Advanced Oxidation Processes (AOPs) for Bacteria Removal over MOFs-Based Materials

Hongyu Chu; Tianyu Wang; Chong-Chen Wang

doi:10.7536/220501

Progress in Chemistry ›› 2022, Vol. 34 ›› Issue (12) : 2700-2714 DOI: 10.7536/220501

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Advanced Oxidation Processes (AOPs) for Bacteria Removal over MOFs-Based Materials

Hongyu Chu ¹^,²
, Tianyu Wang ¹^,²
, Chong-Chen Wang ¹^,²^,^*

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Abstract

The pathogenic bacteria have exerted great threat to the safety of human being. Conventional antibacterial agents like antibiotics suffer from some limitations against drug-resistant bacteria. Thus, it is imperative to design novel antibacterial agents for efficient bacteria removal. Due to the tunable pores, abundant surface charge, periodically dispersed metal clusters and rich active sites, metal-organic frameworks (MOFs) can efficiently remove bacteria not only via the slowly released metal ions, but also via the corresponding advanced oxidation processes (AOPs) including photocatalysis, persulfate activation, Fenton-like reaction and photo-electrocatalysis. This review summarizes recent progress of antibacterial performances over MOFs-based AOPs catalysts (pristine MOFs, MOFs composites, MOFs derivatives and MOFs monoliths), in which the design strategies, antibacterial properties and antibacterial mechanisms are discussed. Finally, the challenges and the potential applications of MOFs-based catalysts are proposed.

Contents

1 Introduction

2 MOFs-based AOPs catalysts for bacteria removal

2.1 Pristine MOFs

2.2 Photosensitized MOFs

2.3 MOFs photo-electrodes

2.4 MOFs heterojunctions

2.5 MOFs derivatives

2.6 MOFs monoliths

3 Conclusions and outlooks

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Keywords

metal-organic framework / advanced oxidation process / catalyst / antibacterial / mechanism

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Hongyu Chu, Tianyu Wang, Chong-Chen Wang. Advanced Oxidation Processes (AOPs) for Bacteria Removal over MOFs-Based Materials. Progress in Chemistry, 2022, 34(12): 2700-2714 DOI:10.7536/220501

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1 Introduction

With the abuse of antibiotics, more than a dozen antibiotic-resistant bacteria have emerged in the past 50 years, which pose a great threat to human health^[1,2]^[3⇓~5]. Even Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus), which are ubiquitous in nature, have developed resistance. For example, Methicillin-resistant Staphylococcus aureus (Methicillin-resistant resistant S. aureus, MRSA) has been detected in wastewater. Bacteria exposed to antibiotics for a long time can enhance their resistance to antibiotics by changing their metabolic pathways and binding sites, modifying the targets of antibiotics and overexpressing active efflux systems^[6]. Therefore, it is necessary to find antibacterial materials with multi-mechanism synergy or low selectivity for bacterial cells as alternatives to antibiotics. Organic antibacterial agents represented by quaternary ammonium salts and chitosan and inorganic antibacterial agents represented by metal ions or simple substances have gradually become the main antibacterial materials^[7,8]. However, due to their poor stability and difficult to control the release of active ingredients, these antibacterial materials are easy to fail in a short time, and may have a greater toxic effect on environmental organisms and human normal tissues^[9]. Therefore, the development of new antibacterial materials is imminent.

Metal-organic frameworks (MOFs) are a kind of hybrid porous crystalline materials constructed by organic linkers and inorganic Metal clusters through coordination^[10]. The structural diversity, morphology, and active sites of MOFs materials can be controllably adjusted by selecting different metal centers and different organic ligands under a variety of synthesis conditions.As a result, MOFs are endowed with a variety of functions and have a wide range of potential applications in the fields of adsorption, catalysis, sensing, gas storage and separation, antibacterial algae removal, supercapacitors and sample pretreatment^[11,12]^[13⇓~15]^{[16⇓⇓~19]}^[20⇓~22]^[23,24]^[25,26]^[27]^[28,29]. The main ways of MOFs inhibiting microorganisms can be divided into five aspects. Even if bacteria are resistant, they are difficult to survive, which is an advantage that traditional antibiotics do not have: (1) the slow release of metal ions/functional ligands, which non-selectively interact with cell components^[6]^{[25,26,30,31]}; (2) direct contact between active sites in MOFs and microbial cells^[32]; (3) nano-sized MOFs are ingested by cells and play a direct role inside the cells^[33]; (4) When guest molecules (generally drugs represented by antibiotics) are introduced into the pores of MOFs, there will be synergistic effect with guest antibacterial drugs^[34,35]; (5) Inducing the generation of Reactive oxygen species (ROS) under certain conditions (such as light) and removing bacteria through Advanced oxidation processes (AOPs). Among them, AOPs technology is an important method to efficiently kill harmful microorganisms, which can degrade bacterial components and prevent bacterial regeneration^[36].

In this paper, the work on improving the bactericidal performance of AOPs by MOFs through controlling the morphology, coordinating with a variety of metals, photosensitizing, preparing photoelectrodes, constructing heterojunction complexes (including constructing heterojunction derivatives), preparing derivatives, and preparing macroscopic MOFs matrix is summarized. Finally, the existing research bottlenecks are listed, and the research and development directions of MOFs-based materials in AOPs sterilization are prospected.

2 MOFs-based materials for advanced oxidation sterilization

MOFs can produce a large amount of ROS under the conditions of energy input such as light, ultrasound, and/or assisted by external oxidants such as H₂O₂ and persulfate, which can attack bacterial cells and promote their gradual decomposition^[37]^[38]. However, the conductivity of single MOFs is poor, and the recombination rate of photogenerated carriers is generally fast, so it is necessary to take various measures to improve the sterilization performance of AOPs^[39]^[40,41]. (1) facilitates the separation of photogenerated carriers^[41,42]. The photogenerated holes (h⁺) produced in the reaction have strong oxidation ability, and also react with other substances to produce stronger ROS. To avoid the recapture of h⁺, a common strategy is to construct electron (e^-) capture traps that suppress the recombination of photogenerated electrons and holes. Electrons can also be conducted to other sites by composite electron acceptor materials. The electrons separated from the holes can also promote the formation of various free radicals and non-free radicals in the photo-Fenton system and the persulfate system, thereby further promoting the reaction^[43]; (2) to optimize the band structure^[44]. By combining with other narrow band gap semiconductor materials or photosensitizing materials to construct heterojunctions, construct derivatives, modify functional groups, and prepare bimetallic MOFs, the range of light absorption can be broadened, and the transport of carriers can be accelerated to promote the generation of ROS^[39]^[45]^[46]^[47]^[39,46,48].

2.1 Single MOFs

For a single MOF, its catalytic activity can be improved by controlling its morphology. Ye et al. Synthesized Cu-TCPP (BA) -MOF with ultrathin structure by one-pot method using copper ion (Cu²⁺) as metal node and -tetrakis (4-carboxyphenyl) porphine (Meso-Tetra(4-carboxyphenyl)porphine,H₂-TCPP) in porphyrin compound as organic linker^[49]. The addition of Benzoic acid (BA) in the synthesis process effectively promotes the coordination of porphyrin centers with copper ions, and weakens the face-to-face stacking (H-stacking) and edge-to-edge aggregation (J-aggregation) between MOF layers by increasing the charge repulsion between MOF layers, thus inducing the anisotropic growth process and obtaining the ultra-thin flake morphology^[50]. The thickness of this Cu-TCPP (BA) -MOF is only 2.06 nm, which is close to the thickness of the graphene layer. The MOF material can completely remove Escherichia coli with 10⁷CFU·mL^-1 under visible light irradiation at 2000 W·m^-2 for 50 min. The ultrathin morphology of the material is beneficial to the exposure of catalytic active sites^[51]. Among them, the Cu²⁺ and Cu⁺ cycles promote the generation of active substances. In the presence of peroxymonosulfate (PMS), Cu (II) -TCPP (BA) -MOF was transformed into Cu (I) -TCPP (BA) -MOF induced by light, and was oxidized by HS₅^- to produce ¹O₂ and · OH, which effectively killed E. coli, as shown in Figure 1 (a). The reaction is a non-radical advanced oxidation process dominated by ¹O₂.

In addition to controlling the morphology, the preparation of bimetallic MOF can also enhance its AOD performance. Bimetallic MOF can combine the advantages of many different types of metal clusters, and can also make up for the disadvantages of a single metal in some aspects, thus making the material more capable of performing well. At the same time, the stability of MOFs can be further improved^[47].

Both ZIF-8 and ZIF-67 have antibacterial activity, but single ZIF-8 only responds to ultraviolet light, while ZIF-67 has a visible absorption band, but its stability is relatively poor^[52]^[53]. Considering that the crystal structure and lattice parameters of ZIF-8 and ZIF-67 have good compatibility, the bimetallic MOF can be prepared by combining the advantages of the two. Ahmed et al. Synthesized bimetallic zeolite imidazole-type MOF with equal ratio of zinc and cobalt by one-pot coprecipitation of Zn²⁺ and Co²⁺ with 2-methylimidazole (Hmin) (Fig. 1(b))——Zn₅₀Co₅₀-ZIF^[47]. The water stability of Zn₅₀Co₅₀-ZIF is better than that of single ZIF-67 due to the unique Zn-N bond of ZIF-8. The cobalt element in Zn₅₀Co₅₀-ZIF will produce d-d transition, so it has the characteristic visible light absorption band of ZIF-67. Compared with pure ZIF-67, the visible absorption band of ZIF-67 showed a slight red shift, which was mainly due to the presence of Zn²⁺, which diluted the chromophore of Co²⁺ and slightly reduced the degree of d-d transition of Co. The bimetallic Zn₅₀Co₅₀-ZIF can effectively remove more than 60% of MRSA within 30 min under white light (the initial concentration is 1 mg·mL^-1). Dichlorofluorescein (DCFH) was used to detect the ROS produced in the photocatalytic process, and the results showed that ·O₂^- and · OH were the main active substances. In addition, the bimetallic Zn₅₀Co₅₀-ZIF has relatively good thermal and water stability. Compared with ZIF-67 alone, the material can maintain the stability of the frame structure after 10 days of immersion in water. Jiang et al. Prepared a bimetallic Zr/Ti-based PCN-224 type MOF material by exchanging Ti and part of Zr using a post-synthesis cation exchange method, as shown in Fig. 1 (C)^[54]. The absorption band of the bimetallic MOF extends to the visible region, and the photosensitivity of the bimetallic MOF is also significantly enhanced. The MOF could remove more than 96% of drug-resistant Acinetobacter baumannii, drug-resistant Escherichia coli, MRSA and methicillin-resistant Staphylococcus epidermidis with an initial concentration of 10⁵CFU·mL^-1 within 20 min. They further loaded the material on nanofiber fabric by electrospinning and found that it could promote wound healing as a dressing. Chen et al. Replaced the ligand H₂-TCPP in PCN-224 with Zn-TCPP, and prepared a bimetallic MOF with Zn involved in coordination, Zn-PCN-224, by a one-pot method^[55]. Since the strong spin-orbit of the Zn center can affect the excitation process, the singlet to triplet conversion energy decreases, further lowering the energy barrier. Therefore, the MOF can promote the transformation of photogenerated electron and hole pairs from singlet state to triplet state under visible light, thereby selectively generating ¹O₂, as shown in fig. 1 (d). Compared with PCN-224, Zn-PCN-224 could remove all E. coli within 6 H, which was 3. 5 times more efficient than PCN-224 alone under the same conditions. This study provides a new way to achieve photocatalytic sterilization without the separation of photogenerated electrons and holes.

2.2 Photosensitized MOFs.

The use of some ligands with photosensitive properties or the modification of photosensitive groups on MOFs can enhance the absorption ability of materials to visible light, thus promoting the catalytic sterilization performance of materials under visible light^[56].

Polydopamine (PDA) is an electron-rich (π-electron) photosensitizer, which can not only conduct electrons and inhibit the recombination of photogenerated electrons and holes, but also produce photothermal effect to convert light into heat to promote photocatalytic reaction^[56]. Wu et al. Used PDA to modify PCN-224 and utilized its photothermal effect and photocatalytic reaction to remove Escherichia coli and Staphylococcus aureus^[57]. The modification of PDA not only enhances the absorption of visible light, but also promotes the electron transfer between itself and MOF. The modified PCN-224 can not only convert more heat, but also achieve synergistic antibacterial and promote electron transfer, thereby promoting the generation of ¹O₂ to enhance the sterilization performance, as shown in fig. 2 (a). The material was able to remove 99.62% and 99.97% of Staphylococcus aureus and Escherichia coli, respectively, in 20 min under 660 nm light (the initial concentration of the two bacteria was 3×10⁷CFU·mL^-1).

Yan et al. Used the photosensitizer Chlorin E6 (Ce6) to modify ZIF-8 by coupling, and constructed a photocatalytic material ZIF-8-Ce6 with a response wavelength of 650 nm^[58]. MRSA with 10⁶CFU·mL^-1 can be completely removed within 30 min by using this material. The mechanism of sterilization is mainly the synergistic effect of the generation of ¹O₂ and the release of Zn²⁺ ions in ZIF-8. The contact between the active sites on the surface of the material and the bacteria also contributes to the inhibition of bacterial growth, as shown in Figure 2 (B).

2.3 MOFs photoelectrode

Photoelectrocatalysis is a heterogeneous photocatalytic process, which can further inhibit the recombination of photogenerated carriers by applying a bias voltage to the photoelectrode containing the catalyst, thus improving the efficiency of the original photocatalysis^[59]. Among them, the anode material is a key component in the photoelectrocatalytic process. Using MOFs as anodes can not only promote the separation of carriers, but also improve the stability of photoelectrodes to avoid their corrosion^[60].

Rosal et al. Synthesized two Zr-based MOFs (Zr-NDC and Zr-NDC-2NH₂) using naphthalene-2,6-dicarboxylic acid (NDC) and 4,8-diaminonaphthalene-2,6-naphthalene dicarboxylic acid (4,8-diaminonaphthalene-2,6-dicarboxylic acid,NDC-2NH₂) instead of terephthalic acid, respectively^[61]. Then the two kinds of MOFs were deposited on the graphite sheet as the anode (working electrode), and the Pt/Ti mesh was used as the cathode to explore the photoelectrocatalytic removal performance of the materials for Staphylococcus aureus under simulated solar illumination and electrification conditions. The results showed that the prepared electrode was able to achieve 99% removal of S. Aureus (initial concentration of 10⁸cells·mL^-1) within 20 min. Compared with the traditional terephthalic acid, the ligand used increases the conjugation effect of the aromatic ring, reduces the band gap value of the material, and enhances the light absorption capacity, thereby improving the photoelectrocatalytic sterilization performance of the material. Experiments were carried out under different light sources, and the results showed that the material had the best killing effect on Staphylococcus aureus under sunlight. This is due to the fact that the energetic photons in the solar spectrum can compensate for the energy difference between exciting the Ligand-to-cluster charge transfer (LCCT) from the ligand-to-cluster state. The anode bias generated after electrification can effectively inhibit the recombination of photogenerated carriers, so the sterilization effect is better than that under the condition of illumination alone, as shown in Figure 3. Due to the introduction of -NH₂ group into Zr-NDC-2NH₂, the absorption ability of Zr-NDC-2NH₂ for visible light and the generation ability of photocurrent were further improved, but there was no significant difference in the sterilization performance between Zr-NDC and Zr-NDC-2NH₂.

2.4 MOFs heterojunction

Heterojunction materials overcome the problems of easy recombination of narrow band gap photogenerated carriers and difficult generation of wide band gap photogenerated carriers in traditional semiconductor materials and molecular materials^[62]. Heterojunction materials are mainly divided into three categories: (1) semiconductor-semiconductor (S-S) heterojunction; (2) Semiconductor-metal (S-M) heterojunction^[62]; (3) a ternary heterojunction of semiconductor-semiconductor-metal or semiconductor-semiconductor-semiconductor. S-S heterojunction can be divided into type I heterojunction, type II heterojunction, type III heterojunction, P-N heterojunction and type Z heterojunction^[63]. S-M heterojunction can be further divided into Schottky heterojunction, Ohmic heterojunction and heterojunction mediated by Localized surface plasmon resonance (LSPR). S-S heterojunction and LSPR heterojunction are the most common MOFs-based heterojunctions used for sterilization.

There are usually four strategies to construct heterojunctions between MOFs and other materials: (1) MOFs are grown in situ on other materials that have been synthesized; (2) growing other materials on the synthesized MOFs in situ; (3) simultaneously adding a precursor of the MOFs and a precursor of other materials into a reaction system so that the precursors grow together to form a composite; (4) The synthesized MOFs and other materials were compounded by mechanical grinding and impregnation (Fig. 4)^[64].

Noble metal Nanoparticles (NPs) can produce LSPR effect under visible light, so they often play an important role in photocatalytic reactions, such as electron traps and reactive sites^[65⇓~67]. Sohrabnezhad et al. Used a hydrothermal method to load Ag/Ag₃PO₄ on IRMOF-1 (MOF-5), and explored the removal performance of Ag/Ag₃PO₄, IRMOF-1 and Ag/Ag₃PO₄-IRMOF-1 on Escherichia coli and Staphylococcus aureus in the dark and under visible light^[68]. When the concentration of Ag/Ag₃PO₄-IRMOF-1 was 100μg·mL^-1, the composite could inhibit the growth of all E. coli within 9 H in the dark (bacteria concentration was 10⁸CFU·mL^-1), and the bacteriostatic effect was much higher than that of Ag/Ag₃PO₄ and IRMOF-1 alone. The heterojunction material can remove all Escherichia coli within 2 H under illumination, and the sterilization effect is also much higher than that of Ag/Ag₃PO₄ and IRMOF-1 alone. This is because the electrons on the Ag₃PO₄ Conduction band (CB) can flow to the Fermi level on Ag NPs instead of staying on the Ag₃PO₄ lattice, thus effectively protecting Ag₃PO₄ from being dissolved. Then the electrons will continue to transfer to the Highest occupied molecular orbital (HOMO) of the organic ligand on IRMOF-1, which accelerates the separation of photogenerated carriers. In addition, Ag NPs will undergo LSPR effect and produce high-energy electrons, which can be transferred to IRMOF-1. With the electron transfer process, ·O₂^- was generated on the surface of the material, which together with h⁺ played a role in destroying bacterial cells, as shown in Fig. 5 (a). It is worth noting that the amount of Ag⁺ dissolved in Ag/Ag₃PO₄-IRMOF-1 is lower than that in Ag/Ag₃PO₄ under illumination, which is due to the fact that the electron transfer in the heterostructure effectively protects Ag₃PO₄ from being dissolved.

Polyaniline (PANI) is a kind of conductive polymer, which has the ability to respond to visible light. It can not only act as an electron donor, but also conduct h^+[69~71]. Wang et al. Prepared MIL-88B @ COF @ PANI ternary composite catalysts containing different proportions of MIL-88 B using stepwise self-assembly and injection methods^[72]. Among them, MIL-88B @ COF-200 @ 10% PANI was the most effective for the removal of E. coli (initial concentration of about 8×10¹⁰CFU mL^-1) and S. aureus (initial concentration of about 4×10¹¹CFU mL^-1), and the removal rate of the two bacteria was more than 90% in 60 min. The mechanism of photocatalytic sterilization is mainly due to the fact that MIL-88B and PANI, COF-200 and PANI constitute a double p-n heterojunction system. PANI with π-π stacking structure is used as a medium to promote the migration of photogenerated carriers and enhance the absorption capacity of the material for visible light; The electrons in the π^* orbital of PANI are transferred to the CB of MIL-88B and COF-200, respectively, and the h⁺ in the Valance band (VB) of MIL-88B and COF-200 are transferred to the π orbital of PANI, respectively. The consequent · OH, ·O^2- and h⁺ are the main reactive species of the reaction, as shown in Fig. 5 (B).

Compared with Fenton/Fenton-like reaction, the activation of Peroxydisulfate (PDS) and PMS by MOFs-based materials can produce $\mathrm{SO}_{4}^{\cdot-}$ with stronger selectivity and higher redox potential, and the reaction process is also very rapid, and the applicable pH range of the $\mathrm{SO}_{4}^{\cdot-}$ is wider^[73]. These $\mathrm{SO}_{4}^{\cdot-}$ attack the organic components of the bacterial cell, causing the cell to disintegrate. Pulgarin et al. First loaded ZIF-67 NPs on Graphene oxide (GO) in situ by room temperature stirring method^[74]. Then the Ag-ZIF-67 @ GO nanocomposite materials were obtained by immersing the ZIF-67 @ GO in silver nitrate solution and reducing Ag NPs on the ZIF- 67 @ GO in situ using NaBH₄ as a reducing agent. The material can activate PMS under visible light and remove all E. coli within 15 min (initial concentration of 10⁶CFU·mL^-1). Through comparative experiments and free radical trapping experiments, it was found that the reaction process was dominated by free radicals, and · OH and $\mathrm{SO}_{4}^{\cdot-}$ were the most important ROS. This antibacterial process involves multiple reaction pathways, including direct activation of PMS by visible light and activation of PMS by cobalt ions (Co²⁺, Co³⁺). The results of XPS characterization proved that a small amount of AgO formed during the synthesis process formed a new heterojunction with ZIF-67. The LSPR effect of Ag facilitates the transfer of photogenerated electrons from ZIF-67 to the Ag⁰ nanoparticles via AgO, thus promoting the generation of free radicals (as shown in Fig. 5 (C)).

Materials with photoresponse in the Near-infrared (NIR) region generally have photothermal effect, which can cooperate with ROS to kill bacteria through heat production^[75]. Prussian blue (PB) is widely used to inhibit the growth of fungi and cancer cells due to its photosensitivity and photothermal properties, and it is also a MOF with relatively low cytotoxicity^[76]^[77]. PB is not only a near-infrared responsive material, but also can be complexed with other MOFs^[76,78]. Wu et al. Prepared PB/PCN-224 heterojunction on the synthesized PB by using precursor in-situ oil bath synthesis, so that PCN-224 was attached to the surface of PB^[79]. The photocatalytic degradation performance of the material on Staphylococcus aureus and its biofilm in 10⁷CFU·mL^-1 under visible light of 660 nm was investigated. Cell morphology, lysate, and intracellular ROS were monitored. Meanwhile, cytotoxicity experiments were performed in vitro and wound healing experiments were performed in vivo. Under the irradiation of 660 nm light, the composite could remove 99. 84% and 99. 3% of Staphylococcus aureus and its biofilm within 15 min. The material showed little toxicity to mouse fibroblasts (NIH-3T3) in vitro. In vivo experiments in mice have shown that it can accelerate wound healing due to its excellent antibacterial properties, and the damaged tissue can be restored to its original state after 8 days. The main mechanism of the reaction is that the introduction of porphyrin ligand into PCN-224 enlarges the absorption range of MOF for visible light. PB plays a dominant role in the light-driven thermal effect of the heterojunction; PB and PCN-224 form a type II heterojunction, which promotes the transmission of photogenerated carriers between them and improves the performance of photocatalytic sterilization. ¹O₂ is the main active species in this photocatalytic reaction, as shown in Fig. 6 (a).

Wu et al. Also introduced porphyrin ligand H₂TCPP into the defects of UiO-66, and prepared TCPP-doped UiO-66 and PB @ TCPP @ UiO66 core-shell structure materials, in which, TCPP-doped UiO66 was the outer layer and PB was the inner layer^[80]. In this heterojunction structure, TCPP can promote the electron transfer of PB and inhibit the recombination of photogenerated carriers, as shown in Fig. 6 (B). Under the irradiation of dual-wavelength light (808 nm near-infrared light and 660 nm red light), the composite can not only produce ¹O₂, but also photothermal effect under near-infrared light, which can remove 99. 31% of Staphylococcus aureus (initial concentration of 10⁸CFU·mL^-1) and 98. 68% of Escherichia coli in 10 min, respectively.

Sulfur-doped g-C₃N₄ can increase the VB position and improve the migration efficiency of photogenerated carriers^[81]. Based on this idea, Younis et al. Used in-situ encapsulation of 5% zinc-doped titanium nitride (Zn_0.05TiO_xN_y) and composited it with MOF-5 and large particle g-C₃N₄(BCN)/ sulfur-doped g-C₃N₄(SCN) by microwave method^[82]. The inactivation of Escherichia coli, Staphylococcus aureus and Candida albicans (C. albicans) in industrial textile wastewater in the dark and under the visible Light of light-emitting diode (LED) was investigated. The results showed that Zn_0.05TiO_xN_y@SCN and Zn_0.05TiO_xN_y@MOF-5 could remove 97% ~ 99.3% of bacteria under the induction of visible light, and the efficiency of photocatalytic bacteria removal was 0.91~1.69 mCFU·Einstein^-1. This is due to the fact that Zn_0.05TiO_xN_y@SCN and Zn_0.05TiO_xN_y@BCN belong to the Z-type heterojunction, while Zn_0.05TiO_xN_y@MOF-5 is the I-type heterojunction. Among them, · OH, ·O₂^-, h⁺ are the main reactive species involved in the reaction, as shown in Fig. 6 (C).

The semiconductor MnO₂ has the advantages of weak toxicity, good biocompatibility, easy synthesis, good photostability and low cost^[83,84]. However, the disinfection effect of MnO₂ alone is still not ideal^[83,84]. Zhou et al. Used a two-step synthesis method to grow ZIF-8 in situ on the MnO₂ synthesized in the first step, and prepared MnO₂/ZIF-8 nanorods^[85]; Cell Counting Kit-8 (CCK-8) assay was used to explore the cytotoxicity of Cell Counting Kit nanorods on human bronchial epithelial cells (16HBE). Multidrug-resistant Escherichia coli (bnbio BNCC186732) was selected as a representative strain to explore the synergistic photocatalytic bactericidal performance of MnO₂/ZIF-8 nanorods under simulated sunlight (xenon lamp, light intensity 100 mW·cm^-2). The results showed that the material had a rapid sterilization effect under sunlight, and could completely remove the multidrug-resistant Escherichia coli of 5×10⁵CFU·mL^-1 within 30 min, and had good biocompatibility. ¹O₂ is the main active species in the sterilization process. In the photocatalyst heterostructure, there is h⁺ conduction between VB of ZIF-8 and VB of MnO₂. The h⁺ on VB and the indirectly generated · OH in the two materials, together with the indirectly generated ¹O₂ on CB of ZIF-8, play the role of oxidative sterilization, as shown in Fig. 6 (d). The increase of oxygen vacancies in the heterojunction suppresses the recombination of photogenerated electrons and holes.

MoS₂ has a graphene-like structure and is widely used in photothermal therapy. However, the electron and hole pairs generated by a single MoS₂ under the excitation of light are easy to recombine^[86]. Complexing MoS₂ with MOFs can effectively solve the above deficiencies. Wu et al. Directly mixed Zn²⁺ solution with MoS₂ to prepare Zn-doped MoS₂^[87]. Then the heterojunction nanosheets of ZIF-8@Zn-MoS₂ were prepared by ZIF-8 in-situ growth method using the difference between the work functions of Zn-MoS₂ and ZIF-8. Among them, the doping of Zn reduces the work function of MoS₂ and reduces its band gap value, which can promote the movement of the generated electrons to the surface of the material. A built-in electric field is formed between ZIF-8 and Zn-MoS₂, which constitutes a p-n type heterojunction and can accelerate the separation and migration of photogenerated carriers, as shown in Fig. 6 (e). The material was able to remove 99.9% of S. Aureus (initial concentration of 10⁵CFU·mL^-1) in 20 min under visible light at 660 nm. The mechanism of sterilization is the synergistic effect of ROS (mainly ¹O₂) produced by photocatalysis, photothermal effect and Zn²⁺ release. Among them, the release of Zn²⁺ also helps to promote wound healing.

2.5 MOFs derivatives

MOFs can not only be directly compounded with other semiconductors and/or conducting polymers, but also be used as self-sacrificial templates. Metal/metal oxide-doped carbon-based catalytic materials or metal sulfides produced by calcination can retain the unique structure of the original MOFs, and may also form a hollow or core-shell structure, which not only improves the stability of the material, but also makes the uniformly dispersed active sites more conducive to the transport and capture of carriers^[45]^[92,93].

Zhang et al. Prepared Ag/ZnO @ C hollow particles by salt sealing method using ZIF-8 impregnated with Ag⁺ as precursor^[89]. The derivative has a hollow ZnO shell structure with a specific surface area of up to 113 m²·g^-1. The silver nanocrystals are uniformly embedded in the surface of ZnO, which is beneficial to the rapid transfer of e^- between the two phases. At the same time, the introduction of silver produces LSPR heterojunction, which enhances the visible light absorption range of the material. Experiments for removal of E. Coli were carried out under dark conditions and simulated sunlight. The results show that the material can achieve complete removal of E. coli with a concentration of 10⁷CFU·mL^-1 within 120 min, in which ·O₂^- and · OH are the main active substances, as shown in Fig. 7 (a). Wang et al. Derivatized Zn-BTC microrods to obtain ZnO-C hollow nanocomposites by pyrolysis, and then obtained Ag-ZnO-C materials by in-situ photoreduction of AgNO₃^[90]. Unlike the Ag/ZnO @ C prepared by Zhang et al., the carbon-based material is caterpillar-like and retains the rod-like structure of the original MOF^[89]. They proposed a "directional attachment" growth mechanism to explain the mechanism of structure formation. The three-dimensional hierarchical structure formed by the carbon doping of the ZnO crystal and the amorphous carbon matrix in the material, combined with the LSPR effect of Ag, is beneficial to the absorption of visible light. Carbon doping plays the role of electron reservoir and electron transfer, which promotes the formation of active material. The experimental results show that the material can efficiently remove Escherichia coli with an initial concentration of 10⁶CFU·mL^-1 under visible light at a rate of 6.25×10⁵CFU·mg^-1·min^-1. Subsequently, the material was loaded on the nanofiber membrane, which also had better AOPs sterilization performance, as shown in Fig. 7 (B).

Chen et al. Prepared TiO₂ and carbon-doped materials C1-MIL-125 and C2-MIL-125 using a one-step hydrothermal method and a two-step hydrothermal method, respectively, using poplar wood hydrolysate and the precursor of MIL-125 (Ti)^[94]. Characterization by XRD and Transmission electron microscope (TEM) shows that the two derivatives have crystalline phases with two Transmission electron microscope of anatase and rutile. C1-MIL-125 is a spherical particle, while C2-MIL-125 is a rough flaky particle. The C2-MIL-125 prepared by the two-step hydrothermal method has larger specific surface area and richer porosity, and can promote the transfer of photogenerated electrons. TEM can observe the uniform distribution of carbon dots in C2-MIL-125, which can effectively improve the absorption of visible light, and facilitate the distribution and transmission of photogenerated electrons, thus promoting the production of more ROS. Both derivatives killed more than 98% of E. coli in 20 min compared to dark controls with initial E. coli colonies of approximately 422 CFU and 401 CFU. Among them, · OH, ·O₂^- and ¹O₂ were the main active species in the reaction system. Li et al. Directly calcined the NH₂-MIL-125(Ti) at high temperature to obtain the graphitic carbon material C-Ti-MOF with uniformly embedded TiO₂ nanodots, as shown in Fig. 7 (C)^[95]. The composite combines the advantages that the carbon nanomaterial can absorb near-infrared light to generate photothermal effect and the TiO₂ can carry out photocatalytic reaction, and the carbon nanomaterial also widens the absorption range of the original TiO₂ to visible light. When the dosage of the material is only 0.16 mg·L^-1, it can almost completely remove 10⁷CFU·mL^-1 of Staphylococcus aureus. Among them, ·O₂^- and ¹O₂ are the main active substances in the reaction system.

CuS is also a photoresponsive material in the near infrared region^[96]. Wu et al. Used Cu-based MOF (HKUST-1) as a self-sacrificial template to convert part of HKUST-1 into derivative CuS NPs by in-situ sulfurization and uniformly embedded in HKUST-1^[97]. Through characterization, it was found that HKUST-1 could restrain the CuS nanoparticles and prevent the excessive release of Cu²⁺ ions, which helped to reduce the toxicity of the material to cells. The material (CuS @ HKUST-1) has good killing effect on Escherichia coli and Staphylococcus aureus. Within 20 min, 99.7% of Staphylococcus aureus and 99.8% of Escherichia coli (initial concentration of 10⁷CFU·mL^-1) could be removed by the synergistic effect of photothermal effect and ROS. The sterilization mechanism of this material is shown in Fig. 7 (d). Wu et al. Continued to modify PDA on CuS @ HKUST-1, which further enhanced the heat and free radical generation ability of nanoparticle materials^[57]. Compared with CuS @ HKUST-1, the killing efficiency of PDA modified CuS @ HKUST-1 against Staphylococcus aureus and Escherichia coli reached 99. 77% and 99. 57%, respectively.

2.6 MOFs-based macroscopic materials.

MOFs and their derivatives or composites are mostly powder structures, or need to be ground into powder before application. These powder materials are not easy to be recycled or removed in water, and because some MOFs powder particles have high surface energy, they are easy to agglomerate in water, which reduces the number of active sites exposed and the contact area with the target, thus affecting the efficiency of sterilization^[98]. The poor water stability of some MOFs powders leads to the rapid dissociation and release of metal ions, which not only increases the toxicity to aquatic organisms or normal cells, but also shortens the service life and action time of the materials^[99]. In addition, MOFs powder is not conducive to the use in large-scale sewage treatment facilities. The ultrafine powder formed by dispersed MOFs can lead to a sharp increase in bed pressure drop and reactor blockage in practical water treatment facilities, which is not suitable for the treatment of pollutants in continuous influent water^[100]. Therefore, it is necessary to load MOFs on suitable substrates to prepare macroscopic MOFs-based components (such as membranes, gels, coatings, fiber papers, etc.) To solve the above problems^[101]^[102]^[103]^[78]. The interaction between the substrate and MOFs mainly includes: (1) The substrate increases the stability and durability of the original MOFs-based materials, while reducing the release rate of metal ions. The substrate can improve the stability of MOFs materials and alleviate the ion release behavior caused by the dissociation of MOFs through the bonding or physical masking effects between functional groups and MOFs^[104,105]. (2) The substrate increases the effective contact area between the original MOFs-based material and the target microorganism. By loading MOFs-based materials on planar films or other substrates, the effective contact area with bacteria can be increased, and it is also more conducive to more efficient absorption and utilization of energy in incident light to produce more active radicals^[106]. (3) The substrate increases the recyclability of the original MOFs-based material and endows the composite with excellent mechanical properties (wear resistance, flexibility, shape memory properties, etc.)^[107,108]. (4) MOFs change the characteristics of the original substrate. On the one hand, MOFs can regulate the hydrophilicity, pore distribution and structure of the substrate; on the other hand, the incorporation of MOFs can also change the original charge characteristics of the membrane substrate, resulting in electrostatic attraction or repulsion to bacteria^[101]^[109].

Fluore scence resonance energy transfer (FRET) effect can effectively promote the production of ROS^[110,111]. graphene quantum dots (GQDs) can be used as FRET donors due to their fluorescence emission peak in the range of 400 nm ~ 600 nm, while PCN-224, as a commonly used porphyrin ligand MOF, can absorb visible light in the range of 400 nm ~ 500 nm and produce graphene quantum dots, so it can be used as FRET acceptors, and the two can form donor-acceptor pairs through recombination, thus promoting the photodynamic process^[112]^[112]^[113]. Wei et al. Used GQDs complexed with PCN-224 and immobilized on cotton fibers after amination treatment for killing a variety of bacteria^[112]. The results showed that the composite could kill more than 99.9% of various bacteria (S. aureus, B. subtilis, P. aeruginosa and E. coli) with an initial concentration of S. Aureus through the photodynamic process, and the reaction mechanism is shown in Fig. 8 (a). The material has guiding significance in the preparation and application of antibacterial fabrics.

CdS is a kind of photocatalyst which can respond to visible light, but it is easy to agglomerate in water, and the photogenerated carriers are easy to recombine, and the material itself is also prone to photocorrosion^[114,115]. The above problems can be solved by compounding CdS with MIL-101 and preparing macroscopic film materials. Wang et al. Synthesized CdS @ MIL-101 composites by solvothermal method, and then loaded the composites on Polyvinylidene fluoride (PVDF) by phase inversion method and immersion precipitation method to prepare membrane devices with different CdS @ MIL-101 loadings^[91]. The membrane device was combined with an underwater LED light source to explore its ability to remove Escherichia coli and Staphylococcus aureus. The results showed that when the loading mass fraction of CdS @ MIL-101 was 1%, the membrane device could remove 92% and 95% of Escherichia coli and Staphylococcus aureus in 10⁸CFU·mL^-1 within 3 H, respectively, and the continuous water treatment cycle (when the transmembrane pressure was greater than 35 kPa, it was regarded as the end of a cycle) of the membrane device could be extended from 10 ~ 14 d to 25 ~ 26 d. Confocal laser scanning microscope (CLSM) results showed that the Membrane device could significantly reduce the bacteria attached to the Membrane bioreactor (MBR), and at the same time, its hydraulic performance was better than that of the membrane without composite. Through active material trapping experiments and Photoelectrochemical tests, the researchers found that the CdS loaded on the octahedral MIL-101 surface formed a type II heterojunction with MIL-101, which promoted the migration of photogenerated electrons and holes. Among them, · OH and h⁺ are the main active species, as shown in Fig. 8 (B).

Metal mesh can not only be used as a support for MOFs, but also provide a metal ion source for the in situ growth of MOFs^[116]. An et al. Synthesized MIL-100 (Fe) on steel wire mesh by in-situ growth method, and PANI was uniformly dispersed on MIL-100 (Fe) by electrochemical deposition and heat treatment^[88]. With the assistance of a small amount of H₂O₂, Fenton-like bacteria killing and thiamphenicol degradation under visible light were studied. The results showed that the material could completely kill Escherichia coli with an initial concentration of 10⁷CFU·mL^-1 within 60 min, in which ·O₂^- and · OH were the main ROS; MIL-100 (Fe) and PANI formed a relatively stable type II heterojunction, which promoted the transport of photogenerated carriers between them, inhibited the recombination of photogenerated carriers, and improved the photocatalytic sterilization performance. It is worth mentioning that Fe (III) and Fe (II) in MIL-100 (Fe) can form a redox cycle, which can continuously produce · OH, as shown in Figure 8 (C). The material also has good stability and more than 90% removal efficiency of Escherichia coli in six cycles.

Zhao et al. Prepared UiO-66 polymer films by visible-light-mediated Dopamine (DA) co-deposition^[117]. Under the irradiation of light, a large number of ROS are produced, which can induce the polymerization of DA to form the structure of the membrane. At the same time, in order to improve the response ability of the membrane material to light, they also introduced (Rose bengal, RB) photosensitizer to make the membrane material produce more ¹O₂, and the inhibition performance on Escherichia coli and Staphylococcus aureus was significantly enhanced, as shown in Fig. 8 (d).

Wei et al. Loaded PCN-224 and Ag-NPs on Knitted carbon textile (KCT) in situ, and explored the removal performance of Escherichia coli and Staphylococcus aureus under visible light irradiation^[118]. The results showed that the composite was able to remove 6 log and 4.49 log of E. Coli and S. Aureus, respectively, within 30 min (initial concentration of 10⁸CFU·mL^-1). The mechanism of sterilization is mainly the synergistic effect of the ¹O₂ produced by the excited triplet state of PCN-224 and the heat produced by Ag NPs through the LSPR effect. In addition, ¹O₂ is also able to dissociate Ag NPs into Ag⁺ to exert a triple antibacterial effect, as shown in Fig. 9 (a). The fabric has good stability and can still remove 6 log of Escherichia coli after 10 cycles of cleaning.

Xie et al. Loaded Poly (ε-caprolactone) (PCL) with UiO-66 and MOF-535, respectively, using the pressure drop coating method^[119]. In the preparation process, benzoic acid is used to partially replace the ligand to create a certain number of defects, which strengthens the coordination between the metal cluster in the MOF and the carbonyl in the PCL, regulates the interfacial properties, and thus improves the force between the PCL and the MOF. The material can inhibit E. coli within 30 min under LED visible light (Fig. 9 (B)), in which ¹O₂ is the main active substance. The mixed matrix membrane can maintain stable sterilization performance in three cycles and has good stability.

3 Conclusion and prospect

At present, the use of MOFs-based materials for sterilization is limited to the use of Escherichia coli and Staphylococcus aureus as target bacteria, and there are few studies on fungi and protozoa^[120]. The rise of antibiotic-resistant pathogens is also a concern, but so far there has been little work on these organisms^[120]. It is necessary to increase the species of target bacteria because different species of microorganisms are sensitive to the same antibacterial material to different degrees. In addition, the precise molecular mechanism of bacteriostasis needs to be further improved and supplemented. By comparing the responses of parental strains and their knockout mutants, the key genes determining the inactivation efficiency can be identified^[120]. In the future, we can try to combine this method to discuss the mechanism of bacteriostasis in depth. Moreover, there is no uniform standard for the experiment of advanced oxidation sterilization. The reaction conditions (such as catalyst dosage, initial concentration of microorganisms, light source, oxidant dosage, temperature and pH of the reaction system) and the species and survival state of microorganisms in different works are quite different, so it is difficult to compare multiple works horizontally^[121]. In the future, relatively unified evaluation criteria for measuring the antibacterial performance and biological toxicity of MOFs-based materials should be developed. For example, the standard strain and culture conditions used in the experiment, the composition and type of the unified culture medium, and the comprehensive weighted analysis of various bacteriostatic experiments (plate culture method, inhibition zone method, fluorescence chromogenic method, minimum inhibitory concentration method and minimum bactericidal concentration method) by using the analytic hierarchy process to calculate the comprehensive index of the bacteriostatic performance of the material. Finally, it is necessary to consider the migration and transformation of nanomaterials in the environment and the biological toxicity in vivo to evaluate the application potential of nanomaterials in the field of environmental remediation and medical treatment^[122,123].

The potential application fields of MOFs antibacterial materials in the future are (1) water treatment: MOFs with antibacterial properties are prepared into membrane modules, which can prevent the occurrence of biofilm formation in the process of water treatment due to their excellent antibacterial ability, and contribute to the maintenance of membrane flux^[25]. In particular, the development of adsorption/catalytic multifunctional membranes with antibacterial properties is of great significance for deep water purification and seawater desalination projects^[124]. For example, Zhou et al. Prepared MIL-125 (Ti) @ PVDF catalytic films with antibacterial ability by a simple phase inversion method^[125]. The composite membrane material has an inhibition effect on Escherichia coli while catalyzing and degrading rhodamine B organic pollutants under visible light, and can effectively prevent membrane pollution caused by microorganisms. Ma et al. Grown zinc metal-azole framework material MAF-4 (ZIF-8) on Polyethersulfone (PES) substrate by in-situ crystallization method, and then prepared defect-free MAF-7 shell on MAF-4 by epitaxial growth^[126]. The MAF-7 @ 4/PES composite membrane has strong antifouling ability, and the water flux of the membrane only decreases by 22. 4% in 60 min in the presence of Bovine serum albumin (BSA). Therefore, the hybrid membrane material can be used as a catalytic membrane with self-purification function. (2) Medical and health field: MOFs with antibacterial properties can not only be prepared into coatings for medical devices, protective clothing and packaging materials, but also be prepared into dressings for adjuvant treatment of wound healing in vitro^{[105,107,127]}^[102]. In addition, MOFs can also be used to prepare targeted drugs through their own antibacterial properties or their porous drug loading, which can trigger desorption and release drugs under special conditions, so as to carry out precise treatment of targets (such as tumors)^[128,129]. (3) Personal daily necessities: MOFs-based antibacterial materials can also be prepared into antibacterial coatings for daily use (such as stationery, contact lenses, masks, indoor walls, etc.) To improve the quality of life. For example, Wang et Al. coated Al-based MOF and V (IV) -based MOF (BIT-66) on commercial non-woven fabrics and blended with commercial ethylene-vinyl acetate copolymer respectively to prepare coatings that can be covered on indoor walls. These two coatings can play a role in photocatalytic sterilization under indoor light conditions, which can reduce indoor bioaerosol pollution and control air humidity^[130,131]. At the same time, Wang et al. Also loaded ZIF-8 as a coating in the mask, which can effectively intercept microorganisms in the air under simulated sunlight^[103].

In recent years, iron-based MOFs have been favored by researchers because of their relatively simple synthesis methods and relatively weak biological toxicity of iron ions^[37]. Although the antibacterial performance of iron ion itself is relatively weak, most iron-based MOFs can be excited by visible light because of their abundant Fe-O clusters, thus producing active substances with oxidative sterilization performance, so they can be used for visible light-induced advanced oxidation sterilization^[132]. Meanwhile, iron-based MOFs have been largely applied to activated persulfate advanced oxidation (SR-AOP) for degradation of organic pollutants^[133,134]. Therefore, the sterilization performance of iron-based MOFs through SR-AOP pathway should be widely explored in the future, which will help to promote the application of low-cost and environmentally friendly MOFs-based materials in water treatment of self-cleaning catalytic membrane materials.

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Funding

National Natural Science Foundation of China(22176012)

Beijing Natural Science Foundation(8202016)

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1 Introduction

2 MOFs-based materials for advanced oxidation sterilization

2.1 Single MOFs

2.2 Photosensitized MOFs.

2.3 MOFs photoelectrode

2.4 MOFs heterojunction

2.5 MOFs derivatives

2.6 MOFs-based macroscopic materials.

3 Conclusion and prospect

References

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