2022). Despite these promising results, the application of
tocatalytic system. ZnWO4/NiAl-LDH composites were prepared as a LDH-based electrocatalysts for the degradation of micropollutants is
coating layer on commercially available PVDF membranes for photo limited to lab-scale investigation.
catalysis (Zhao et al., 2020a). The ZWLDH-20 nanocomposite exhibited
the best photocatalytic degradation of methylene blue dye, reaching
approximately 94% within 90 min under visible-light irradiation at a pH
22
5. Conclusion and future prospects matrices and operating conditions to investigate the practica
bility of LDHs, as most published studies are limited to labo
This study comprehensively discusses the progress in the LDH and ratory tests using distilled water.
LDH-based materials for water treatment. Despite significant advances
in research on LDH, future research should focus on following the CRediT authorship contribution statement
followings:
Ahmad Farhan: Conceptualization, Data curation, Methodology,
▪ The synthesis of composite materials based on LDHs often in Writing – original draft. Aman Khalid: Data curation, Investigation,
volves slow pyrolysis and traditional modification procedures, Writing – original draft. Nimra Maqsood: Data curation, Writing –
which require rigorous acidic or alkaline treatment, high tem original draft. Sidra Iftekhar: Visualization, Writing – review & editing.
peratures, high pressure, or powerful oxidation/reduction re Hafiz Muhammad Adeel Sharif: Visualization, Writing – review &
actions. It is crucial to prioritize the development of innovative, editing. Fei Qi: Validation, Writing – review & editing. Mika Sillanpää:
simple, cost-effective, and environmentally sustainable modi Visualization, Writing – review & editing. Muhammad Bilal Asif:
fication techniques, which are specifically designed for LDH- Project administration, Resources, Visualization, Writing – review &
based adsorbents. These advancements will contribute to the editing.
scale-up of LDH-based adsorbants in water treatment.
▪ Researchers are currently conducting extensive investigations
into the adsorption mechanism, including the adsorption of Declaration of competing interest
high-valent heavy metal ion such as Cr6+. It has been observed
that Cr6+ in the form of CrO2− 4 can be reduced to Cr
3+
when The authors declare that they have no known competing financial
exposed to LDHs-based composites. However, the exact mech interests or personal relationships that could have appeared to influence
anism of this reduction process has not been fully understood. the work reported in this paper.
Questions such as the impact of the LDH type on the reduction
of Cr6+ and the specific structure or functional group involved Data availability
in this process remain unexplored. Similarly, the precise
mechanism of adsorption for the elimination of Pb2+ and Cd2+ Data will be made available on request.
is still a topic of debate. Nevertheless, there is a general
consensus that a comprehensive understanding of the adsorp
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Progress in layered double hydroxides (LDHs): Synthesis and application in

• Layered double hydroxides (LDHs) show

1. Introduction focused on synthetic and functionalization of LDHs, as well as adsorp

Fig. 1. A schematic representation of LDH structure (Gao et al., 2014).

Fig. 2. A generic route to the synthesis of crystalline LDH.

Fig. 6. Mechanism of methyl orange (MO) adsorption by MgAl-LDH.

NiCo-LDH/ Ni(NO3)2⋅6H2O Green 2.0 mg Hg2+ 250 mg L− 1

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Science of the Total Environment

Progress in layered double hydroxides (LDHs): Synthesis and application in

• Layered double hydroxides (LDHs) show

1. Introduction focused on synthetic and functionalization of LDHs, as well as adsorp­

Fig. 1. A schematic representation of LDH structure (Gao et al., 2014).

Fig. 2. A generic route to the synthesis of crystalline LDH.

Fig. 6. Mechanism of methyl orange (MO) adsorption by MgAl-LDH.

NiCo-LDH/ Ni(NO3)2⋅6H2O Green 2.0 mg Hg2+ 250 mg L− 1

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1. Introduction focused on synthetic and functionalization of LDHs, as well as adsorp