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Zhi, K. Activation Persulfate by Various Iron-Based Catalysts. Encyclopedia. Available online: https://encyclopedia.pub/entry/18701 (accessed on 20 April 2024).
Zhi K. Activation Persulfate by Various Iron-Based Catalysts. Encyclopedia. Available at: https://encyclopedia.pub/entry/18701. Accessed April 20, 2024.
Zhi, Keke. "Activation Persulfate by Various Iron-Based Catalysts" Encyclopedia, https://encyclopedia.pub/entry/18701 (accessed April 20, 2024).
Zhi, K. (2022, January 24). Activation Persulfate by Various Iron-Based Catalysts. In Encyclopedia. https://encyclopedia.pub/entry/18701
Zhi, Keke. "Activation Persulfate by Various Iron-Based Catalysts." Encyclopedia. Web. 24 January, 2022.
Activation Persulfate by Various Iron-Based Catalysts
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This entry is adapted from the peer-reviewed paper 10.3390/app112311314

Advanced oxidation technology of persulfate is a new method to degrade wastewater. As the economy progresses and technology develops, increasingly more pollutants produced by the paper industry, printing and dyeing, and the chemical industry are discharged into water, causing irreversible damage to water. Methods and research directions of activation persulfate for wastewater degradation by a variety of iron-based catalysts are reviewed. This entry describes the merits and demerits of advanced oxidation techniques for activated persulfate by iron-based catalysts. In order to promote the development of related research work, the problems existing in the current application are analyzed.

iron-based catalysts activation persulfate degrading wastewater

 1. MeFe2O4 (Me = Cu, Co, Zn, etc.)

In terms of activation mechanism, transition metal compounds react with PS to produce a large amount of ·SO4−; the reaction equation follows:
Mn+ + S2O82− → M(n+1)+ +·SO4− + SO42−
As can be seen from the above reaction, metal ions are in a free state dispersed in the solution during the reaction process. Although the wastewater can be degraded by the activation persulfate mechanism, it belongs to homogeneous catalysis; metal ions will be dissolved in the aqueous solution, which causes difficult separation from solution. Therefore, the production cost is greatly increased due to its difficult recycling nature, and it is easy to cause secondary pollution to the environment. Therefore, MeFe2O4 with a low metal leaching rate has become a new research direction. Through PS/PMS [1] heterogeneous catalytic technology, these problems can be effectively solved [2][3][4].
At present, there are several common methods for preparing iron-based catalysts: hydrothermal, solvothermal, sol–gel preparation, and coprecipitation methods.
In the hydrothermal method, the solute is dispersed into the solution, stirred, and heated in the reactor, and finally washed and dried to obtain the required product [5].
Similar to the hydrothermal method, the solvothermal method changes water into an organic solvent. By dissolving one or more precursors in a nonaqueous solvent, the reaction occurs in liquid phase or supercritical conditions [6].
The sol–gel method is to dissolve the metal alkoxides in organic solvents, form homogeneous solutions, add other components, react at a certain temperature to form gels, and finally make products by drying [7].
Coprecipitation is an important method to prepare composite oxide ultrafine powder containing a large variety of metal elements [8].
The electron transfer between transition metal oxides is much higher [9] than that between single transition metal oxides. Generally, AB2O4 [10][11] structure is referred to as spinel structure. CuFe2O4 is a typical spinel ferrite with a magnetic structure, which has high chemical stability and low metal leaching rate. Taking CuFe2O4 as an example, compared with single transition metal oxides, Fe and Cu elements can play a role in the reaction; respectively, they can also activate PS to produce ·OH and ·SO4−.
G. Xian et al. [12] comprehensively compared the catalytic degradation effects of CoFe2O4, CuFe2O4, MnFe2O4, and ZnFe2O4. In detail, CuFe2O4 presented the best and fastest catalytic performance in organics removal. Almost 87.6% azo dye acid orange 7 (AO7) was removed in PS solution coupled with CuFe2O4 [12]. Additionally, it was known that CuFe2O4 had the best catalytic effect. Moreover, through the quenching experiment, it was not ·OH but ·SO4− that played a major role in the reaction.
Table 1 shows the degradation effects of some different MeFe2O4-activated PS/PMS on different kinds of wastewater. It can be seen from the table that the iron-based catalyst with spinel structure mainly acts on ·SO4− in the mechanism of activation persulfate; the effect of ·OH is slightly worse [13]. Of course, there are also some nonfree radical pathways, which degrade pollutants in water by generating singlet oxygen 1O2 [14][15][16].
Table 1. Effect of Different MeFe2O4-activated PMS on degradation of different wastewater [5][6][7][8][13][17][18][19].
Catalyst Pollution Main Mechanism Pollutant Concentration Catalyst Concentration Oxidant Oxidation Concentration T/min Degradation Rate/% Number of Cycles Synthesis
Techniques		 Ref.
PbFe2O4 Thionine 1O2 10 μM 0.4 g/L PMS 400 μM 20 100 Not mentioned Solution combustion [17]
CoFe2O4–loaded quartz sand Sulfachloropyridazine
sodium		 ·SO4−
·OH		 2 g/L 10 g PMS 75 mg/L 150 90 Not mentioned Citrate combustion [18]
CoFe2O4-SAC Norfloxacin (NOF) ·SO4−
·OH		 10 mg/L 0.1 g/L PMS 0.15 g/L 120 TOC reduction
81		 5
(>80%)		 Hydrothermal [13]
The biochar loaded with CoFe2O4 nanoparticles Bisphenol A
(BPA)		 ·SO4−
·OH		 10 mg/L 0.05 g/L PMS 0.5 g/L 8 93 Not mentioned Hydrothermal [5]
C3N4@MnFe2O4-graphene Metronidazole ·SO4−
·OH		 20 mg/L 1.0 g/L PS 0.01 M 90 94.5 5
(>80%)		 Solvothermal [6]
Zn0.8Cu0.2Fe2O4 Atrazine ·SO4− 4.4 μM 200 mg/L PS 0.5 mM 30 95 Not mentioned Sol–gel [7]
CuFe2O4/O3 2,4-Dichlorophenoxyacetic acid
(2,4-D)		 Not mentioned 20 mg/L 0.20 g/L PMS
O3		 PMS 2.0 mM;
O3 16.0 mg/L;		 40 88.9 5
(>80%)		 Coprecipitation [8]
CoFe2O4 Atrazine
(ATZ)		 ·SO4− 10 mg/L 0.4 g/L PMS 0.8 mM 30 >99 5
(>60%)		 Hydrothermal [19]

2. MeFe2O4 Combined with the Carrier

The carrier recombination method can increase the specific surface area and increase the contact of chemical sites [20], thus greatly improving the rate of chemical reaction. At present, SiO2 [20][21], black phosphorus [22][23], and rGO [24][25] (reduced graphene oxide) are commonly used as carriers. After compositing with the carrier, it is closely combined with the carrier by van der Waals force [24] or electrostatic interaction [26], making it difficult to fall off the surface of the carrier.
Pure graphene is a benzene-ring-like two-dimensional nanomaterial consisting of sp2 hybrid orbitals. However, its high production cost limits its large-scale application. Afterward, by improving Hummer’s method, a large number of oxygen-containing functional groups were linked at the edge of the plane by a strong oxidant, hence the name GO (graphene oxide) (Figure 1); rGO (Figure 2) was obtained by sodium borohydride and other means of reduction, which has low synthesis cost and is suitable for use as a good carrier of catalysis.
Applsci 11 11314 g001 550
Figure 1. Plane structure (left) and solid structure (right) of GO (bond line type).
Applsci 11 11314 g002 550
Figure 2. Plane structure (left) and solid structure (right) of rGO (bond line type).
Taking CuFe2O4, a representative of MeFe2O4, as an example, by comparing the effect of pure CuFe2O4 with that of CuFe2O4 combined with the carrier, it can be seen that the latter has a stronger catalytic effect under acidic and photoinduced conditions [27]. CuFe2O4 in CuFe2O4–rGO is closely combined with the oxygen-containing groups on rGO through electrostatic interaction, as shown in Figure 3. Images from a scanning electron microscope are shown in Figure 4.
Applsci 11 11314 g003 550
Figure 3. Chemical structural formula of CuFe2O4-rGO [26].
Applsci 11 11314 g004 550
Figure 4. TEM images of (a,b) rGO/CuFe2O4 nanostructures under different magnifications [26].
Table 2 shows the degradation effects of some CuFe2O4 and rGO composite materials on different kinds of wastewater. It can be seen from the table that the composite catalyst can still produce good effects even without the presence of PS. Not only the Cu, Fe, and other elements in the catalyst can produce pure chemical catalytic effect, but the carrier rGO can produce electron transition under the light condition, promoting the transfer of electrons, and plays a part of the photocatalytic effect [28][29]. Table 2 contains some other carriers, which can also greatly influence degradation of different kinds of wastewater.
Table 2. Effects of partial MeFe2O4 and carrier composite materials on degradation of different kinds of wastewater [27][30][31][32][33][34][35][36].
Catalyst Pollution Main Mechanism Pollutant Concentration Catalyst Concentration Oxidant Oxidation Concentration T/min Degradation Rate /% Number of Cycles Synthesis
Techniques		 Ref.
CuFe2O4-
20%rGO		 Methylparaben SO4−·
·OH		 10 mg/L 0.2 mg/L PS 5 mM 120 96 Not mentioned Sol-gel [30]
CuFe2O4-
1% (w/w)
rGO		 Phenol ·OH 20 ppm 5 mL 30%
H2O2		 6 mg/L 240 100 Not mentioned Coprecipitation [27]
CuFe2O4/g-C3N4 Propranolol SO4−· 0.02 mM 1 g/L PS 1 mM 120 82.2 Not mentioned Sol-gel [31]
CoFe2O4/CCNF Dimethyl phthalate SO4−· 0.05 mM 0.5 g/L PMS 1.5 mM 60 >90 5
(>90%)		 Sol-gel [32]
TiO2@CuFe2O4/UV 2,4-D SO4−· 20 mg/L 0.1 g/L PMS 0.3 mM 60 97.2 5
(>90%)		 Sol-gel [33]
ZnS-ZnFe2O4 Rhodamine B SO4−· 20 mg/L 20 mg PS 5 mg 90 97.67 3
(>95%)		 Hydrothermal [34]
Fe2O3@CoFe2O4 NOF SO4−·
·OH		 15 μM 0.3 g/L PMS 0.4 mM 25 89.8 4
(90%)		 Hydrothermal [35]
Nitrogen and sulfur codoped CNTs-COOH loaded CuFe2O4 2-Phenylbenzimidazole-5-sulfonic acid SO4−· 5 mg/L 50 mg/L PMS 1:100 (molar ratio) 40 98 5
(>95%)		 Coprecipitation [36]
@: the composite of two materials.

3. Activation Persulfate by Fe0

In recent years, activation persulfate based on Fe0 (zero-valent iron, ZVI) have been widely used in chemical production and environmental remediation [37][38]. As mentioned above, the activation persulfate/Fe (II) mechanism can cause secondary pollution to water, so ZVI/PS [39][40] is used instead to reduce a series of problems caused by the reduction of Fe2+ content due to the change of pH and other factors in water [37].
ZVI/PS system has strong reducibility (Fe0,E0 = −0.44 V) [41]. Compared with CuFe2O4, its reaction process is more complex, as shown in Figure 5. Fe0 is first converted to Fe2+ in the presence of acid and oxidant, then further oxidized to Fe3+ by Fe2+, and finally to Fe(IV) [42][43]. The reaction mechanism follows [44]: According to the reaction equation, the reaction is easily affected by pH, and the reaction will gradually slow with the increase of pH. Weng et al. [45] point out that the Fe0/PS system exhibits two-stage kinetics. The kinetic first stage is mostly attributed to a heterogeneous reaction occurring on the surface of the Fe0 aggregate. As the reaction proceeds, decolorization shifts from the slow kinetic first stage to the fast kinetic second stage when sufficient Fe2+ ions are maintained in the system [46].
Fe0 + 2H+ → Fe2+ + H2
2Fe0 + O2 + 2H2O → 2Fe2+ + 4OH−
Fe0 + S2O82− → Fe2+ + 2SO42−
Fe0 + HSO5− → Fe2+ + SO42− + OH−
Fe2+ + S2O82− → Fe3+ + SO42− + ·SO4−
Fe2+ + HSO5− → Fe3+ + SO42− + ·SO4−
Fe0 + S2O82− → Fe2+ + 2·SO4− + SO42−
Fe0+2 HSO5− → Fe2+ + 2OH− + 2·SO4−
Fe2+ + S2O82− + H2O → FeIVO2+ + 2SO42− + 2H+
Fe2+ + HSO5− → FeIVO2+ + SO42− + H+
Applsci 11 11314 g005 550
Figure 5. Schematic of the formation of ·SO4− and Fe(IV) in nZVI/persulfate systems containing methyl phenyl sulfoxide [47].
Figure 6 shows the proposed degradation pathway of 2,4-D [48]. By examining Figure 6, it can further confirm that macromolecular organic matter is decomposed into small molecular organic matter, which is gradually mineralized.
Applsci 11 11314 g006 550
Figure 6. The proposed degradation pathway of 2,4-D [48].
Table 3 shows the degradation effects of various types of polluted water bodies activated by PS/PMS based on elemental iron. Usually, an appropriate amount of H2O2 [49] will be added to the water when PS is activated by Fe0, so as to reduce the cost of oxidant. Through the analysis of the table, it can be seen that the effect of ZVI when used alone [50] is worse than when it is combined with the carrier or when other conditions exist.
Table 3. Degradation effect of different kinds of wastewater based on PS/PMS activated by different kinds of iron [51][52][53][54][55][56][57][58].
Catalyst Pollution Main Mechanism Pollutant Concentration Catalyst Concentration Oxidant Oxidation Concentration T/min Degradation Rate /% Number of Cycles Synthesis
Techniques		 Ref.
nZVI Sulfamethazine ·OH
·SO4−		 50 mg/L 2 mM PS
H2O2		 1 mM
0.5 mM		 30 96 Not mentioned Sol-gel [54]
CN-Fe Sulfamethazine ·SO4−
·OH
1O2		 50 μM 0.5 g/L PMS 1 mM 15 82 Not mentioned Carbothermal [53]
Carbon-coated nZVI 4-chlorophenol ·SO4−
·OH		 150 μM 0.25 g/L PMS 1 mM 120 96 Not mentioned Commercially available [52]
US-nZVI Chloramphenicol ·SO4−
·OH		 5 mg/L 0.5 g/L PMS 1 mM 90 98.1 Not mentioned Liquid phase reduction [51]
Fe0@Fe3O4 Dibutyl phthalate ·OH
·SO4−		 18 μM 0.5 g L−1 PS 1.8 mM 180 94.7 6
(>68%)		 Calcination [55]
Fe0@Fe3O4 Atrazine ·OH
·SO4−		 500 μg/L 25 mg/L PMS 1 mM 2 100 Not mentioned Reduction [56]
Fe@C Bisphenol S ·OH
·SO4−		 5 mg/L 0.5 g/L PMS 1.0 mM 60 92.8 Not mentioned Resin carbonization [57]
Fe@C/PB 2,4-DichloroPhenol ·OH
·SO4−		 20 mg/L 0.6 g/L PMS 2.0 g/L 50 99.4 Not mentioned Calcination [58]
@: the composite of two materials.

4. Fe3O4

Fe3O4 magnetite, also known as magnetic iron oxide, is a black crystal with a rotating spinel structure (Figure 7). In magnetite, Fe2+ and Fe3+ are disordered on the ferrite octahedron, so electrons can transfer rapidly between Fe2+ and Fe3+; thus, reversible redox reactions can occur at the same position on the octahedron.
Applsci 11 11314 g007 550
Figure 7. Crystal structure of Fe3O4.
However, since Fe3O4 is easy to accumulate in solution and contact sites are reduced after agglomeration, single Fe3O4 is rarely used. Using the composite carrier method [59] can not only solve these problems, but also speeds the reaction rate, making it more cost effective when applied in industrial production. He et al. [60] pointed out that the Fe3O4/GO/Ag composite microspheres are formed using magnetic Fe3O4 as cores, followed by coating an internal layer of GO and an outer layer of Ag nanoparticles, as Figure 8 shows. The synthesized Fe3O4/GO/Ag composite catalyst under the action of NaBH4, methylene blue, and ciprofloxacin can be completely degraded within 12 min. Figure 8 shows SEM images of Fe3O4/GO/Ag composite catalyst. In Figure 9, we can clearly observe that Ag has been completely attached to the Fe3O4/GO surface, which can increase the specific surface area and improve the chemical reaction rate.
Applsci 11 11314 g008 550
Figure 8. Illustration of the fabrication of Fe3O4/GO/Ag composite microspheres [60].
Applsci 11 11314 g009 550
Figure 9. Typical FESEM images of (a) Fe3O4, (b) Fe3O4/GO, (c) Fe3O4/GO/Ag, and (d) Fe3O4/Ag microspheres. Inserts are magnified FESEM images of Fe3O4/GO/Ag and Fe3O4/Ag microspheres [60].
Table 4 shows the research progress of Fe3O4 and its composite materials on the degradation of different pollutants reported at present. According to the data in the table, when Fe3O4 is compounded with the carrier, the catalytic performance is greatly improved.
Table 4. Effects of Fe3O4 and its composite-material-activated PS/PMS on degradation of different kinds of wastewater [61][62][63][64][65][66][67].
Catalyst Pollution Main Mechanism Pollutant Concentration Catalyst Concentration Oxidant Oxidation Concentration T/min Degradation Rate /% Number of Cycles Synthesis
Techniques		 Ref.
Fe3O4 BPA ·SO4−
·OH		 20 mg/L 2.0 g/L PMS 5 mM 30 27.53 Not mentioned Commercially available [61]
CuO-Fe3O4-BC BPA ·SO4−
·OH		 20 mg/L 2.0 g/L PMS 5 mM 30 100 4
(>85%)		 Coprecipitation [62]
rGO-Fe3O4 NOF 1O2
·OH
·SO4−		 20 mg/L 0.5 g/L PS 1 g/L 30 89.69 Not mentioned Coprecipitation [62]
Fe3O4 Sulfamonomethoxine ·SO4− 0.06 mM 2.4 mM PS 1.2 mM 15 100 Not mentioned Coprecipitation [63]
Fe3O4@Zn/Co-ZIFs Carbamazepine ·SO4− 5 mg/L 25 mg/L PMS 0.4 mM 30 100 Not mentioned Solvothermal [64]
Fe3O4/microwave irradiation (3 kW/L) p-Nitrophenol ·SO4− 20 mg/L 2.5 g/L PS 15:1 (molar ratio) 28 94.2 Not mentioned Not mentioned [65]
Fe3O4/MC p-Hydroxybenzoic acid ·SO4− 1.0 g/L 0.2 g/L PS 1.0 g/L 30 100 Not mentioned Sol-gel [66]
Fe3O4/graphene aerogels Malachite green Not mentioned 20 mg/L 0.2 g/L PS 1.0 mM 12 91.7 Not mentioned Sol-gel [67]
@: the composite of two materials.

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Subjects: Chemistry, Applied
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Keke Zhi
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Update Date: 24 Jan 2022
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