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Progress in Chemistry 2023, Vol. 35 Issue (10): 1415-1437 DOI: 10.7536/PC230510   Next Articles

• Review •

Millimeter-Sized Nanocomposites for Advanced Water Treatment: Preparation, Synergistic Effects and Applications

Wanyi Fu1, Yuhang Li1, Zhichao Yang1, Yanyang Zhang1,2, Xiaolin Zhang1,2, Ziyao Liu1, Bingcai Pan1,2,*()   

  1. 1 State Key Laboratory of Pollution Control and Resource Reuse, School of Environment, Nanjing University,Nanjing 210023, China
    2 Research Center for Environmental Nanotechnology (RCENT), Nanjing University,Nanjing 210023, China
  • Received: Revised: Online: Published:
  • Contact: *e-mail: bcpan@nju.edu.cn
  • Supported by:
    National Key R&D Program(2022YFA1205601); National Key R&D Program(2022YFA1205602); National Natural Science Foundation of China(21925602); National Natural Science Foundation of China(22236003)
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Nanomaterial features a high surface area-to-volume ratio and strong surface effects, offering excellent performance in water treatment and broad application prospects. Incorporating nanoparticles into millimeter-scale hosts to prepare millimeter-sized nanocomposite materials can couple the high reactivity of nanoparticles with the easy operability of millimeter-scale hosts. This is an important technical approach to overcome the engineering application bottlenecks of nanomaterials, such as their tendency to agglomerate, low stability, potential environmental risks, and difficult separation. This review summarizes the preparation methods, structural characteristics, and adsorptive and catalytic oxidative removal of pollutants from aqueous systems by millimeter-sized nanocomposites. It elaborates on the confinement effects from the perspectives of confined growth of nanoparticles, confined adsorption properties, and confined catalytic oxidation properties, as well as the synergistic purification effect between the hosts and nanoparticles. Finally, the scientific issues and practical challenges that urgently need to be addressed in the development of millimeter-sized nanocomposites are discussed. We believe this review will provide theoretical guidance and technical references for promoting the practical applications of nanomaterials.

Contents

1 Introduction

2 Common hosts and preparation methods of millimeter-sized nanocomposites

2.1 Polymeric hosts

2.2 Carbon-based hosts

2.3 Natural mineral based hosts

2.4 Ceramic-based hosts

3 Confinement effects and synergistic purification effects of millimeter-nanometer structure

3.1 Confined growth of nanoparticles in millimeter-sized hosts

3.2 Confined adsorption and regeneration of nanoparticles inside millimeter-sized hosts

3.3 Confined catalytic oxidation of nanoparticles inside millimeter-sized hosts

4 Practical applications of millimeter-sized nanocomposites in water treatment

4.1 Applications in adsorption

4.2 Applications in catalytic degradation

5 Conclusions and perspectives

5.1 Research gaps in scientific issues regarding nanoconfinement effects

5.2 Challenges to be addressed for practical applications of nanocomposite materials

Key words: millimeter-sized nanocomposite, confinement effects, water decontamination, adsorption, catalytic oxidation
Fig.1 (a) Categories of millimeter-scale host materials and (b~g) typical preparation methods for millimeter-sized nanocomposites[1,9,13,22,30,40]
Table 1 Studies on millimeter-sized nanocomposites with polymers as hosts applied in water decontamination
Millimeter-scale hosts Appearance
size of
hosts (mm)		 Embedded
nanoparticles		 Size of
nano-
particles
(nm)		 Preparation methods Target pollutants Removal mechanism Adsorption capacity (mg/g) Removal efficiency Treated water matrix Experimental scale Operation duration ref
Macroporous ion exchange resins
D201a 0.7~0.9 HZO N.A.b Impregnation-precipitation Phosphate Adsorption 21.3 N.A Effluent from
municipal WWTPe		 Fixed-bed column 1800 BV 2
D201 0.6~0.7 HZO 20~40 Impregnation-precipitation As(V) Adsorption 70.53 N.A. Acidic mining effluent Fixed-bed column 2900 BV 3
D201 0.4~1.0 HLO 3.56~
67.23		 Impregnation-precipitation Phosphate Adsorption N.A. 91.23% River water Pilot-scale fixed-bed 8 months,
10 m3/d		 5
D201 0.9~1.1 nZVI 2~11 Impregnation-precipitation Cu(Ⅱ)-
EDTA		 Adsorption N.A. 88.3% Synthetic solution Fixed-bed column 500 BV 6
D201 0.4~0.8 HFO N.A. Impregnation-precipitation Selenite Adsorption ~37 N.A. Simulated wastewater Fixed-bed column ~1200 BV 107
D201 0.6~1.0 HFO N.A. Iron exchange-
precipitation		 Phosphate Adsorption 17.8 N.A. Industrial effluent from a pesticide plant Fixed-bed column ~930 BV 10
D201 N.A. Li/Al LDHsc 5~20 Iron exchange-
precipitation		 Fluoride Adsorption 32.6 N.A. Fluoride contaminated groundwater Fixed-bed column ~155 BV 84
D201 0.7~0.9 CeO2 2.5~4.2 Iron exchange-
precipitation		 As(Ⅲ) Oxidation-adsorption 9.96 99.6% Simulated wastewater Fixed-bed column ~6500 BV 108
D201 0.6~0.8 nZVI 10~30 Iron exchange-reduction Se(Ⅵ) Adsorption N.A. >99% Simulated wastewater Fixed-bed column ~1240 BV 109
D201 (chloride type) 0.6~1.0 HFO 12.3 Iron exchange-
precipitation		 Phosphate Adsorption N.A. <0.5 mg/L Biochemical effluent
from municipal WWTP		 Field fixed-bed 3500~4000 BV 79
Cation exchanger D001 ~1 HFO N.A. Impregnation-precipitation Cu(Ⅱ)-
citrate		 Adsorption/
Oxidation		 N.A. 81.6% Simulated wastewater Fixed-bed column 1300 BV 110
Strongly basic anion
exchanger HAIX		 0.5~0.7 HFO N.A. Iron exchange-
precipitation (commercial ArsenXnp)		 As Adsorption N.A. <50 μg/L Arsenic well water Field fixed-bed 29 000 BV 7
Strongly basic anion
exchanger HAIX		 0.3~1.2 HFO 3~5 Iron exchange-
precipitation (commercial
ArsenXnp)		 As(V) Adsorption N.A. <10 μg/L Arsenic drinking water Field fixed-bed 91~120 days 86
Anion exchanger IRA-900 N.A. HFO N.A. Iron exchange-
precipitation		 Phosphate Adsorption N.A. <10 μg/L Secondary effluent
from municipal WWTP		 Fixed-bed column 1500 BV 111
Anion exchanger
DOWEXTM M4195		 0.3~0.8 HFO N.A. Impregnation-
precipitation		 Phosphate Adsorption N.A. <10 μg/L Simulated wastewater Fixed-bed column ~320 BV 112
Cross-linked ion exchange resins
Highly cross-linked
anion exchanger of
polystyrene matrix		 0.6~0.7 HZO N.A. Impregnation-precipitation Fluoride Adsorption 20.9 <1.5 mg/L Simulated fluoride-
containing groundwater		 Fixed-bed column ~80 BV 82
Cross-linked anion
exchanger		 0.45~
0.55		 HFO 11.6 Impregnation-precipitation As(V) Adsorption 31.6 <10 μg/L Simulated wastewater Fixed-bed column 2950 BV 12
Strongly basic anion
exchanger of poly-
styrene matrix		 0.7~1.0 HMO 5.0~7.0 Impregnation-precipitation Phosphate Adsorption N.A. <0.5 mg/L Simulated wastewater Fixed-bed column 460 BV 54
Gel type ion exchange resins
Gel anion exchanger IRA-900 N.A. HFO N.A. Swelling-precipitation As(V) Adsorption N.A. >90% Simulated wastewater Fixed-bed column 10,000 BV 64
Gel cation exchanger C-100 0.3~0.5 HFO 20~100 Coprecipitation Pb(Ⅱ) Adsorption N.A. <0.2 mg/L Lead-acid battery
wastewater		 Field fixed-bed 6500 BV 88
Gel strongly basic anion exchanger 201 × 4 N.A. HFO N.A. Iron exchange-
precipitation		 As(V) Adsorption N.A. <10 μg/L Simulated wastewater Fixed-bed column 3900 BV 22
Synthetic polymers
Polystyrene bead 2 FeOOH 2.0~7.3 Flash freezing-in situ growth As(V) Adsorption 140~190 N.A. Single contaminant
solution		 Laboratory beaker N.A. 13
Polystyrene bead 2 α-Fe2O3 3 Flash freezing-in situ growth As(V) Adsorption 32.0 <10 μg/L Simulated wastewater Fixed-bed column ~2900 BV 55
PDMS sponged 9 TiO2-Au 3~15 Sugar-template method RhB Photocatalysis N.A. ~96% in
3 h		 Single contaminant
solution		 Laboratory beaker N.A. 113
Polyurethane sponge N.A. Iron oxide N.A. Hydrothermal growth
method		 As(Ⅲ),
As(V)		 Adsorption As(Ⅲ): 4.2
As(V): 4.6		 <50 μg/L Simulated wastewater Fixed-bed column As(Ⅲ): 123 BV
As(V): 144 BV		 23
Natural polymers
Chitosan N.A. Iron oxide N.A. Impregnation-deposition Phosphate Adsorption N.A. 52.3% Stream water Pilot-scale adsorption tower 33 days 81
Bead cellulose 0.3~0.9 Fe(OH)3 200~300 Impregnation-deposition As(Ⅲ),
As(V)		 Adsorption As(Ⅲ): 99.6
As(V): 33.2		 <10 μg/L Simulated fluoride-
containing groundwater		 Fixed-bed column As(Ⅲ): 2200 BV
As(V): 5000 BV		 24
Table 2 Studies on millimeter-sized nanocomposites with carbon-based materials and natural minerals as hosts applied in water decontamination
Millimeter-scale hosts Appearance size of hosts (mm) Nanoparticles Size of na-
noparticles (nm)		 Preparation methods Target pollutants Removal mecha-nism Adsorption capacity (mg/g) Removal efficiency Treated water matrix Experimental scale Operation duration ref
Carbon-based material
Activated carbon 0.25~0.5 HFO 2 Impregnation-calcination As(V) Adsorption 5 N.A.a Single contaminant solution Laboratory conical flask N.A. 28
Straw biochar 5~10 Ce 2~5 Impregnation-precipitation- pyrolysis Phosphate Adsorption 77.7 N.A. Single contaminant solution Laboratory batch
adsorption experiments		 N.A. 114
Corncob biochar N.A. FeNi 880 Carbonization-activation RhB Photo-Fenton catalysis N.A. 97% in
90 min		 Single contaminant solution Laboratory photo-reactor N.A. 30
Biochar aerogel N.A. nZVI 50~100 Impregnation-Pyrolysis
reduction		 U (Ⅵ) Adsorption-reduction 720.8 90.1% in
80 min		 Single contaminant solution Laboratory conical flask N.A. 31
Coffee ground
biochar		 N.A. Pd 2~11 Impregnation-calcination 4-nitrophenol and meth-
ylene blue		 Catalytic reduction N.A. N.A. Single contaminant solution Laboratory beaker N.A. 115
Natural minerals
Zeolite N.A. nZVI 37~110 Impregnation-reduction As(V) Adsorption 47.3 59% in
180 min		 Single contaminant solution Laboratory batch
adsorption experiments		 N.A. 116
Zeolite 0.8~1.2 HAlO N.A. Impregnation-ion exchange Phosphate Adsorption 7.0 N.A. Simulated wastewater Fixed-bed column 137 BV 117
Zeolite N.A. La N.A. Hydrothermal method Phosphate Adsorption N.A. >95% Primary and secondary
effluent from wastewater
treatment plant		 Laboratory batch
adsorption experiments		 N.A. 118
Zeolite 0.18~0.25 Mg-Al-La ternary hy-droxides 82.1 Coprecipitation Phosphate Adsorption 80.8 <0.5 mg/L Single contaminant solution Fixed-bed column ~4800
BV		 119
Diatomite N.A. HFO N.A. Impregnation-calcination As Adsorption 20.5 < 50 μg/L Groundwater containing high
concentrations of arsenic		 Fixed-bed column 937 BV, 44 d 120
Diatomite N.A. Magnetite 15 Hydrosol method Cr(Ⅵ) Adsorption 69.2 N.A. Single contaminant solution Laboratory batch
adsorption experiments		 N.A. 121
Diatomite 0.15 nZVI 10 Hydrothermal reduction method Phosphate Adsorption 37.0 N.A. Single contaminant solution Laboratory batch
adsorption experiments		 N.A. 122
Diatomite 0.05 nZVI 20~60 Impregnation-reduction Simazine Catalytic reduction 0.97 N.A. Single contaminant solution Laboratory beaker N.A. 123
Table 3 Studies on millimeter-sized nanocomposites with ceramic-based materials as hosts applied in water decontamination
Millimeter-scale
hosts		 Appearance size
of hosts		 Nanoparticles Size of
nanoparticles		 Preparation methods Target pollutants Removal mecha-
nism		 Adsorption capacity
(mg/g)		 Treated water
matrix		 Experimental scale Operation duration ref
Al2O3 spheres
Al2O3 sphere 3-5 mm Cu-Co
bi-mental		 N.A.a Impregnation- carbothermal reduction COD of coal-gasification wastewater Catalytic ozonation 58.8% Coal-gasification wastewater Pilot-scale fixed-
bed, 5 m3/d		 30 days 39
Al2O3 sphere 3-5 mm Fe N.A. Impregnation-calcination P-nitrophenol Catalytic ozonation TOC: 68.1% Single contaminant
solution		 Laboratory fixed bed reactor 45 min 40
Al2O3 sphere 10.3 mm Fe2O3 N.A. Impregnation-calcination COD and color of distillery wastewater Catalytic ozonation COD: ~78%
Color: ~90%		 Distillery wastewater Laboratory ozone
reaction column		 30 min 124
γ-Al2O3 sphere 3-5 mm MnxCe1-xO2 ≤25nm Impregnation-calcination COD of coking wastewater Catalytic ozonation COD: >45.6% Bio-treated coking
wastewater		 Full-scale applica-
tion, 100 m3/h		 885 days 104
γ-Al2O3 sphere N.A. Mn-CeOx N.A. Impregnation-calcination Bromaminic acid Catalytic ozonation TOC: 64.7% Chemical industry
wastewater		 Pilot-scale ozone
oxidation tower		 22 days 106
γ-Al2O3 sphere 2 mm Cu-Mn oxides 5~10nm High-gravity-assisted im-pregnation Nitrobenzene Catalytic ozonation TOC: 81.7% Single contaminant
solution		 Laboratory high-
gravity rotating
packed bed		 60 min 125
γ-Al2O3 sphere 2 mm Ce-MnOx N.A. High-gravity-assisted im-pregnation Nitrobenzene Catalytic ozonation TOC: 98.3% Single contaminant
solution		 Fixed-bed column 100 min 126
Ceramic membranes
ZrO2/TiO2 flat
ceramic mem-brane		 Diameter 47 mm, thickness 2.5 mm FeOCl N.A. Impregnation-calcination Bisphenol A Fenton-like >82% Simulated wastewater Laboratory mem-
brane filtration		 120 h 75
α-Al2O3 flat ceramic
membrane		 Length 1046 mm, width 280 mm Mn oxides N.A. Impregnation-calcination DOC, PPCPs, EDCs Ozonation-ceramic membrane filtra-tion-biologically active carbon filtra-tion DOC:47.5%
PPCPs:98.5%
EDCs:99.8%		 Secondary effluent
from WWTP		 Pilot-scale,
20 m3/d		 48 days 46
α-Al2O3 flat ceramic mem-brane Diameter 22 mm, thickness 2 mm Co3O4 N.A. Impregnation-calcination Sulfamethoxazole PMS fenton-like 59% Single contaminant
solution		 Laboratory mem-
brane filtration		 100 min 44
α-Al2O3 flat ceramic
membrane		 Diameter 38 mm, thickness 2.5 mm Ti-Mn/TiO2 100nm Dip coating- calcination Dye Red-3BS and Aniline Catalytic ozonation CODCr:52.1% Simulated wastewater Laboratory mem-
brane filtration		 6 h 93
Al2O3 spheres
α-Al2O3 tubular
ceramic membrane		 Length 1016 mm, diameter 30 mm Ti-Mn/TiO2 20nm Dip coating- calcination Aquaculture wastewater Catalytic ozonation-membrane filtration CODMn: 38.0%
Color: 93.1%		 Aquaculture wastewater Pilot-scale 240 min 45
α-Al2O3 tubular
ceramic membrane		 Length 250 mm, outer diameter 10 mm, inner diam-eter 7 mm Ce/TiOx 8.3nm Sol-impregnation-calcination Diethyltoluamide Catalytic ozonation- membrane filtration 40% Single contaminant solution Laboratory mem-
brane filtration		 30 min 47
Tubular ceramic
membrane		 Length 1000 mm, diameter 30 mm TiO2 200~
500nm		 Impregnation-calcination COD of
dyestuff wastewater		 Membrane filtration- catalytic ozonation CODCr: >90% Secondary effluent
from dyestuff
WWTP		 Pilot-scale, 10 t/d 30 days 43
AAO template Diameter 24 mm, thickness 0.06 mm Fe3O4 N.A. Solvothermal
method		 Para-chlorobenzoic acid Heterogeneous Fenton N.A. Single contaminant
solution		 Laboratory con-
tinuous flow-through
experiment		 N.A. 66
Fig.2 Growth behavior and adsorption mechanism of confined and bulk zirconium phosphate[49]
Fig.3 Confined adsorption properties of milli-sized nanocomposites. (a) Changes in crystal phase of La(OH)3 for phosphate adsorption[63]; (b) The Donnan membrane effect of ion exchange resin for the enrichment and ion exchange of pollutants[11]; (c) The confinement-driven calcium phosphate partitioning crystallization and improved anti-pollution ability[65]
Fig.4 Confined catalytic oxidation in membrane pores. (a) Intensive utilization of HO· in confined space[66]; (b) Size exclusion effect of membrane pores on large molecular organic compounds and confined oxidation of small molecular organic compounds[75]
Fig.5 Millimeter-sized nanocomposites developed by Prof. Bingcai Pan’s research group. (a) Appearance of different composite materials; (b) Material samples; (c) Large-scale production of nanoscale composite materials; and (d) Fixed-bed water treatment engineering equipment
Fig.6 Catalytic ceramic membranes developed by Professor Xie Quan’s research group. (a) Tubular ceramic membranes; (b) membrane components; (c) flow diagrams and (d) on-site photos of pilot-scale equipment[91,92]
Fig.7 Flat ceramic membrane developed by Prof. Xihui Zhang’s research group. (a) flat ceramic membrane sheet; (b) ceramic membrane modules; (c) on-site photos and (d) process flow diagram of the pilot-scale ozone-ceramic membrane-BAC experimental equipment[95]
Fig.8 Mn-CeOx/γ-Al2O3 ozone catalysts developed by Professor Guoquan Zhang’s research group at Dalian University of Technology, with production photos and pilot-scale plant equipment diagram[106]
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