shen2021_good

Environmental Science and Pollution Research (2021) 28:7599–7620
https://doi.org/10.1007/s11356-020-11877-8
REVIEW ARTICLE
Recent advances in the application of magnetic Fe3O4 nanomaterials

for the removal of emerging contaminants
Yaoxin Shen 1,2 & Bo Jiang 1,2,3 & Yi Xing 1,2
Received: 24 April 2020 / Accepted: 29 November 2020 / Published online: 4 January 2021
# The Author(s), under exclusive licence to Springer-Verlag GmbH, DE part of Springer Nature 2021
Abstract
Emerging contaminants (ECs) are widely distributed and potentially hazardous to human health and the ecological system.
However, traditional wastewater treatment techniques are not sufficient to remove ECs. Magnetic nanomaterials are made of
ferromagnetic or superparamagnetic magnetic elements such as iron and nickel, which can be easily separated from the aqueous
solution, making them ideal adsorbents for contaminants in water. This review focused on the synthesis approaches of magnetic
Fe3O4 nanoparticles (MFNs), as well as surface modification in order to improve their stability and functional diversity. Also, a
detailed summary on the state-of-art application of magnetic nanomaterials on the removal of ECs was addressed. Additionally,
challenges and future prospective of applying magnetic nanomaterials into real-world cases were discussed, in which the green
and simple synthesis and evaluation of the toxic effects of MFNs are still of great challenge. This work summarizes the recent
progress of using magnetic nanomaterials as promising and powerful tools in the treatment of ECs-contaminated water, benefit-
ing researchers interested in nanomaterials and environmental studies.
Keywords Emerging contaminants (ECs) . Magnetic nanoparticles . Environmental remediation . Synthesis
Introduction contaminants in water bodies (Jurado et al. 2019), convention-

al wastewater treatment technology is insufficient to remove
Emerging contaminants (ECs), such as pesticides, antibiotics, ECs. This work presents a detailed summary of recent progress
endocrine disruptors (EDCs), and pharmaceutical and personal in ECs, including their possible hazards, detection methods,
care products (PPCPs), are a group of naturally occurring or and removal approaches, which can improve the understand-
synthetic organic compounds, which attract public and scien- ing of the toxic mechanisms of ECs and the interaction be-
tific attention owing to their wide range of distribution and tween ECs and the ambient environment, as well as providing
potential severe risks to human health and the ecological sys- solution for the removal and treatment of ECs in the environ-
tem (Agas et al. 2018), particularly to aquatic organisms ment. Particularly, the application of magnetic Fe3O4 nanopar-
(Sarkar and Singh 2018). Also, since the concentrations of ticles (MFNs) in the removal of ECs has drawn great attention
the widely spread ECs are much lower than those of other in recent decades. The synthesis approaches of MFNs, their
use in the removal of ECs, as well as the challenges and future
Responsible Editor: Philippe Garrigues prospective are addressed, serving as powerful tools for their
application in wastewater treatment of ECs.
* Bo Jiang
[email protected]
1
Characteristics, detection, and removal of ECs
School of Energy and Environmental Engineering, University of
Science & Technology Beijing, Beijing 100083, People’s Republic
of China Types of ECs
2
Beijing Key Laboratory of Resource-Oriented Treatment of
Industrial Pollutants, University of Science & Technology Beijing, Pesticides
Beijing 100083, People’s Republic of China
3
National Engineering Laboratory for Site Remediation Technologies, Pesticides, a group of chemical agents, are used in agriculture
Beijing 100015, People’s Republic of China to control the negative effects posed by pests and microbes
7600 Environ Sci Pollut Res (2021) 28:7599–7620
and optimize plant growth conditions (Sun et al. 2018b). By ciprofloxacin in the estuaries of the Basque Country and the
far, the pesticide abuse problem has drawn significant con- Gorliz WWTP was 3803 ng/L (Mijangos et al. 2018). He et al.
cerns on food safety, agricultural sustainability, and the eco- investigated 43 antibiotics from 14 sites along the Eastern
logical environment (Jin and Fang 2018). Based on their Shore of the Chesapeake Bay, suggesting that norfloxacin
chemical structures, pesticides are classified into organochlo- (94.1 ng/L), enrofloxacin (17.8 ng/L), sulfamethoxazole
rine pesticides, organophosphorus pesticides, organic nitrogen (14.8 ng/L), and clarithromycin (9.7 ng/L) were at the highest
pesticides, organic sulfur pesticides, organic mercury pesti- concentrations in the investigated area (He et al. 2019).
cides, carbamate pesticides, and pyrethroid pesticides. Due
to their persistence in the environment, pesticide residues Drinking water disinfection by-products
may induce serious health problems to humans. For example,
organochlorine pesticides can lead to chronic toxicity and var- Drinking water disinfection by-products (DBPs) are the by-
ious neurological diseases to humans via bioaccumulation products formed by chemical reactions of the disinfectants
along food chain (Han et al. 2019a, b). Though the use of (chlorine, ozone, chlorine dioxide, or chloramine) with organic
organochlorine pesticides has been banned since 1983 in substances in the process of drinking water disinfection (Hu
China, some are still detectable until now. The Pearl River et al. 1999). Huang et al. conducted a 12-month investigation
Delta in South China is one of the most typical areas with on the concentration of DBPs in drinking water in China, dem-
high concentrations of organochlorine pesticides, e.g., dichlo- onstrating that the concentrations of the THMs, three
rodiphenyltrichloroethane (DDT) at 12.50 ng/L (Ivorra et al. trihaloacetaldehydes (THAs), four haloacetonitriles (HANs),
2019). Also, as a typical kind of pesticides, pentachlorophenol and four haloacetamides (HAcAms) were 1.3–74.8 μg/L, 0.1–
has been banned for decades due to its long-term durability. 11.4 μg/L, ≤ 6.4 μg/L, and 0.1–3.1 μg/L, respectively (Huang
However, pentachlorophenol is still detected in groundwater et al. 2017). Chowdhury investigated the occurrence of THMs
(Zhang et al. 2019a). Organophosphorus pesticides could ac- and HAAs in Newfoundland and Labrador, Canada, suggesting
cumulate in human body via food chain, causing toxic effects that the average concentrations of THMs and HAAs were 97.6
by inhibiting acetylcholinesterase (AChE) activity and threat- and 129.2 μg/L in surface water and 29.1–43.5 and 15.8–64.3
ening central nervous system (Jiang et al. 2018a). μg/L in groundwater (Chowdhury 2017). The carcinogenicity
of DBPs have long been investigated and demonstrated that
Antibiotics exposure to THMs, e.g., chloroform, was positively correlated
to bladder cancer and rectum cancer (Larson et al. 1993).
Antibiotics are widely used to treat microbe-induced diseases
and are also applied at sub-therapeutic levels via animal feed Brominated flame retardant
to maintain meat quality and quantity (Jin et al. 2017).
Antibiotics are difficult to be absorbed and degraded by or- Brominated flame retardants (BFRs), such as polybrominated
ganisms, and nearly 80–90% are released into the environ- biphenyls (PBBs), and polybrominated diphenyl ethers
ment via urine and feces (Han et al. 2019a, b). The main (PBDEs), with low cost and excellent flame retardant proper-
categories of antibiotics existed in the environment include ties, are usually added in in electronic products in order to
tetracycline, sulfonamide, macrolide, quinolone, aminoglyco- reduce the risk of fire during the use of electrical and electron-
side, β-lactam, and glycopeptide (Tran et al. 2018). ic equipment (Miller et al. 2015). BFRs can interfere with the
Antibiotics can interfere with photosynthesis and metabolism endocrine system, immune system, and nervous system of the
of biomes, resulting in potential risks to aquatic and terrestrial organism, and particularly thyroid hormones and sex hor-
organisms (Martin-Laurent et al. 2019). Woodhead et al. in- mones (Legler 2003).
vestigated the toxicity of five macrolides, suggesting that the Restrictions on BFRs have been established worldwide.
toxic mechanism of solithromycin and clarithromycin is pri- PBDEs have been newly listed as POPs in the Fourth
marily due to the inhibition of the mitochondrial electron Conference of the Parties to the Stockholm Convention,
transport chain. Furthermore, although the environment- 2009. The US state government also established restrictions
present concentrations of antibiotics are at trace levels (ng/L on flame retardants in 2013. The European Union Directive on
to μg/L), exposure to antibiotics can alter microbial commu- the Restriction of the Use of Certain Hazardous Substances
nity in the environment, and microbes may acquire antibiotic (RoHS) in electrical and electronic equipment has regulated
resistance due to increasing abundance of antibiotic resistance the concentrations of PBBs and some PBDEs in plastics lower
genes (ARGs) (Gong et al. 2018). than 1000 mg/kg.
Antibiotics and their residues are ubiquitously found in A previous report found that PBDEs in surface water of the
aquaculture and poultry farming, as well as natural water bod- Three Gorges Dam region, China, ranged from 2.0 to 17.6 and
ies and wastewater treatment plant (WWTP). Mijangos et al. 0.8 to 11.1 ng/L in the upstream and downstream, respectively
reported that the highest detectable concentration of (Ge et al. 2014). Another recent investigation revealed that
Environ Sci Pollut Res (2021) 28:7599–7620 7601
ΣPBDE concentrations in Bay sediment were < 5 ng/g dry livestock (Daughton 2004). PPCPs in aqueous environments
weight (dw) in the San Francisco Bay water (Sutton et al. 2019). are present in trace concentrations (generally ng/L) (Pérez-
Lemus et al. 2019). Mijangos et al. conducted a survey on
Perfluoro organic compounds 41 multiclass PPCPs in three estuaries of the Basque
Country, demonstrating high concentrations of PPCPs, in-
Perfluorinated compounds (PFCs) are a general term for syn- cluding sulfamethoxazole (8963 ng/L) , trimethoprim (5843
thetic organic compounds in which hydrogen atoms bonded to ng/L), sucralose (4532 ng/L), valsartan (1811 ng/L) and
a carbon atom are completely replaced by fluorine atoms acesulfame (1261 ng/L) in Gorliz WWTP (Mijangos et al.
(Meinert 1994). It mainly includes perfluorooctane acids 2018). Another case found that concentrations of atenolol,
(PFOAs), perfluorooctane sulfonate (PFOS), metoprolol, venlafaxine and chloramphenicol in four sewage
perfluorobutanesulfonate (PFBS), perfluorocarboxylic acids treatment plants in Hong Kong were up to ng/L to mg/L in
(PFCAs), perfluorinated sulfonic acids (PFSAs), and fluoro- both influent and effluent (Ruan et al. 2019).
carbons (fluorotelomer alcohols, FTOHs) (Keerthi 2005).
PFCs have unique hydrophobic and oleophobic properties Endocrine disruptors
and strong surface activity; therefore, they are widely used
in the synthesis of industrial chemicals, e.g., surfactants, flame Endocrine disrupting compounds (EDCs), including natural
retardants, and coating additives. The development, produc- endocrine disruptors and synthetic endocrine disruptors such
tion, use, and disposal of a large number of products contain- as environmental estrogens (polyhalogen compounds, pheno-
ing PFCs have allowed them to migrate to environmental me- lic compounds, phthalates, pesticides, and PPCPs), have the
dia and organisms through various pathways (Hoff et al. character of hydrophobicity, low-concentration effect, and
2003). PFCs are reported with oxidative stress, acute toxicity, long half-life (Quynh and Toan 2019). EDCs are drawing
inhibition of growth, hepatotoxicity, cardiovascular toxicity, increasing concern as they are being detected globally, and
thyroid toxicity, neurotoxicity, immune system toxicity, and some EDCs can harm the physiology of organisms, e.g., fish
potential carcinogenicity (Hagenaars et al. 2013). The WHO and mammals, leading to endocrine abnormalities and organ
IARC has divided perfluorooctanoic acid and its salts into variation (Xi et al. 2013). Exposure to EDCs results to disrup-
human suspected carcinogens and classified as Category 2B. tion or imbalance of the systemic hormonal regulation of the
Strict regulation on PFCs has been established in the last skeleton including bone modeling and remodeling, local hor-
decades. In 2009, nine PFOS and its salts were listed as new mones, and cytokine/chemokine release (Agas et al. 2018).
POPs in the Stockholm Convention; thereafter, the production Cesen et al. reported a high concentration of caffeine in the
and usage of PFOS is eventually eliminated. In January 2017, wastewater of three Slovenians and three WWTPs at 283–
the European Union’s REACH (Registration, Evaluation, and 1390 ng/L. Several bisphenols were quantified for the first
Authorization of Chemicals) regulation included seven time in Europe in 2017, with the average concentrations rang-
perfluorinated substances of high concern. USEPA has com- ing from 0.704 to 476 ng/L (Cesen et al. 2019). Zhou et al.
pleted banned PFOA in 2015, as well as mandating a health conducted an investigation on 21 kinds of EDCs in
advisory level of PFOA and PFOS in drinking water at 70 ng/ Xiangjiang River, demonstrating that the concentrations of
L. Sweden issued a statement prohibiting PFOS from entering bisphenol A, 4-tert-octylphenol, 4-n-nonylphenol, estrone,
the Swedish market and strictly controlling the entry of PFOS. and 17β-estradiol were at ng/L, and those of alkylphenols
However, due to the persistence of PFCs, they are still and caffeine ranged from 0.8 to 3.1 × 103 ng/L and 0.1 to
detected with high concentration in the environment. 49.8 ng/L, respectively (Zhou et al. 2019).
Newton et al. investigated the occurrence of PFCs in surface
water and sediment of the Tennessee River, revealing that Organic ultraviolet absorbents
PFOS, PFBS, and PFOA were the most abundant, with con-
centrations up to 220, 160, and 120 ng/L, respectively UVAs, including organic UV filters and UV stabilizers, are
(Newton et al. 2017). Schaider et al. detected PFCs from 20 beneficial in protecting against UVA (320–400 nm) and UVB
public drinking water supply wells at Massachusetts, USA, (280–320 nm) radiation (Tang et al. 2018). Organic UV filters
suggesting that the maximum concentration of PFOA and are widely used in sunscreens and other cosmetics, and UV
PFOS was 22 and 97 ng/L, respectively (Schaider et al. 2014). stabilizers are mainly used in textiles, plastics, paints, adhe-
sives, and other polymer materials to prevent the aging and
Pharmaceutical and personal care products degradation of polymers under sunlight irradiation (Li et al.
2018b). According to the chemical structure, UVAs can be
Pharmaceutical and personal care products (PPCPs) refer to divided into salicylates, benzophenones, benzotriazoles,
products which are primarily used for personal health and substituted acrylonitriles, triazines, and hindered amines
cosmetic purposes or to enhance the growth and health of (Kehayoglou et al. 1997). In 2018, Hawaii passed a bill
banning the use of sunscreens containing benzophenone and developed a sensitive amperometric acetylcholinesterase
2-ethylhexyl-4-methoxycinnamate, drawing attention to the (AChE) biosensor based on SnO2 nanoparticles, carboxylic
issue of contamination by organic UV filters (Schneider and graphene, and Nafion-modified glassy carbon electrode for
Lim 2019). Tang et al. studied the distribution of UVAs in the detection of methyl parathion and carbofuran. The detec-
Chao Lake and its inflowing rivers, demonstrating that the tion limits of methyl parathion and carbofuran were 5 × 10−14
concentrations of total 12 UVAs (Σ12 UVAs) ranged between M and 5 × 10−13 M, exhibiting high sensitivity and acceptable
162 and 587 ng/L in water and 9.70 and 178 ng/g in sediment stability (Zhou et al. 2013). Lu et al. synthesized one-
(Tang et al. 2018). dimensional bimetallic Pd@Au core-shell nanorods with uni-
form Au shell, which was applied to construct a highly sensi-
Detection methods of ECs tive acetylcholinesterase (AChE) biosensor, with the detection
limit of 3.6 pM for organophosphate pesticides (Lu et al.
Chemical detection methods 2018). However, the biological approaches are often contro-
versial for their unstability and unreliability, as biological el-
Chemical analysis, e.g., UV-Vis, GC-MS, GC-MS/MS, and ements are easy to be affected by environmental factors
LC/MS, is the most commonly used for the detection of ECs (Monteleone et al. 2013).
according to their physical and chemical properties (Hassine
et al. 2012). Sikder et al. (2018) determined the concentration Conventional approaches for the removal of ECs from
of soluble silver nanoparticles in seawater rapidly by UV-Vis, water bodies
and the results showed good agreement with those obtained by
ICP-MS. However, the trace level of certain ECs in water ECs can be removed from the aqueous phase via physical,
bodies may be lower than the detection limits of the analytical chemical, and biological approaches, or their combination.
equipment, thereby cannot be easily determined via these Physical methods mainly include coagulation sedimentation,
well-established standard analytical instrumentation. Also, adsorption, and membrane process. Chemical methods in-
chemical analyses are not available for rapid and fast screen- volve in advanced oxidation process, photocatalytic degrada-
ing of ECs in emergency situations due to its complex pre- tion, and activate persulfate degradation. Biological methods
treatment of samples, laborious manual operation, and long include bacterial, fungal, and algae degradation, which utilizes
duration for detection (usually several hours to several days). bacteria, fungi, and algae to mineralize contaminants into sim-
Other protocols, such as the magnetic nanoparticles which can ple small molecules (Norvill et al. 2016), e.g., water and car-
bound to the target surface and quickly be separated by apply- bon dioxide.
ing an external magnetic field, are used to simplify the pre-
treatment of chemical analysis. Yan et al. synthesized a novel Physical methods
type of 3-fluorobenzoyl chloride functionalized magnetic
nanoparticles (Fe3O4@SiO2@FBC) for the extraction and de- Coagulation sedimentation is mature and widely used for the
termination of perfluorinated compounds (PFCs). By cou- removal of contaminants. However, coagulation sedimentation
pling with ultra-high performance liquid chromatography is believed not to effectively remove ECs by comparison with
with tandem triple quadrupole mass spectrometry (UHPLC- other conventional contaminants (Bonvin et al. 2016).
MS/MS), the detection limits of PFCs ranged from 0.01 to Westerhoff et al. examined the removal of 60 kinds of PPCPs
0.06 ng/L (Yan et al. 2013). and EDCs in drinking water source by coagulation and precip-
itation via aluminum sulfate. However, the removal rate of 46
Biological detection methods kinds of ECs was less than 20%, compared to that of polycyclic
aromatic hydrocarbons at 60–80% (Westerhoff et al. 2005).
Compared with traditional chemical approaches, biological Adsorption removes pollutants by porous, multi-active ad-
approach for ECs detection is rapid, easy to operate, and sorptive materials through electrostatic attraction, ion ex-
cost-effective, and therefore with high throughput and avail- change, complexation, and coordination (Bonvin et al.
able as a fast screening approach for ECs (Jiang et al. 2017). 2016). Adsorption has the advantages of low cost, easy to
Additionally, biological approach is feasible for evaluating the operate, and high removal efficiency, without secondary pol-
toxic effects and bioavailability of ECs on organisms (Unnati lution (Tahmasian and Morsali 2012). Common adsorbent
et al. 2019). Both traditional biomonitoring technologies, e.g., materials, with large surface area and rich in functional
bioindicators and biomarkers, and emerging biology tech- groups, such as -OH, -COOH, and -SH, include activated
niques, e.g., biosensors and immunoassays, are involved in carbon (Zhang et al. 2016a, b), zeolites and clay minerals
ECs detection (Rahman et al. 2018). Among them, biosensors (Torrellas et al. 2015), and nanomaterials (Hu et al. 2019).
are considered one of the most promising technologies for Traditional adsorptive materials are reported with good re-
direct detection of ECs (Zhou et al. 2017). Zhou et al. moval effects on ECs. However, traditional adsorbents are
expensive and difficult to regenerate, in which the desorption to generate sulfate radicals and improve the oxidation ability
process is affected by many factors, e.g., the nature of the of inactivated persulfate, including heat, radiation, alkali, and
adsorbent itself, the physicochemical properties of the adsor- transition metal (Wacławek et al. 2017). Wang et al. (2018b)
bate, and the chemical properties and composition of the so- used ultraviolet to activate persulfate and degrade dibutyl
lution (Almomani et al. 2020). Therefore, it is urgent to de- phthalate (DBP), suggesting that the increasing persulfate
velop adsorption materials with high stability, large adsorp- dose could enhance the degradation of DBP when persulfate
tion capacity, and easy recycling. dose was below 1.6 mmol/L. Additionally, the combination of
The membrane is a material with selective separation func- two or more composite ways to activate persulfate is also used
tion. The process of separation and purification of different to improve contaminant removal efficiency. Memarian et al.
components by selective separation of the membrane is called compared ultrasonic and ultrasonic/thermal activation of per-
membrane separation. Membranes used in water treatment sulfate degradation of 3,4 dihydropyrimidines, and the degra-
mainly include microfiltration (MF), ultrafiltration (UF), dation rates were 20% and 99.3%, respectively (Memarian
nanofiltration (NF), and reverse osmosis (RO) (Zhang et al. and Farhadi 2008).
2020a, b). The membrane process has the advantages of con-
venient operation, high removal efficiency, and no secondary Biological methods
pollution, possessing good retention of new contaminants.
Egea et al. applied RO to remove ECs including caffeine, Compared to physical and chemical approaches, biological
theobromine, theophylline, amoxicillin, and penicillin G, with methods are easier to implement on a large scale without sec-
100% removal of the contaminants (Egea-Corbacho Lopera ondary pollution (Del Alamo et al. 2018). Kassotaki et al.
et al. 2019). However, membrane fouling and cleaning are (2019) demonstrated the capacity of heterotrophic biomass
currently the biggest obstacles, as well as other limiting factors in conventional activated sludge for the removal of estrone,
such as high energy consumption and large quantities of high- 17β-estradiol, and estriol. Lucas et al. (2016) regarded the
ly concentrated contaminants (Wang et al. 2017). fungal treatment as an alternative wastewater treatment for
the elimination of forty-seven antibiotics, with 77% of antibi-
Chemical methods otics removed after the fungal treatment. However, removal
efficiency of biological methods is sometimes low and unsta-
Traditional advanced oxidation is now the most promising ble. Also, nutrients are required to sustain microbial growth
chemical approach for the removal of contaminants, but in- for biodegradation (Cajthaml et al. 2009).
complete oxidation may produce unknown active by-products
with potential toxicity which is even higher than that of the
contaminants themselves (Richardson et al. 2007). Advanced Characteristics and synthesis of magnetic
oxidation technology is characterized by the generation of Fe3O4 nanoparticles
hydroxyl radicals (·OH) with strong oxidation ability (Yang
et al. 2009). The organic compounds that are difficult to de- Nanomaterials refer to materials that have at least one dimen-
grade by large molecules are oxidized into low-toxic or non- sion in nanometer scale (0.1–100 nm) or are composed of
toxic small molecules (Glaze et al. 1987). Mansouri et al. them as basic units. Nanomaterials can be viewed as both
(2019) investigated several advanced oxidation processes in- materials and atoms (Jiang et al. 2018b) endowing them with
cluding O3/H2O2, O3/TiO2, O3/activated carbon, O3/Al2O3, good physical and chemical properties, e.g., small size effects,
O3/Fe2+/H2O2, and UV/TiO2 on the removal of diethyl phthal- surface chemical effects, and unique optical, electrical, cata-
ate (DEP), suggesting that the O3/Al2O3 process was the most lytic, thermal, and magnetic properties, as well as accessible
efficient, however, with a large energy consumption once ap- quantum behaviors, e.g., macroscopic quantum tunneling ef-
plied on an industrial scale. fects (Vunain et al. 2016). Nanomaterials can be used in en-
As the ozonation process is usually of high cost, it is often vironmental remediation or clean-up to bind with and neutral-
assisted by photocatalysis (Benitez et al. 2013). Wang et al. ize toxins.
(2019) prepared photocatalysts of Bi-doped TiO2 nanocom- Magnetic nanomaterials are nanomaterials with
posites supported by powdered activated carbon (PAC), and superparamagnetic property, which enables them to maintain
the degradation rate of sulfamethazine reached 81.18% in structurally stable (Netto et al. 2013). Superparamagnetism
300 min under visible light irradiation at 400–780 nm. is when an external magnetic field is applied, the electrons
Another newly developed advanced oxidation technology in the atomic orbital are arranged in an orientation to gen-
is persulfate oxidation by activating persulfate (PS/PMS) to erate magnetism. When the applied magnetic field disap-
generate sulfate radicals (SO4·-), which is efficient, thorough, pears, the electrons in the material can rapidly restore the
environment-friendly, highly selective, and mild in reaction disordered arrangement, making the magnetism disappear
conditions (Waldemer et al. 2007). Persulfate activators are (Britos et al. 2019). Compared with non-magnetic materials,
magnetic nanomaterials are economic feasible and environ- Chemical synthesis method
mentally friendly. With the relatively large surface area for
high mass transference, as well as magnetic property that Chemical methods for MFNs synthesis are usually easy to
can be easily separated from the aqueous solution, magnetic operate, however, with relatively strict reaction conditions
nanomaterials are particularly beneficial on the solid-liquid and high energy consumption. The principles, operation con-
separation in adsorption process for wastewater treatment ditions, as well as advantages and disadvantages of each
(Adeleye et al. 2016). chemical synthesis method are addressed.
Magnetic materials in environmental application include
pure metal (Fe, Co, Ni), cobalt oxide (Co3O4), nickel oxide Co-precipitation method Co-precipitation is operated under
(NiO), iron oxide (Fe2O3, Fe3O4), iron sulfide (FeSX), and the protection of inert gas, such as nitrogen or argon, in which
metal alloy (Fe–Pt, Al–Ni). Due to the toxicity of Co, Ni, a suitable ratio of mixed iron salt and ferrous salt solution are
and the complex composition in wastewater, some toxic sub- prepared and mixed with a suspension solution, followed by
stances may be produced when the Co and Ni magnetic ma- an alkaline precipitant (usually NaOH or ammonia as a pre-
terials are used, and these residual substances still exist in cipitant), thereby obtaining MFNs (Abboud et al. 2015).
wastewater after magnetic separation (Javed and Usmani Co-precipitation method is simple and easy to operate,
2013). Nano iron sulfide has stronger adsorption, reduction, while the size and morphology of particles are not easy to
and co-precipitation capability for heavy metal ions (Su et al. control. Also, the nanoparticles are easy to be oxidized and
2015). However, the introduction of sulfur causes various an- agglomerated (Yang et al. 2018). The co-precipitation method
ion and anion existing in the natural environment and affect- was further modified aiming at improving surface oxidation
ing the reaction process (Kim et al. 2013). Fe-Pt alloy can be and agglomeration of nanoparticles by adding surfactant or
divided into disordered face-centered cubic structure and or- assisted by ultrasound. Poddar et al. (2018) applied co-
dered face-centered tetragonal structure. Fe-Pt nanoparticles precipitation method to synthesize Fe3O4 particles and further
are mainly used as new ultra-high density magnetic storage sonicated at a frequency of 20 kHz for 30 min under nitrogen
materials (Tokuoka et al. 2014). Ferromagnetic nanomaterials atmosphere. This sonication-assisted synthesis of MFNs
have great advantages over other magnetic nanomaterials in achieved a better size (75.1 nm vs. 286.1 nm) and magnetic
wastewater treatment. Compared with Co and Ni, iron is wide- saturation value (62.37 emu/g vs. 42.16 emu/g) by compari-
ly sourced and cheap, which is more conducive to practical son with mechanical stirring.
application (Zhou et al. 2018). In addition, ferro-based mag-
netic materials have a high activity and can adsorb contami- Hydrothermal method Hydrothermal synthesis of MFNs is by
nants in wastewater more efficiently (Huang et al. 2010a). heating the solution under high pressure in an autoclave, and
Recently, the application of magnetic Fe3O4 nanoparticles soluble salts containing valent and trivalent (commonly ferric)
(MFNs) in the removal of ECs are receiving a rising attention transition metal salts are dissolved separately and mixed to-
due to the advantages of large specific surface area, easy to gether. Then, organic solvents are added drop by drop under
recycle and reuse, low cost, and no secondary pollution continuous vigorous stirring (Guo et al. 2018). The MFNs
(Rostami et al. 2013). This work mainly focused on the syn- obtained by hydrothermal method can control the crystal
thesis and application of MFNs, as well as the mechanisms for shape, making it possible to obtain large quantities of MFNs
contaminants removal. with controlled shape and size; however, the reaction condi-
tions are relatively strict (Hedayati et al. 2017).
Synthesis approaches for MFNs Guo et al. (2017) dissolved FeSO4·7H2O in water, stirred it
vigorously at room temperature, and added Na2S2O3 and then
Chemical and physical methods are usually used for the syn- NaOH drop by drop. Finally, the solution was heated for 12 h
thesis of MFNs (Table 1). Chemical methods for the synthesis at 413 K. The size of MFNs was within the range of 80–120
of magnetic nanomaterials are usually conducted in liquid nm, and the magnetization saturation value was 57.59 emu/g.
phase, e.g., co-precipitation, hydrothermal, solvothermal,
sol-gel, thermal decomposition, microemulsion, and oxidation Solvothermal method The solvothermal method was devel-
method. Chemical synthesis is relatively simple and widely oped on the basis of the hydrothermal method, and the solvent
used, which is more suitable for application in industry (Jeong water used in the hydrothermal method is replaced by an or-
et al. 2007). Physical method mainly includes mechanical ball ganic solvent. Solvothermal method facilitates the dissolve of
milling and evaporative condensation. The particle size ob- a substance that is insoluble or insoluble at normal tempera-
tained by the physical preparation method is easy to control. ture or generates a dissolved state of the substance by a chem-
However, the requirement of experimental equipment is high, ical reaction so that it is supersaturated to form a core (Hong
so it is not often used in the laboratory and industry (Janot and et al. 2005). Fan et al. (2019) synthesized MFNs in a
Guérard 2002). solvothermal system by modified reduction reactions between
Table 1 Characteristics and synthesis of MFNs
Synthesis methods Advantages Disadvantages References
Chemical synthesis Co-precipitation method Simple and easy to operate The size and morphology of Yang et al. (2018)
method particles are not easy to control,
easy to be oxidized,
and agglomerated
Hydrothermal method Well-controlled shape and size The reaction conditions are Hedayati et al. (2017)
relatively strict
Solvothermal method Uniform size, high purity, High temperature and pressure Iordache et al. (2018)
good dispersion, good and are required
well-controlled crystal shape,
and high crystallinity
Sol-gel method Low-cost raw materials, simple High temperature annealing is Xu et al. (2007)
equipment requirement, required
and easily controlled process
Thermal decomposition Good crystallinity, easy control High energy consumption, Vitalii et al. (2016);
method of size, and good dispersion expensive reagents, Zhang et al. (2016a, b)
and impure products
Microemulsion method Easy to operate Large amounts of organic solvents Hao et al. (2010)
are needed, which are harmful
to the environment
Oxidation method Uniform morphology and Particles tend to aggregate and Altan et al. (2016)
narrow size distribution precipitate
Physical synthesis Mechanical ball milling Good reproducibility and easy Low purity and high energy Janot and Guérard (2002)
method control of particle size, consumption
high in stability
Thermal plasma synthesis High product yield The requirements are relatively Huang et al. (2010b)
high, with large investment
FeCl3 and ethylene glycol. The average diameter of the ob- precursor and solvent were stirred to obtain sols, which were
tained MFNs was 400 nm, and the magnetization saturation further heated to obtain the gel. The resulting gel was calcined
value was 73.69 emu/g. for 30 min for the formation of iron oxide nanostructures, with
The solvothermal method for the synthesis of MFNs has the diameter of 25–30 nm.
the advantages of uniform size, high purity, good dispersion,
good and well-controlled crystal shape, and high crystallinity Thermal decomposition method Thermal decomposition
(Iordache et al. 2018). Also, sonication can be applied to im- method for the synthesis of MFNs involves the decomposition
prove the property of synthesized MFNs (Einollahi Peer et al. of metal organic compounds (such as iron acetylacetonate and
2018). However, the reaction must be carried out under high iron pentacarbonyl) by heating high-boiling organic solvents,
temperature and pressure, limiting its application in industrial with the addition of a blocking agent and a stabilizer (Xu et al.
cases (Zhao and Yuan 2016). 2020). During this procedure, the iron atoms generate into iron
nanoparticles and finally oxidized to Fe3O4. Wei et al. (2018)
Sol-gel method In the sol-gel method, a compound containing synthesized Fe3O4@C by the pyrolysis of (Fe)2(4H4CO6)3 pre-
a highly chemically active component is used as a precursor, a cursor. Fe3O4@C-1 was obtained by a heating precursor under
raw material of an iron salt, a solvent, and a surfactant that is 500 °C in the N2 flow for 5 h. Then, the annealed Fe3O4@C-1
uniformly mixed in a liquid phase, which forms a stable trans- sample was dispersed into HCl solution, stirred for 20 min, and
parent sol system in the solution via hydrolysis and conden- collected through vacuum filtration to obtain the product
sation reaction. Sols are further heated to obtain the gel, which Fe3O4@C-2, which gained a larger surface area than that of
is calcined for the formation of iron oxide nanostructures the Fe3O4@C-1 sample (29.715 m2/g vs. 24.334 m2/g).
(Shah et al. 2018). Sol-gel method has the advantages of The MFNs prepared by thermal decomposition have
low-cost raw materials, simple equipment requirement, and good crystallinity, easy control of size and morphology,
easily controlled process. However, high temperature anneal- and good dispersion, which however suffers from high
ing is required to obtain high crystallinity nanoparticles (Xu energy consumption, expensive reagents, and impure prod-
et al. 2007). ucts (Zhang et al. 2016a, b). Also, the raw materials can
Shah et al. (2018) synthesized iron oxide sols, using ferric only be dissolved in organic solvents, which are toxic and
chloride (FeCl3 ·6H2O) as the precursor, hexane and water and high cost of preparation, greatly restricting its industrial
ethanol as the solvents, and oleic acid as the surfactant. The production (Vitalii et al. 2016).
Microemulsion method The microemulsion method involves spheroidal Fe3O4 nanoparticles was ∼ 90 emu/g, with an av-
a thermodynamically stable dispersion of mutually incompat- erage size of 15–40 nm. High product yield can be obtained in
ible two-phase solutions, which is a ternary system formed by the thermal plasma process. However, the requirements for the
mixing water (or polar solution), oil (hydrocarbon), and sur- experimental equipment are relatively high, with large invest-
factant (sometimes possibly adding an alcohol co-surfactant) ment (Huang et al. 2010b).
at an appropriate ratio (Shao et al. 2013). This system is
regarded as a reaction site, in which an iron salt and a solvent Surface modification of MFNs
are added to precipitate nanoparticles. However, large
amounts of organic solvents are needed, which are harmful As a magnetic adsorbent, MFNs can be used for the removal
to the environment and difficult to achieve large-scale indus- of environmental pollutants. However, due to the large specif-
trial production (Hao et al. 2010). Xia et al. (2018) prepared ic surface area and the interaction of magnetic dipoles, MFNs
xylene solution containing iron (II) acetate, oleic acid, and are prone to agglomeration. Also, MFNs have strong surface
oleyl amine with vigorous stirring. After slowly heating, de- chemical activity; they are easily demagnetized by oxidation
ionized water was added to the reaction solution, and the and lead to insufficient surface hydroxyl groups (Maleki et al.
resulting mixture was then aged at the same temperature, 2015). Therefore, surface modification of MFNs cannot only
followed by the addition of ethanol to precipitate the nanopar- protect the magnetic Fe3O4 from agglomeration but also in-
ticles. The average particle size of the MFNs was 12.4 ± 1.9 crease the functional groups on the surface of the magnetic
nm. Other combination of ternary systems were also used, Fe3O4, so that pollutants can be adsorbed on the surface and
e.g., water/cyclohexane/Span 80-Tween 80/isopropyl alcohol enhance the adsorption performance.
(Nourafkan et al. 2017) and cyclohexane/n-hexanol/Extran In order to enhance the dispersibility and stability of mag-
(Sahu et al. 2016). netic nanomaterials, it is necessary to functionally modify and
coat the magnetic nanomaterials. Both organic compounds
Oxidation method The oxidation method relies on the precip- (e.g., polymer and organic small molecule materials) and in-
itation of ferrous hydroxide and its partial oxidation with mild organic compounds (e.g., silicon dioxide, sulfide, gold or met-
oxidants such as nitrate. Partial oxidation of ferrous salts was al oxide) can be used for the surface modification and
first described by Baudisch and then refined by Sumotomoto functionalization of magnetic nanomaterials. The polymer
and Matijevic to prepare magnetite nanoparticles of different used for nanoparticle modification is usually selected from
sizes (Sugimoto and Matijević 1980). Uniform spherical mag- polysaccharide polymer, amino acid polymer, polyvinyl alco-
netite particles with different sizes can be obtained via the hol, polyethylene glycol, and polyacrylamide (Ge et al. 2012;
oxidation method. Nevertheless, strong magnetic attraction Shao et al. 2016). Organic small molecules are usually ob-
due to a high degree of magnetization and hydrophobicity tained from materials having specific functional groups such
interaction will in many cases cause particles to aggregation as -NH2, -COOH, -OH, and -SH. Inorganic material modifi-
and precipitation (Vereda et al. 2013). cation usually presents a core-shell structure, e.g., SiO2 and
TiO 2 (Zarei et al. 2018), as well as other inorganic
Physical synthesis of nanoparticles nanomaterials including Ag (Ramesh et al. 2016), graphene
(Zhang et al. 2018b), and carbon nanotubes (Li et al. 2017).
Mechanical ball milling is a method of impacting and grinding Chemical modification, surface deposition, polymer coat-
micron-sized particles into nano-sized particles in a ball mill. ing, spray drying, and microemulsion are the most common-
The magnetic nanoparticles prepared by mechanical ball mill- ly used approaches for the modification of nanoparticles.
ing have good reproducibility and easy control of particle size,
and are not only low in cost but also high in stability, so they Chemical modification
can be stored for a long time (Janot and Guérard 2002). For
instance, Zhang et al. (2018b) adopted a new method for pre- Chemical modification refers to the chemical reaction between
paring nano-powder by a high-frequency magnet assisted the adsorbent surface and the effective groups of the modifica-
aqueous solution ball milling. The average size of the particles tion, including crosslinking reactions, coupling agent method,
was about 20 nm, and the saturation magnetization was 38.56 and surface grafting. However, the introduction of non-
emu/g. The thermal plasma synthesis of nanoparticles utilizes magnetic materials will greatly reduce the magnetic properties
thermal plasma or vacuum to pelletize the reactants, and the of the MFNs. Chen et al. (2019) reported preparation of MFNs
particles are gasified and then cooled to condense (O’Dell with amino groups (Fe3O4-NH2) and polyethyleneimine
et al. 2004). Anupama et al. (Anupama et al. 2017) synthe- (BPEI) grafting (Fe3O4-PEI) by solvothermal method using
sized MFNs via the high-yield thermal plasma route, in which branched polyethyleneimine (BPEI) and β-cyclodextrin (β-
phase transition occurred from γ-Fe2O3 to Fe3O4 at the tem- CD) and then synthesized Fe3O4-PEI/β-CD composites based
perature of 473–573 K. The magnetization value of the on PEI and β-CD amidation (Fig. 1). These resulting particles
Fig. 1 Schematic illustration for the preparation of Fe3O4-PEI/β-CD composite (Chen et al. 2019)
size were 30–50 nm, where Fe3O4-PEI exhibited spherical par- The hard template method has a relatively strong reaction
ticles and was much larger in size. The saturation magnetization condition, which will affect the final structure of the target
value for Fe3O4-NH2, Fe3O4-PEI, and Fe3O4-PEI/β-CD was product (Zhang et al. 2006). Kim et al. (2011) reported a
81.3 emu/g , 64.2 emu/g, and 60.3 emu/g, respectively. new type of magnetic mesoporous carbon material, synthe-
sized with SBA-15 and pyrrole as template and carbon source,
for the adsorption of Hg(II), with the adsorption rate at 97%.
Template modification The soft template method, without first synthesizing a
silicon-based mesoporous material template, can obtain a
Template modification refers to the use of organic matter with magnetic ordered mesoporous carbon directly in a reaction
microporous structure as a template to make the reactants or system (Rujiralai et al. 2019). Hu et al. (2019) introduced a
monomers react or polymerize to form target products in these series of mesoporous carbon materials with different pore di-
micropores or interlaminar spaces with nanoscale (Wan et al. ameters using Fe3O4 as the magnetic source and phenolic
2005). Iron oxide can grow in the mesoporous pore size, and resin as the carbon source, and the addition of cyanoguanidine
the framework structure also affects the growth of iron oxide was used to adjust the pore size. The prepared magnetic or-
during the formation of the crosslinked polymer (Shima et al. dered mesoporous carbon material can be used as an effective
2005). A schematic representation for the formation of MFNs adsorbent for simple and rapid removal of minocycline from
via template modification method is shown in Fig. 2. water.
According to the template used, the template modification
method is divided into hard template method and soft mold
method. When the magnetic mesoporous carbon material is Surface deposition or coating modification
synthesized by the hard template method, the template struc-
ture must be ordered and has good stability so that some re- Surface deposition or coating modification refers to the meth-
actions such as carbonization and washing can be avoided. od that inorganic or organic compounds form a coating layer
Fig. 2 Schematic representation for the formation of MFNs assembly outside the pores of hard template
on the surface of ferric oxide particles to improve their oxida- bonded to the surface of the magnetic particles to obtain a
tion resistance and dispersion (Danalıoğlu et al. 2017). An polymer modified product (Zulfikar et al. 2016). “Grafting
example illustrating the synthesis of magnetic Fe3O4@GO from” means firstly grafting an initiator or a double bond on
adsorbents via surface deposition method is shown in Fig. 3. the surface of the magnetic particles and then adding a
Modification deposited or coated on MFNs can increase par- crosslinking agent to surface-polymerize with the monomer
ticle size and reduce specific surface area (Xing et al. 2015). to obtain a modified product, as shown in Fig. 4 (Lü et al.
The composite magnetic microsphere prepared by the surface 2017).
deposition or coating modification often contains impurities “Grafting to” can continuously increase the length of the
such as a solvent and a precipitant, and the morphology is polymer chain through the grafting reaction. Ge et al. (2012)
difficult to control (Roto et al. 2016). Peng et al. (2012) added ferrous salt and ferric salt into NaOH solution to co-
employed an improved surface coating method, in which precipitate Fe3O4, followed by 3-aminopropyltriethoxysilane
FeCl3, FeSO4, ammonium hydroxide, and sodium humate (APS) in toluene refluxing under nitrogen. Acrylic acid and
solution were added in order. The obtained black substance crotonic acid copolymer (AA-co-CA) was prepared by free-
was Fe3O4/HA nanoparticles, with saturation magnetizations radical polymerization in distilled toluene, and AA-co-CA
of Fe3O4/HA at 61.2 emu/g. The core of the Fe3O4 magnetic was immobilized on Fe3O4@APS by the reaction of amino
nanoparticle had a typical size ∼ 10 nm while Fe3O4/HA at groups in Fe3O4@APS and carboxyl in AA-co-CA copoly-
104–189 nm. Also, Fe3O4 and coatings added in different mer. However, due to steric hindrance, the polymer chains
proportions can obtain different particle sizes and saturation “grafted to” the surface of the nanoparticles will shield the
magnetization. Yang et al. (2018) mixed FeCl3·6H2O and surface active sites. The longer the polymer chains are, the
FeSO4·7H2O with sodium dodecyl sulfate (SDS) to synthe- more significant the steric hindrance shielding effect is,
sized Fe3O4, and graphene oxide (GO) powders were poured resulting in a lower grafting rate (Anbarasu et al. 2014).
into the suspension. The saturation magnetization of different In “grafting from,” only the small molecular weight mono-
Fe3O4@GO adsorbents ranged from 1.55 to 33.64 emu/g with mer is connected to the chain end of the growth chain, which
varying ratios of GO and Fe3O4. effectively overcomes the shortcomings of the “grafting to”
method, and thus can form a polymer chain layer with a high
Polymer grafting or coating modification bonding density (Masoumi et al. 2014). Shao et al. (2016)
modified MFNs by c-methacryloxypropyltrimethoxy-silane
The method of grafting or coating a polymer on the surface of with the “grafting from ” me th od. The m ag netic
a magnetic micro-nanomaterial is mainly divided into the Fe 3O 4@PAA core-shell nanospheres were prepared by
“grafting to” and “grafting from” modes. “Grafting to” refers distillation-precipitation polymerization of acrylic acid (AA),
to the existing poly gathering through the action of static elec- with N,N-methylenebisacrylamide as the crosslinker and 2,2-
tricity, coordination, covalent bonds, etc. The compound is azobis(isobutyronitrile) as the initiator. The average diameter
Fig. 3 The schematics illustrating the formation of magnetic Fe3O4@GO adsorbents

Fig. 4 Schematic illustration of the fabrication process of Fe3O4@MOFs
of Fe3O4@PAA was 361 ± 24 nm, with a saturation magne- Application of MFNs in the removal of conventional
tization at 40.57 emu/g. contaminants
Application of MFNs in the removal of heavy metals

Microemulsion modification
Until now, the application of MFNs in the removal of contam-
The advantage of microemulsion modification is that it is in- inants are most commonly found in heavy metals. Heavy
expensive and the reaction is carried out at room temperature. metals are persistent in the environment, which may lead to
However, though the coating material is thin enough, the total changes in microbial community composition, e.g., decrease
size is still much larger, leading to a reduced saturation mag- in microbial diversity and increase in the accumulation of
netization (Lu et al. 2010). Ramesh et al. (2016) developed a metal-resistant bacteria (Shi et al. 2020; Jiang et al. 2018c;
new W/O microemulsion technology to prepare Fe3O4/Ag Wang et al. 2020; Zhang et al. 2012, 2018a, 2019b, 2020a).
core/shell nanocomposites. The Fe3O4 nanoparticles and The adsorption mechanism of heavy metals by MFNs in-
Fe3O4/Ag nanocomposites were both in spherical shape while volves electrostatic attraction, surface complexation,
the former with an average diameter of 7 ± 2 nm, and the latter precipitation, and ion exchange. Xie et al. (2019) used the
with an average diameter of 10 ± 2 nm. The saturation mag- hydrothermal method and co-precipitation method to prepare
netization of Fe3O4/Ag nanoparticles was drastically reduced Mg/Fe layered double hydroxide loaded with magnetic
(40 emu/g vs. 62 emu/g of Fe3O4), probably due to the con- (Fe3O4) carbon spheres (MCs@Mg/Fe-LDHs) for the adsorp-
tribution of surface effects. tion of Pb(II) and Cu(II), with the adsorption capacity at
With the assistance of microwave, the size of MFNs can be 759.265 and 338.976 mg/g, respectively. The surface of
greatly reduced. Lu et al. (2016) prepared Fe3O4@SiO2 core- MCs@Mg/Fe-LDHs was negatively charged and attracts pos-
shell nanoparticles for the first time by a new microwave- itively charged ions such as Pb(II) and Cu(II) by electrostatic
assisted reverse phase microemulsion method. The saturation bonding. Excess surface hydrogen groups and carbonate ions
magnetization was 96.9 emu/g for Fe3O4 and 32.7 emu/g for from the inner layers lead to precipitation. Moreover, the
Fe 3 O 4 @SiO 2 , and the size of the prepared magnetic nanoscale pore structure and the oxygen group on the surface
nanomaterials decreased from 30 to 14 nm. can also adsorb more metal ions.
Also, the MFNs surface coated with silica contains a large
number of oxygen-containing functional groups, which can
rapidly accumulate on the adsorbent in a short time (Dai et al.
Application of MFNs in the removal 2018). Fan et al. (2019) immobilized persimmon tannin (PT)
of contaminants from aqueous environment onto Fe3O4@SiO2 microspheres to recover precious metals
from industrial wastewater containing gold and palladium,
With the development of surface modification of and the adsorption capacity of Au(III) was 917.43 mg/g.
nanomaterials, the adsorption capacities of MFNs are sig- Phenolic hydroxyl group participated in the adsorption reaction
nificantly enhanced to achieve a better removal of mul- and acted as a major electron donor. In addition, Pd(II) could
tiple contaminants in water. This section focused on the chelate with oxygen bearing groups from Fe3O4@SiO2@PT,
application of MFNs in both laboratory and natural water with the adsorption capacity of 196.46 mg/g.
bodies for the removal of various contaminants, includ- Additionally, carboxyl group, amino group, and other
ing conventional contaminants, e.g., heavy metals and functional groups had a certain effect on the adsorption
dyes, as well as ECs, e.g., pesticides, perfluorochemicals, performance. For instance, Sun et al. (2018a) immobilized
and antibiotics. the Fe3O4/LDH with calcium alginate (CA) to adsorb Cd(II),
Pb(II), and Cu(II), and the adsorption capacity was 74.06, wastewater. The possible uptake mechanisms for MO and
266.6, and 64.66 mg/g. During the adsorption process, the Pb(II) by the Fe3O4-PEI/b-CD hybrid adsorbent are illustrated
heavy metal ions formed complexation with Sur-OH- or in Fig. 5, in which the positively charged n-containing groups
Sur-O- and -COO- group, and precipitation with carbonate. of the β-CD cavity and PEI could remove the methyl orange
Guo et al. (2018) synthesized a magnetic silica gel adsorbent (MO), and the oxygen-containing group at the edge of β-CD
(Fe3O4-Si-COOH), in which carboxyl groups played an im- and the free amino group in PEI were the active sites for Pb(II)
portant role in the adsorption of Pb(II), Zn(II), and Cd(II), with uptake, respectively.
the adsorption capacity at 155, 110, and 93 mg/g, respectively. Metal-organic frameworks (MOFs) are a new class of mi-
The oxygen-containing functional groups on the surface of croporous materials that are consist of metals/metal clusters
MFNs and hydrogen in water can form stable surface com- and organic ligands which linked to each other (Shao et al.
plexes with metal ions (Sun et al. 2018a), which plays an 2016). The advantages of magnetic nanoparticle and the high
important role in the adsorption of heavy metals. Wang et al. adsorption capacity of MOF can be combined to remove dyes.
(2018a) synthesized La-doped magnetic biochar (LaxFe-BC) Alqadami et al. (2018) prepared the magnetic MOF
to adsorb Sb(V). In contrast to pristine biochar and un-doped (Fe3O4@AMCA-MIL53(Al)); the maximum monolayer ad-
magnetic biochar, the Sb(V) adsorption capacity in La-doped sorption capacities of methylene blue (MB) and malachite
magnetic biochar was greatly improved, increasing from 2.22 green (MG) were 325.62 and 329.61 mg/g at 318 K. The
mg/g and 4.85 mg/g to 18.92 mg/g at pH of 7. Because of the electrostatic interactions between the electron rich oxygen
large amounts of hydroxyl groups on the surface, LaxFe-BC and cationic dyes, hydrogen bonding between -OH group of
was more positively charged compared with Fe-BC, benefit- the adsorbent and dimethylamino (−N(CH3)2) group of dyes,
ing its adsorption on negative [Sb(OH)6]- via electrostatic π-π stacking interaction between the phthalic acid unit in the
attraction. structure of MIL-53(Al)-NH2 and the benzene ring in the dye
MFNs modified by polymer have good stability in solution molecule are responsible for the dyes concentration on
and coordinate with heavy metals through functional groups Fe3O4@AMCA-MIL53(Al). Using 0.01 M HCl/ethanol as
containing O and N (Einollahi Peer et al. 2018), thus removing the desorption agent, the performance of MOF was not signif-
heavy metals. Chitosan is rich in amino and hydroxyl groups icantly decreased after twice desorption.
and can adsorb heavy metals by chelation (Iordache et al.
2018). Omidinasab et al. (2018) prepared magnetic chitosan Application of MFNs in the removal of ECs
nanoparticles to adsorb V(V) and Pd(II) ions, and the maxi-
mum adsorption capacities were 186.6 and 192.3 mg/g, re- Apart from conventional contaminants, MFNs, with good
spectively. The removal rate of V(V) and Pd(II) from actual solid-liquid separation ability and reproducibility, are also
industrial samples were 99.9% and 92.3%, respectively. applied to remove ECs from water. Some studies
MFNs can also effectively recover precious metals from investigated the capacity of MFNs for the removal of
industrial wastewater. Uranium is a key material for nuclear pesticides. Li et al. (2019) reported the magnetic reduced
weapons and fuel for the nuclear power industry, which is graphene oxide (Fe3O4/rGO) for the adsorption of glyphosate
abundant in seawater. Li et al. (2018a) used a plasma method (GLY), and the maximum adsorption capacity reached 70.08
to grafted arsenazo III (ASA) onto the surface of Fe3O4@C mg/g (pH = 4, T = 328), demonstrating high adsorption capac-
core shell. At pH 4.0, the maximum adsorption capacity of ity and easy separation of Fe3O4/rGO. As GLY contains many
U(VI) on Fe3O4@C@ASA reached 46.2 mg/g. In practical functional groups (-COOH, -NH2, and -PO(OH)2), which can
applications, Fe3O4@C@ASA recovered > 99% uranium in form hydrogen bond interaction with -OH and -COOH on the
high salinity Gasikule Salt Lake brine. material surface, a strong electrostatic attraction is generated
between Fe3O4/rGO and GLY. Furthermore, GLY has abun-
Application of MFNs in the removal of residue dyes dant phosphonyl groups capable of forming complexes with
Fe2+ and Fe3+. Another study by Boruah et al. (2017) investi-
As a major source of color in wastewater produced by the gated the capacity of Fe3O4/rGO for the removal of triazine
textile and dye manufacturing industries (Peng et al. 2012), pesticides, with the maximum adsorption capacity at 18–20
residue dyes are usually treated with MFNs. The adsorption mg/g (pH = 5, T = 308). Electrostatic, hydrophobic, and π-π
mechanism of organic pollutants is attributed to physical ad- interactions between pesticides and materials contributed to the
sorption, hydrogen bond interaction (H-bond interaction), adsorption of pesticides. Further, Fe3O4/rGO can be regenerat-
aromatic-aromatic interactions (π-π interactions), and hydro- ed, with the adsorption efficiency of up to 88.66% over seven
phobic interaction. Chen et al. (2019) synthesized bifunctional cycles.
magnetic nano-adsorbents (Fe 3 O 4 -PEI/β-CD) via β- Additionally, MFNs could be a promising and cost-
cyclodextrin (β-CD) and polyethylenimine (PEI), which co- effective adsorbent for removing antibiotics. Hu et al. (2019)
trapped Pb(II) and methyl orange (MO) in complex prepared magnetic mesoporous carbon materials (Fe3O4-
Fig. 5 Proposed mechanisms for

the simultaneous capture of MO
and Pb(II) by Fe3O4-PEI/b-CD
(Chen et al. 2019)
OMC) by the soft template method to adsorb minocycline. Fe3O4@MOF-100(Fe) with core-shell structure in aqueous
The results demonstrated that the adsorption equilibrium was solution, and the maximum adsorption capacity was up to
reached within 10 min and the maximum adsorption capacity 377.36 mg/L, and the removal rate was still up to 80% after
was 193.5 mg/g. Wu et al. (2018) synthesized magnetic cop- 5 times of adsorption. Another recent study prepared Fe3O4 by
per based metal-organic frameworks (Fe3O4/HKUST-1) for euphorbia cochinchinensis extraction via the green synthesis,
the adsorptive removal of ciprofloxacin (CIP) and norfloxacin which can be directly used for the adsorption of doxorubicin
(NOR). The maximum adsorption capacities reached as high hydrochloride (Weng et al. 2018).
as 538 mg/g and 513 mg/g (pH = 7, T = 298 K), which Graphene is rich in electrons and oxygen-containing func-
attributed to the coordination bonds between the open Cu(II) tional groups, which is often combined with MFNs to broaden
sites in HKUST-1 and COO- groups in CIP and NOR zwit- their adsorption applications, particularly in the removal of
terion molecules, the intermolecular hydrogen bonds between EDCs. Chang et al. (2012) suggested that aniline and p-
Cu-O-Cu in HKUST-1 and -NH groups in CIP and NOR chloroaniline could be effectively removed by Fe3O4@GO,
neutral molecules, the acid-base and hydrogen bonds interac- which was prepared by solvothermal method, and the satura-
tion between the NH moiety and the COOH moiety, and the tion magnetization of the Fe3O4@GO was about 120 emug,
π-π interactions between phenyl rings. within 60 min. Ouyang et al. (2015) prepared Fe3O4@GO by
As traditional wastewater treatment processes are difficult to a facile one-pot polylol approach, with the maximum adsorp-
remove perfluorinated compounds effectively (Zhou et al. 2016), tion capacity to bisphenol A (BPA) at 72.80 mg/g. Zhang et al.
the application of MFNs on the removal of perfluorinated com- (2018b) prepared Fe3O4@GO by the co-precipitation method,
pounds are recently drawing attention. Du et al. (2017) reported a and the maximum adsorption capacity for p-tert-butylphenol
novel magnetic fluorinated adsorbent of PFOS synthesized via a (PTBP) was 59.18 mg/g (pH = 4, T = 303 K), which was
simple ball milling of Fe3O4 and vermiculite loaded with a cat- much higher than pristine GO (24.97 mg/g).
ionic fluorinated surfactant (Fe3O4/F-VT). The loading of Fe3O4 Besides, Minh et al. (2018) applied Fe3O4 coated with
nanoparticles increased the hydrophilicity of the surface of F- gamma-APS polymer deposited on graphene oxide
VT, and the fluorophilicity of the C-F chain made the adsorption (Fe 3 O 4 @γ-APS/GO) for the removal of benzotriazole
of PFOS very fast and selective. The capacities of (BTA), a typical UV stabilizer. The maximum adsorption ca-
perfluorobutanoic acid (PFBA), perfluorobutanesulfonate pacity was 312.5 mg/g, attributing to the hydrophobic, elec-
(PFBS), and PFOA were 166, 262, and 681 mg/g, respectively trostatic, and π-π interactions between benzotriazole and the
(pH = 6.4, T = 198 K). adsorbent.
MFNs also presents high adsorption capacity and good Until now, the application of magnetic nanomaterials for
regeneration performance for the removal of PPCPs. Zheng the removal of contaminants, particularly ECs, is still at an
et al. (2018) studied adsorption of diclofenac sodium by early stage that is far from industrial scale. Also, though
MFNs have good performance in the treatment of convention- (LDH) assays (Neda et al. 2018), and in vivo toxicity assays,
al contaminants, their applications in ECs are mostly applied typically mice and Danio rerio (Caro et al. 2019). For in-
in laboratory synthetic water, with very few in natural waste- stance, high concentration of cerium oxide nanoparticles can
water. Table 2 strongly activate the cell’s own antioxidant system in an MTT
assay (Aala et al. 2018). Cerium oxide nanoparticles stimulate
the proliferation of primary mouse embryonic fibroblasts
Challenges and future prospective in vitro, thus disrupting the physiological balance (Popov
et al. 2016). Also, the whole-cell bioreporter assay has been
Despite the recent development of MFNs for removing envi- applied to detect toxic effects of various environmental con-
ronmental contaminants, their application in environmental sci- taminants, e.g., petroleum hydrocarbon (Jiang et al. 2020),
ence are still limited. Several challenges include the agglomer- Cr(VI) (Jiang et al. 2017), and Pb(II) (Song et al. 2014), which
ation of MFNs, the interaction of MFNs and ECs and the un- can also be potentially used in the toxicity evaluation of
certain toxic effects to humans and the ecological system. nanomaterials.
Future design of MFNs for ECs removal Application of MFNs in environmental microbiology
The magnetic and anisotropic effects of magnetic nano-ions More recently, the involvement of MFNs on the development
make them easy to be oxidized and agglomerate (Maleki et al. of whole-cell biosensors for environmental monitoring and
2015), limiting their application. Also, the preparation process the identification of functional microorganisms from complex
of functionalized MFNs is cumbersome and time-consuming, environmental matrix has been studied, broadening its appli-
and large-scale industrial production technology is still imma- cation to the field of environmental microbiology.
ture, which limits its application in practical engineering. As a rapid, sensitive, and cost-effective tool for the deter-
Therefore, the modification of MFNs in order to improve their mination of environmental contaminants and toxicity, whole-
chemical stability and their dispersion in solution is of great cell bioreporters have been extensively used as an alternative
significance (Fan et al. 2019) (Li et al. 2019). The future approach for evaluating the general impacts of individual or
development of MFNs is to simplify the preparation process, mixed chemicals (Jiang et al. 2020). However, when applied
reduce the cost, improve the functionalization technology, and to the soil samples, the performance of whole-cell bioreporters
improve the adsorption specificity. is affected by soil particles which may interference with the
Although MFNs has good performance in the treatment of bioluminescent or fluorescent signals (Jiang et al. 2017).
conventional contaminants, the application of MFNs in the MFNs could attach on the surface of whole-cell bioreporter
removal of ECs are usually conducted with synthetic water cells, which can be separated from the soil suspension and
in the laboratory. Natural wastewater is usually composed of therefore improve sensitivity and repeatability. The toxicity
multiple contaminants, leading to uncertainty in evaluating the and bioavailability of chrome-contaminated and cinder con-
adsorptive capacity of MFNs on one single contaminant. taminated soils were assessed using the MFNs-assisted bio-
Also, ECs in natural wastewater are mostly at trace amount, logical reporting devices (Jiang et al. 2018b; Jiang et al. 2020;
and other contaminants, e.g., heavy metals and organic com- Jia et al. 2016).
pounds, may compete with ECs for the adsorption position of Also, uncultivable microorganisms account for over 99%
MFNs (Vilardi et al. 2018). The interaction between ECs and of all species on earth, playing essential roles in ecological
MFNs should be further investigated to get a better under- processes. MFNs provides as a promising tool for identifying
standing of the mechanism and feasibility of MFNs for ECs the physiological features and metabolic activities of living
under realistic environmental conditions. cells in complex environmental media (Zhang et al. 2011)
via separation by external magnetic field. Living functional
Toxicity assessment of MFNs degraders of phenol (Zhang et al. 2015) and alkane (Wang
et al. 2016) were successfully isolated from activated sludge
The MFNs are small and highly active and can be easily and crude oil-contaminated sites via the MFNs-assisted
absorbed by biological tissues (Duan et al. 2018), so their uncultivation approach.
potential risks to the environment and human health are yet
to be evaluated. Therefore, appropriate approaches for the
evaluation of the possible toxic effects of MFNs on Conclusions
non-targeted organisms and the ecological system need
to be established, such as in vitro cytotoxicity assays, The unique features of small size, strong surface charge, large
typically 3-(4,5)-dimethylthiahiazo(-z-y1)-3,5-di- surface area, and superparamagnetic properties have endorsed
phenytetrazoliumromide (MTT) and lactate dehydrogenase MFNs with the ability to remove multiple contaminants from
Table 2 Application of MFNs in the removal of typical contaminants
Adsorbent type Synthesis method Adsorbate type Adsorption pH Temperature (K) Times of Reference
capacity (mg/g) reuse
MCs@Mg/Fe-LDHs Hydrothermal method and Pb(II) 759.265 6 298 3 Xie et al. (2019)
Co-precipitation method Cu(II) 338.976
Fe3O4@SiO2@PT Solvothermal method and Au(III) 917.43 5 298 Not mentioned Fan et al. (2019)
sol-gel method Pd(II) 196.46
Fe3O4/MgAl-LDH Solvothermal method Cd(II) 74.06 5–6 298 5 Sun et al. (2018a)
Pb(II) 266.6
Cu(II) 64.66
Environ Sci Pollut Res (2021) 28:7599–7620
LaxFe-BC Co-precipitation method Sb(V) 18.92 7 298 ± 1 6 Wang et al. (2018a)

Fe3O4-CSN Co-precipitation method V(V) 186.6 5 293 ± 1 Not mentioned Omidinasab et al. (2018)
Pd(II) 192.3 6
Fe3O4-Si-COOH Hydrothermal method Zn(II) 110 6 298 Not mentioned Guo et al. (2018)
Pb(II) 155
Cd(II) 93
Fe3O4@C@ASA Co-precipitation method U(VI) 46.2 5 298 5. Li et al. (2018a)
Fe3O4-PEI/β-CD Solvothermal method Methyl orange(MO) 192.2 3 303 5 Chen et al. (2019)
Pb(II) 73.1 6
Fe3O4@AMCA- Co-precipitation method Malachite green (MG) 329.61 6.8 318 2 Alqadami et al. (2018)
MIL-53(Al) Methylene blue (MB) 325.62 8.9
Fe3O4@GO Solvothermal method Aniline 375.9 59 318 Not mentioned Chang et al. (2012)
Fe3O4@GO Polyol method Bisphenol A 72.8 8 297 8 Ouyang et al. (2015)
Hummers method
Fe3O4@GO Co-precipitation method P-tert-butylphenol 59.18 6 283 Not mentioned Zhang et al. (2018a)
(PTBP)
Fe3O4/rGO Co-precipitation method Glyphosate 70.08 4 328 Not mentioned Caro et al. (2019)
Fe3O4/rGO Co-precipitation method Hexahydronaphthalene 19.62 5 303 7 Boruah et al. (2017)
Prometryn 18.67
Fe3O4-OMC Polyol method Minocycline 193.5 8 293 8 Hu et al. (2019)
Fe3O4/HKUST-1 Purchased granules Ciprofloxacin 538 7 298 10 Wu et al. (2018)
Norfloxacin 513
Fe3O4/F-VT Ball milling Perfluorobutanoic acid 166 6.4 298 4 Du et al. (2017)
(PFBA) 262
Perfluorobutanesulfonate 681
(PFBS)
PFOA
Fe3O4 Solvothermal method Doxorubicin hydrochloride 31.85 7 313 Not mentioned Weng et al. (2018)
Fe3O4@MOF-100(Fe) Solvothermal method Diclofenac sodium 377.36 5 298 5 Zheng et al. (2018)
Fe3O4@γ-APS/GO Co-precipitation method Benzotriazole (BTA) 312.5 6 313 5 Minh et al. (2018)
7613
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Magn. Magn. Mater. 416:366–372. https://doi.org/10.1016/j.
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jmmm.2016.05.009
environmental contaminants, particularly ECs which are nowa- Anbarasu M, Anandan M, Chinnasamy E, Gopinath V, Balamurugan K
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tion approaches offer MFNs with distinct physiochemical prop- coated Fe3O4 nanoparticles by chemical co-precipitation method for
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development of MFNs is to overcome the agglomeration prop- Anupama AV, Keune W, Sahoo B (2017) Thermally induced phase
erty and cumbersome preparation of MFNs. Also, the possible transformation in multi-phase iron oxide nanoparticles on vacuum
toxic effects of MFNs on non-targeted organisms and the eco- annealing. J Magn Magn Mater 439:156–166. https://doi.org/10.
1016/j.jmmm.2017.04.094
logical system need to evaluated.
Benitez FJ, Acero JL, Real FJ, Roldán G, Rodríguez E (2013) The effec-
tiveness of single oxidants and AOPs in the degradation of emerging
Authors’ contributions BJ designed the content and logic of this review contaminants in waters: a comparison study. Ozone: Sci Eng 35:
paper. YS finished the first-hand manuscript, and BJ and YX revised this 263–272. https://doi.org/10.1080/01919512.2013.794107
manuscript. All authors read and approved the final manuscript. Bonvin F, Jost L, Randin L, Bonvin E, Kohn T (2016) Super-fine pow-
dered activated carbon (SPAC) for efficient removal of
Funding This study was financially supported by the Natural Science micropollutants from wastewater treatment plant effluent. Water
Foundation of China (41807119), the Open Fund of National Engineering Res 90:90–99. https://doi.org/10.1016/j.watres.2015.12.001
Laboratory for Site Remediation Technologies (NEL-SRT201907), special Boruah PK, Sharma B, Hussain N, Das MR (2017) Magnetically recov-
fund of State Key Joint Laboratory of Environment Simulation and Pollution erable Fe3O4/graphene nanocomposite towards efficient removal of
Control (19K04ESPCT), and Beijing Municipal Science and Technology triazine pesticides from aqueous solution: investigation of the ad-
Project (Z181100002418016). sorption phenomenon and specific ion effect. Chemosphere 168:
1058–1067. https://doi.org/10.1016/j.chemosphere.2016.10.103
Data availability Not applicable. Britos TN, Castro CE, Bertassoli BM, Petri G, Fonseca FLA, Ferreira FF,
Haddad PS (2019) In vivo evaluation of thiol-functionalized
superparamagnetic iron oxide nanoparticles. Mater Sci Eng C
Compliance with ethical standards Mater Biol Appl 99:171–179. https://doi.org/10.1016/j.msec.2019.
01.118
Ethical approval Not applicable. Cajthaml T, Kresinova Z, Svobodova K, Moder M (2009)
Biodegradation of endocrine-disrupting compounds and suppres-
Consent to participate Not applicable. sion of estrogenic activity by ligninolytic fungi. Chemosphere 75:
745–750. https://doi.org/10.1016/j.chemosphere.2009.01.034
Caro C, Egea-Benavente D, Polvillo R, Royo JL, Pernia Leal M, García-
Consent to publish Not applicable.
Martín ML (2019) Comprehensive toxicity assessment of
PEGylated magnetic nanoparticles for in vivo applications.
Colloids Surf B Biointerfaces 177:253–259. https://doi.org/10.
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Environmental Science and Pollution Research (2021) 28:7599–7620

Recent advances in the application of magnetic Fe3O4 nanomaterials

Keywords Emerging contaminants (ECs) . Magnetic nanoparticles . Environmental remediation . Synthesis

Introduction contaminants in water bodies (Jurado et al. 2019), convention-

Table 1 Characteristics and synthesis of MFNs

Synthesis methods Advantages Disadvantages References

Fig. 3 The schematics illustrating the formation of magnetic Fe3O4@GO adsorbents

Fig. 4 Schematic illustration of the fabrication process of Fe3O4@MOFs

Application of MFNs in the removal of heavy metals

Fig. 5 Proposed mechanisms for

LaxFe-BC Co-precipitation method Sb(V) 18.92 7 298 ± 1 6 Wang et al. (2018a)

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