A method for in-situ vulcanization of electrodeposited preparation of Pd / Ni3S2 / NF nanosheet array electrode and a method for EHDC

Abstract

The application discloses a method for preparing a Pd / Ni3S2 / NF nanosheet array electrode by in-situ sulfuration electrodeposition. It is known that designing an electrode loaded with a high-efficiency electrocatalyst is a key to chlorophenol (CP) electrocatalytic hydrogen dechlorination (EHDC) and is still challenging. The application adopts an in-situ sulfuration electrodeposition strategy to prepare a novel three-dimensional network structure Pd / Ni3S2 / NF nanosheet array electrode, so as to realize stable EHDC. The EHDC performance of the prepared Pd / Ni3S2 / NF electrode is tested by taking 2-CP as a model pollutant. Complete dechlorination is completed within 240 min. The improvement of the EHDC performance can be attributed to the Ni3S2 nanosheet and Pd nanoparticle, the Ni3S2 replaces Pd0 to generate atomic hydrogen (H ads ), and promotes more Pd 2+ generation, which is beneficial to the rupture of C-Cl bond, so as to improve the mass activity of Pd and the EHDC performance. The research provides a simple and practical strategy for designing a low noble metal loaded catalyst with high EHDC performance.

Description

Technical Field

[0001] This invention belongs to the field of environmental protection technology, specifically relating to a method for preparing Pd / Ni3S2 / NF nanosheet array electrodes by in-situ sulfide electrodeposition and a method for using the electrode for electrocatalytic hydrogenation dechlorination, which can remove chlorophenols. Background Technology

[0002] Chlorophenols (CPs), as common industrial raw materials, are widely used in electronics, dyes, pesticides, papermaking, and pharmaceuticals. They are persistent organic pollutants, difficult to degrade, bioaccumulating, teratogenic, carcinogenic, and mutagenic, posing a significant threat to animals, plants, and the natural environment. Various CPs have been listed as priority pollutants by many countries. Therefore, technologies that can effectively and environmentally remove them are highly desirable. Electrocatalytic hydrogen dechlorination (EHDC) offers advantages such as high efficiency, safety, reactivity, and no secondary pollution, making it a promising dechlorination technology. In EHDC, a large amount of atomic hydrogen (H+) is generated in situ through the electrolysis of water in the cathode aqueous solution. ads ), acting as a reducing agent, attacks and breaks C-Cl bonds, thereby reducing or even eliminating the toxicity of chlorophenols. Therefore, H on the catalyst surface ads Rapid species formation is a key step in EDCH.

[0003] Palladium (Pd) is an excellent EHDC catalyst that can produce H+ over a wide pH range. ads Palladium exhibits good stability. However, due to its high price and low reserves, it is difficult to use for large-scale wastewater treatment. To overcome this problem and reduce the cost of EHDC, it is necessary to improve the mass activity of palladium. In recent years, some researchers have improved the efficiency of EHDC by optimizing or modifying the electrode substrate. Cheng reported the first Pd / Ti mesh electrode for removing 2,4-DCP. Subsequently, various foam electrodes, such as Pd-Ni and Pd-Ti foam electrodes, have been invented. These foam electrodes have a self-supporting three-dimensional porous structure, which promotes the diffusion of contaminants and improves the efficiency of EHDC. However, due to the small synergistic effect between Pd and the substrate, the activity of Pd is often improved by increasing the Pd loading, which results in no improvement in the mass activity of palladium in these electrodes. Summary of the Invention

[0004] Electrocatalytic hydrogen dechlorination (EHDC) exhibits promising performance, but the quality and activity of existing catalysts require further improvement. Compared to conductive polymers and other transition metal oxides, transition metal sulfides demonstrate higher HER performance and lower adsorption energy in alkaline solutions. Furthermore, they offer advantages such as simple preparation, low cost, high conductivity, and large specific surface area. Therefore, modifying Pd-Ni foam electrodes with transition metal sulfides can effectively improve the electrode's hydrogen production efficiency, enhance the quality and activity of Pd, and reduce the dechlorination cost of EHDC. This invention introduces an intermediate layer with high HER performance into the Pd / Ni foam electrode, which can improve the hydrogen production efficiency of the electrode. ads The generation of Pd, and even its replacement. 0 Generate H ads This can effectively improve the quality activity of Pd and reduce the amount of Pd required.

[0005] The present invention adopts the following technical solution:

[0006] A method for preparing Pd / Ni3S2 / NF nanosheet array electrodes by in-situ sulfide electrodeposition involves reacting nickel foam and a sulfur source compound to obtain sulfur-loaded nickel foam; then depositing palladium on the sulfur-loaded nickel foam to obtain the Pd / Ni3S2 / NF nanosheet array electrode.

[0007] A method for removing organochlorine pollutants employs a three-electrode system, using the aforementioned Pd / Ni3S2 / NF nanosheet array electrode as the working electrode to electrochemically reduce the organochlorine pollutants, thereby completing the removal of the organochlorine pollutants.

[0008] In this invention, the sulfur source compound includes thiourea; the reaction temperature is 120–160°C and the reaction time is 3–6 hours, preferably 140–160°C and the reaction time is 4–6 hours.

[0009] In this invention, electrodeposition is performed using pulsed electrodeposition to decorate Ni3S2 / NF with Pd, resulting in Pd / Ni3S2 / NF. During electrodeposition, the plating solution is a sodium chloride solution containing palladium salt, which can be Na2PdCl4. The Pd loading in the Pd / Ni3S2 / NF nanosheets is 0.4–2.5 mg cm⁻¹. −2 Preferably 0.5–2 mg cm −2 More preferably, it is 0.7–1.4 mg cm. −2 .

[0010] This invention discloses the application of the Pd / Ni3S2 / NF nanosheet array electrode prepared by the above-mentioned in-situ sulfide electrodeposition in electrocatalytic hydrodechlorination; it also discloses the application of the above-mentioned electrode in the removal of organochlorine pollutants; and especially in the electrocatalytic hydrodechlorination treatment of chlorophenols.

[0011] This invention presents a novel Pd / Ni3S2 / NF nanosheet array electrode prepared via an in-situ sulfidation strategy, which can accelerate the formation of EHDC. ads To improve the mass activity of Pd, the effects of operating conditions (pH, coexisting ions, and contaminant concentrations) on the EHDC performance of the Pd / Ni3S2 / NF electrode were investigated. This invention synthesizes a Pd / Ni3S2 / NF nanosheet array electrode with excellent EHDC performance using an in-situ sulfide electrodeposition method. This electrode possesses a self-supporting three-dimensional network structure, which improves the dispersibility of palladium nanoparticles and effectively reduces their particle size. The Pd / Ni3S2 / NF electrode exhibits good EHDC performance: 2-CP dechlorination can be achieved within 240 min. Attached Figure Description

[0012] Figure 1 SEM images of (a) NF, (b) Ni3S2 / NF, (c) Pd / Ni3S2 / NF and (d) Pd / NF; elemental mapping images of (e, f and g) Pd / Ni3S2 / NF.

[0013] Figure 2 TEM images of (a) Ni3S2 / NF and (b) Pd / Ni3S2 / NF.

[0014] Figure 3 XRD images of (a) Pd / Ni3S2 / NF, Ni3S2 / NF, and Pd / NF; (b) Ni3S2 / NF of Pd / Ni3S2 / NF. 3+ XPS images of Pd / Ni3S2 / NF and Pd / NF in Pd 3d; (c) XPS images of Pd / Ni3S2 / NF and Pd / NF in S2p.

[0015] Figure 4 The study aimed to evaluate the EHDC performance of (a) Pd / Ni3S2 / NF at different voltages; (b) the EHDC degradation rate of Pd / Ni3S2 / NF at different voltages; (c) the EHDC performance of NF, Pd-NF, Ni3S2 / NF, and Pd / Ni3S2 / NF at -0.8V; and (d) the degradation rate of NF, Pd-NF, Ni3S2 / NF, and Pd / Ni3S2 / NF at -0.8V. The Pd loading was 0.83 mg / cm³. −2 .

[0016] Figure 5 (a) Durability test of Pd / Ni3S2 / NF catalyst in EHDC reaction; (b) CV curves of fresh Pd / Ni3S2 / NF and Pd / Ni3S2 / NF after use; Pd loading: 0.83 mg cm⁻¹−2 .

[0017] Figure 6 The following are examples of EHDC performance of Pd / Ni3S2 / NF at different Pd loadings: (a) Pd / Ni3S2 / NF at different initial pollutant concentrations; (b) Pd / Ni3S2 / NF at different pH values; (c) Pd / Ni3S2 / NF in the presence of 10 mM coexisting ions; Pd loading in b, c, and d is 0.83 mg / cm³. −2 .

[0018] Figure 7 The EHDC performance of Pd / Ni3S2 / NF in 2 mg soil was evaluated; the Pd loading was 0.83 mg cm⁻¹. −2 . Detailed Implementation

[0019] This invention presents a novel Pd / Ni3S2 / NF nanosheet array electrode prepared via an in-situ sulfidation strategy, which can accelerate the formation of EHDC. ads To improve the mass activity of Pd, the effects of working conditions (pH, coexisting ions and contaminant concentration) on the EHDC performance of the Pd / Ni3S2 / NF electrode were investigated.

[0020] The raw materials used in this invention are all commercially available products, and the specific preparation and testing methods are conventional techniques. Thiourea was purchased from Shanghai Lingfeng Chemical Reagent Co., Ltd., and sodium tetrachloropalladium was purchased from TCI (Shanghai) Chemical Industry Development Co., Ltd. All reagents were used directly without further purification. Nickel foam was purchased from Suzhou Suke Precision Instrument Co., Ltd. A 1cm×3cm×1mm piece of nickel foam was ultrasonically treated with acetone, 3M hydrochloric acid, ethanol, and deionized water in sequence to remove surface impurities.

[0021] Example 1: Preparation of Pd / Ni3S2 / NF

[0022] The cleaned nickel foam was placed in a 15 mL polytetrafluoroethylene-lined high-pressure reactor containing 1 mg thiourea and 10 mL deionized water. The reactor was sealed and reacted at 150 °C for 5 h. After cooling to room temperature, the resulting material was removed and rinsed with water to obtain Ni3S2 / NF. Subsequently, Pd / Ni3S2 / NF was obtained by pulse electrodeposition on the prepared Ni3S2 / NF, with 5000 cycles at a high potential of 0 V and a low potential of −1.5 V (vs. Hg / Hg2Cl2) (pulse width = 0.2 s). The electroplating solution was a 30 mL Na2PdCl4 aqueous solution containing 0.5, 1, 1.5, and 2 mM Na2PdCl4, respectively. ICP-MS detected almost no Pd in ​​the residual solution, corresponding to Pd loadings of 0.42, 0.83, 1.32, and 1.8 mg cm⁻¹, respectively. −2 .

[0023] Based on the above method, palladium was directly pulsed electrodeposited on the cleaned nickel foam to obtain Pd-NF. The electroplating solution was 30 mL Na2PdCl4 solution containing 1 mM Na2PdCl4. ICP-MS detected almost no Pd in ​​the residual solution.

[0024] Materials characterization. Scanning electron microscopy (SEM) images were obtained using a Regulus 8230 instrument operating at 15 kV. Transmission electron microscopy (TEM) images were obtained using a FEI Tecnai G2F20 microscope equipped with a field emission gun operating at 120 kV. X-ray diffraction (XRD) characterization was performed on an X'Pert-pro MPD diffractometer (PAN Analysis, Netherlands). Cu Kα radiation was used in the 2θ range from 5° to 80°. Surface composition and valence states were analyzed by X-ray photoelectron spectroscopy (XPS, Thermo Scientific EXCALAB 250 XI) with 300 W Al Kα radiation. Palladium loading on the catalyst was analyzed by inductively coupled plasma mass spectrometry (ICP-MS, iCAP™ Qc).

[0025] Pd / Ni3S2 / NF was prepared via a simple two-step method. First, an array of Ni3S2 nanosheets was grown in situ on nickel foam using a hydrothermal method. Then, Pd / Ni3S2 / NF was obtained through one-step electrodeposition. As shown in Figure 1a, the initial nickel foam substrate had a smooth surface. Figure 1 Figure b shows the Ni3S2 / NF obtained by sulfidation, indicating that the Ni3S2 nanosheet array is uniformly and densely grown on nickel foam. Figure 1Image c shows the further electrodeposition of Pd nanoparticles on Ni3S2 / NF. The nanosheets become rough, and palladium nanoparticles are uniformly loaded on the surface. Elemental mapping image ( Figure 1 (e, 1f, and 1g) confirmed the uniform distribution of NiS nanosheets and Pd nanoparticles on nickel foam. Transmission electron microscopy was used to observe the Ni3S2 / NF and Pd / Ni3S2 / NF samples. Figure 2 (a) shows a nanosheet structure, similar to Figure 1 (b) The SEM images of Ni3S2 / NF shown are consistent. Transmission electron microscopy images of Ni3S2 nanosheets loaded with Pd nanoparticles are shown below. Figure 2 As shown in b, after electrodeposition, Pd nanoparticles are uniformly dispersed on the Ni3S2 / NF surface, with an average diameter of approximately 20 nm.

[0026] XRD analysis was used to obtain information on the crystal structure and phase composition of the sample. Figure 3 a represents the XRD patterns of Pd / NF, Ni3S2 / NF, and Pd / Ni3S2 / NF. The XRD diffraction peaks of Pd / Ni3S2 / NF and Ni3S2 / NF show that the diffraction peaks at 2θ angles of 21.7°, 31.3°, 37.7°, 38.2°, 44.3°, 49.7°, 50.1°, 54.6°, 55.1°, and 55.3° correspond to the (101), (110), (202), (113), (211), (104), (122), and (300) crystal planes of hexagonal Ni3S2 (PDF#44-1418). Meanwhile, in... Figure 3 In the magnified image of a, obvious diffraction peaks can be observed at 37.7° and 38.2° for both the Pd / Ni3S2 / NF and Ni3S2 / NF electrodes, corresponding to the characteristic peaks of the Ni3S2 (003) and (021) surfaces, respectively, indicating that Ni3S2 / NF was successfully loaded onto nickel foam. Furthermore, obvious diffraction peaks can be observed at 40.1°, 46.6°, and 68.1° for both the Pd / Ni3S2 / NF and Pd / NF electrodes, corresponding to the characteristic peaks of the Pd (111), (200), and (220) surfaces (PDF#46-1043), confirming the successful bonding of Pd nanoparticles with Ni3S2 nanosheets, consistent with the SEM and TEM results.

[0027] XPS was used to characterize the surface composition and elemental valence states of Pd / Ni3S2 / NF, Ni3S2 / NF and Pd / NF electrodes. Figure 3 b is the XPS image of Ni 2p in Pd / Ni3S2 / NF, with peaks at 873.3 and 855.5 eV belonging to Ni, respectively. 3+ 2p 1 / 2 and 2p 3 / 2 . Figure 3 c represents the high-resolution XPS spectra of Pd3d in Pd / Ni3S2 / NF and Pd / NF. The main peaks of the Pd-NF electrode at binding energies of 335.39 and 340.67 eV correspond to Pd3d, respectively. 0 3D 5 / 2 and 3D 3 / 2 The peaks at 336.86 and 342.34 eV correspond to Pd, respectively. 2+ 3D 5 / 2 and 3D 3 / 2 The peaks of the Pd / Ni3S2 / NF electrode at binding energies of 335.41 and 340.86 eV correspond to Pd, respectively. 0 3D 5 / 2 and 3D 3 / 2 The peaks at 337.24 and 342.57 eV correspond to Pd, respectively. 2+ 3D 5 / 2 and 3D 3 / 2 It is noteworthy that the Pd binding energy of Pd / Ni3S2 / NF undergoes a positive shift relative to Pd / NF, which may be due to the transfer of electrons from Pd to S. Furthermore, the Pd binding energy of Pd / Ni3S2 / NF... 2+ and Pd 0 Peak area ratio S Pd 2+ / S Pd 0 The value is 3.06, higher than Pd / NF's 0.45, indicating that the introduction of Ni3S2 is beneficial to Pd. 2+ The formation of. Figure 3 d represents the high-resolution XPS spectrum of S. The peaks of Ni3S2 / NF at 162.87 and 164.62 eV belong to S 2p, respectively. 3 / 2 and 2p 1 / 2 The peak at 168.15 eV belongs to sulfate species produced by oxidation on the electrode surface. After Pd is deposited on the Ni3S2 surface, S2p... 3 / 2 and 2p 1 / 2 The peaks shifted negatively by 0.59 and 0.9 eV, respectively, indicating that electrons transferred from the Pd portion to S, meaning that a Pd-S bond was formed between Pd and S.

[0028] Example 2

[0029] Electrocatalytic testing. All electrochemical measurements were performed at room temperature using a CHI760E electrochemical workstation. A basic three-electrode battery system was assembled using a platinum foil (2 × 2 cm) counter electrode, an Ag / AgCl reference electrode, and a sample (Pd / Ni3S2 / NF, i.e., catalyst) as the working electrode. Hydrodechlorination experiments of 2-CP were conducted in an H-type battery (100 mL). To prevent the generation of chlorine gas from Cl- at the anode, a Nafion 117 cation exchange membrane was used to separate the cathode and anode chambers. 50 mL of 50 mmol / L Na2SO4 aqueous solution was added to both the cathode and anode chambers as electrolytes. Additionally, 5 mg of 2-CP was added to the cathode chamber, with a 2-chlorophenol concentration of 100 ppm. Electrochemical reduction of 2-CP was performed using a potentiostatic method, with each degradation experiment lasting 4 hours under magnetic stirring. The results were obtained at 5 mV s⁻¹. -1 The linear sweep voltammetry (LSV) polarization curves were obtained at a scan rate of 50 mV / s. -1 The cyclic voltammetry (CV) curve was obtained.

[0030] Based on the above experiments, different catalysts were used as working electrodes to obtain the EHDC performance of different electrodes; based on the above experiments, catalysts with different palladium loadings were used as working electrodes to obtain the EHDC performance of Pd / Ni3S2 / NF under different Pd loadings; based on the above experiments, different amounts of 2-chlorophenol were added to obtain the EHDC performance of Pd / Ni3S2 / NF under different initial pollutant concentrations; based on the above experiments, the pH of the cathode electrolyte was adjusted using H3PO4-NaH2PO4, NaH2PO4-Na2HPO4, or Na2HPO4-Na3PO4 systems to obtain the EHDC performance of Pd / Ni3S2 / NF at different pH values; based on the above experiments, interfering ions were added to the cathode chamber to obtain the EHDC performance of Pd / Ni3S2 / NF in the presence of 10 mM coexisting ions.

[0031] Analytical methods. The concentration of 2-chlorophenol was determined using high-performance liquid chromatography (HPLC, Agilent, 1260). Experimental conditions were as follows: reversed-phase column C18 (2.7 μm, 4.6 × 100 mm), column temperature 30 °C; flow rate 1 mL / min. -1 The mobile phase consisted of 60% methanol and 40% water (volume ratio); the injection volume was 20 μL; and the UV-Vis detector wavelength was 278 nm.

[0032] Using 2-CP (2-chlorophenol) as a model pollutant, the EHDC performance of the catalyst was evaluated at a constant potential. To investigate the effect of cathode potential on the catalytic performance of the Pd / Ni3S2 / NF electrode, the EHDC efficiency of 2-CP under different cathode potential conditions was compared. Figure 4 a, Figure 4 Figure b shows the EHDC experimental results of the catalyst degrading 100 ppm of 2-cp at voltages of -0.7, -0.8, -0.85, -0.9, and -1.0 V. As shown in the figure, the relationship between the EHDC performance of 2-CP and voltage is volcano-like, meaning that the EHDC efficiency gradually increases with increasing voltage, reaching the optimal degradation effect at -0.8 V. With increasing cathode potential, the removal efficiency of 2-CP significantly improves, reaching a peak at -0.85 V. After 240 min of reaction, the removal rate of 2-CP approaches 100%. When the potential increases further, the removal efficiency decreases. With increasing cathode potential, the hydrogen evolution reaction (HER) becomes dominant, competing for H₂. ads This leads to a decrease in 2-CP removal efficiency. Simultaneously, the H2 generated by HER also occupies some reactive sites, which reduces the adsorption of 2-CP on the electrode surface. Figure 4 c. Figure 4 Table d shows the EHDC performance of NF, Pd-NF, Ni3S2 / NF, and Pd / Ni3S2 / NF electrodes with 100 ppm 2-CP at a cathode potential of -0.8 V. The results indicate that only Pd-containing electrodes can effectively remove 2-CP. Furthermore, the catalyst prepared in this invention exhibits superior hydrodechlorination performance compared to most similar catalysts (Table 1), maintaining or even improving catalyst performance while reducing the Pd loading.

[0033]

[0034] Electrode stability is a key factor in maintaining 2-CP degradation efficiency and evaluating its practical application value. The stability of the Pd / Ni3S2 / NF electrode was evaluated through repeated degradation of 2-CP at a constant operating potential of -0.8V. Figure 5 As shown in Figure a, the degradation efficiency of 2-CP on the Pd / Ni3S2 / NF electrode remained almost unchanged, and the CV curves before and after five consecutive reactions showed no significant change. Figure 5 (b) indicates that Pd / Ni3S2 / NF has good stability.

[0035] Under the same experimental conditions, the effects of Pd loading, initial contaminant concentration, electrolyte pH, and heteroions on the performance of the EHDC catalyst are shown in [reference needed]. Figure 6 .like Figure 6 As shown in Figure a, when the Pd loading is 0.83 mg cm⁻¹ -2At this time, the EHDC performance of Pd / Ni3S2 / NF reaches its optimal level. Figure 6 b shows the EHDC performance curves of Pd / Ni3S2 / NF at different initial concentrations of 2-CP. As can be seen from the figure, Pd / Ni3S2 / NF exhibits good EHDC performance at different initial concentrations. Figure 6 c shows the EHDC performance curves of Pd / Ni3S2 / NF at different pH values. The catalyst exhibits the best EHDC performance at pH 6.04 and pH 8.44. As the acidity or alkalinity of the solution increases, the performance decreases accordingly. However, under strong acid and strong alkaline conditions (pH 2.7 and 12), the EHDC performance can still reach 71%, indicating that Pd / Ni3S2 / NF can be used in a relatively wide pH range. Figure 6 d represents the EHDC performance curves of Pd / Ni3S2 / NF in the presence of different coexisting ions. The catalyst performance is basically unaffected by the presence of chloride, sulfate, carbonate and bicarbonate ions. Sodium chloride, sodium sulfite, sodium carbonate, sodium bicarbonate and sodium sulfide were used as heteroion sources, respectively.

[0036] Example 3

[0037] To explore the practical application of Pd / Ni3S2 / NF, the EHDC performance of the catalyst under soil conditions was simulated. 2 mg of commercially available clean soil was added to the cathode chamber of the system in Example 2 to simulate the EHDC performance under soil conditions. Figure 7 The results showed that the dechlorination rate of Pd / Ni3S2 / NF in soil mud could still reach 69%.

[0038] In conclusion, this invention synthesizes a Pd / Ni3S2 / NF nanosheet array electrode with excellent EHDC performance using an in-situ sulfide electrodeposition method. This electrode possesses a self-supporting three-dimensional network structure, which improves the dispersibility of palladium nanoparticles and effectively reduces their particle size. The Pd / Ni3S2 / NF electrode exhibits good EHDC performance. 2-CP dechlorination can be achieved within 240 min. The Pd / Ni3S2 / NF nanosheet electrode disclosed in this invention has a three-dimensional structure, increasing the electrochemical active area of ​​the electrode, accelerating the diffusion of reactants and products, and improving the utilization rate of active sites. The synergistic effect of Ni3S2 nanosheets and Pd nanoparticles allows Ni3S2 to partially replace Pd. 0 Generate H ads Promote more Pd 2+ The formation of [a specific chemical compound] promotes the breaking of C-Cl bonds, thereby improving the mass activity of Pd and the performance of EHDC. This study provides a simple and practical strategy for obtaining high-efficiency EHDC electrocatalysts with low cost and low noble metal requirements.

Claims

1. A method for removing organochlorine pollutants using a three-electrode system, characterized in that, Comprising the following steps: (1) reacting the nickel foam with thiourea to obtain the sulfur-loaded nickel foam; then depositing palladium on the sulfur-loaded nickel foam to obtain the Pd / Ni3S2 / NF nanosheet array electrode; the reaction temperature is 150°C, and the reaction time is 5 hours; in the Pd / Ni3S2 / NF nanosheet, the loading of Pd is 0.83 mg cm −2 ; Deposition is pulse electrodeposition, 5000 cycles, high potential is 0V, low potential is-1.5V, pulse width=0.2s; (2) The Pd / Ni3S2 / NF nanosheet array electrode is used as a working electrode to electrochemically reduce organic chlorine pollutants, thereby removing the organic chlorine pollutants; The organic chlorine pollutants are 2-chlorophenol or 4-chlorophenol.

2. The method of removing organochlorine contaminants according to claim 1, wherein, The deposition is pulse electrodeposition; during electrodeposition, the electroplating solution is a sodium chloride solution containing a palladium salt.

3. Use of a Pd / Ni3S2 / NF nanosheet array electrode in the removal of organochlorine pollutants, characterized in that, reacting the nickel foam with thiourea to obtain a sulfur-loaded nickel foam; then depositing palladium on the sulfur-loaded nickel foam to obtain a Pd / Ni3S2 / NF nanosheet array electrode; the reaction temperature is 150°C, and the reaction time is 5 hours; in the Pd / Ni3S2 / NF nanosheet, the loading of Pd is 0.83 mg cm −2 ; using the Pd / Ni3S2 / NF nanosheet array electrode as a working electrode, electrochemically reducing an organic chlorine contaminant to remove the organic chlorine contaminant; the deposition is pulse electrodeposition, 5000 cycles, a high potential of 0 V, a low potential of -1.5 V, and a pulse width of 0.2 s; the organic chlorine contaminant is 2-chlorophenol or 4-chlorophenol.

Images