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化学进展 2023, Vol. 35 Issue (10): 1415-1437 DOI: 10.7536/PC230510   后一篇

• 综述 •

毫纳结构复合材料的制备、协同效应及其深度水处理应用

付宛宜1, 李雨航1, 杨志超1, 张延扬1,2, 张孝林1,2, 刘子尧1, 潘丙才1,2,*()   

  1. 1 南京大学环境学院 污染控制与资源化研究国家重点实验室 南京 210023
    2 南京大学 环境纳米技术研究中心 南京 210023
  • 收稿日期:2023-05-11 修回日期:2023-06-10 出版日期:2023-10-24 发布日期:2023-08-07
  • 作者简介:

    潘丙才 南京大学教授、环境学院副院长、南京大学环境纳米技术研究中心主任、国家有机毒物污染控制与资源化工程技术研究中心副主任。国家杰出青年基金获得者,入选教育部长江学者奖励计划、国家高层次人才特殊支持计划等。发表学术论文300多篇,论文总引用>20000次、H指数78,2014年至今连续入选Elsevier中国高被引学者榜单;授权国内外发明专利逾160件。研究方向为深度水处理技术及其原理,包括水处理纳米技术及原理、高级氧化还原技术及原理、污染物形态分析技术等。

  • 基金资助:
    国家重点研发计划(2022YFA1205601); 国家重点研发计划(2022YFA1205602); 国家自然科学基金项目(21925602); 国家自然科学基金项目(22236003)
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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:2023-05-11 Revised:2023-06-10 Online:2023-10-24 Published:2023-08-07
  • 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)

纳米材料具有较高的比表面积和较强的表面效应,在水处理领域展现出优异的净污性能,具有广阔的应用前景。将纳米颗粒负载于毫米级载体中制备毫纳结构复合材料,可有机结合纳米颗粒的高反应活性与载体的良好操作性,是突破纳米材料易聚团失活、难分离、稳定性差、潜在环境风险等工程应用瓶颈并实现规模化应用的重要技术手段。本文综述了毫纳结构复合材料的制备方法、结构特性及其在吸附和催化氧化除污性能及机制方面的研究进展,并从纳米颗粒的限域生长、限域吸附特性和限域催化氧化特性等方面阐述限域效应及载体-纳米颗粒的协同净污效应。最后,针对目前毫纳结构复合材料方向亟待解决的科学问题和实际应用挑战提出了展望,以期为推动纳米材料的实际应用提供一定的理论指导和技术参考。

关键词： 毫纳结构复合材料, 限域效应, 水处理, 吸附, 催化氧化

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
()
图1 用于制备毫纳结构复合材料的(a)载体材料类别及(b~g)各类典型的制备方法[1,9,13,22,30,40]
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]
表1 以高分子聚合物为载体的毫纳结构复合材料应用于去除水中污染物的研究
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
表2 以碳基材料和天然矿物为载体的毫纳结构复合材料应用于水处理的研究
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
表3 以陶瓷基为载体的毫纳结构复合材料应用于/降解去除水中污染物的研究
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
图2 纳米限域与开放体系中磷酸锆的生长行为及吸附机制[49]
Fig.2 Growth behavior and adsorption mechanism of confined and bulk zirconium phosphate[49]
图3 限域体系中纳米颗粒对污染物的吸附特性:(a)La(OH)3吸附磷酸根的晶型变化[63];(b)离子交换树脂的Donnan膜效应对污染物的富集及离子交换作用[11];(c)限域驱动磷酸钙分区结晶并提升抗污染能力[65]
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]
图4 膜孔的限域催化氧化特性:(a)限域空间内HO·高强度、集约化的高效利用[66];(b)膜孔对大分子有机物的尺寸排阻效应及对小分子有机物限域氧化[75]
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]
图5 潘丙才等开发的毫纳结构复合材料。(a)不同复合材料的外观;(b)材料样品;(c)规模化量产的毫纳结构复合材料和(d)固定床水处理工程装置。
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
图6 全燮教授等研发的(a)管式陶瓷膜、(b)膜组件、(c)中试装置流程示意图及(d)现场照片[91,92]
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]
图7 张锡辉等研发的(a)平板陶瓷膜、(b)膜组件、(c)臭氧氧化-陶瓷膜过滤-BAC中试实验现场装置图及(d)流程示意图[95]
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]
图8 大连理工大学张国权等研发的Mn-CeOx/γ-Al2O3臭氧催化剂、量产照片及中试现场装置图[106]
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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