A montmorillonite-loaded zero-valent nano-iron electrode material and its preparation method and application

Abstract

A montmorillonite-loaded zero-valent nano-iron electrode material, its preparation method, and application, pertain to the field of material preparation. The preparation method comprises: dropwise adding a reducing agent solution to a mixed solution containing an iron source and a montmorillonite carrier to react, thereby obtaining the montmorillonite-loaded zero-valent nano-iron material. In the mixed solution, the iron source and the montmorillonite carrier are used in a ratio of 0.0005 to 0.004 mol / g, wherein the iron source is measured as a molar amount of divalent iron ions and the montmorillonite carrier is measured as a mass. The obtained montmorillonite-loaded zero-valent nano-iron material, a binder, and water are mixed to obtain a clay-like solid. The clay-like solid is then granulated and calcined to obtain a granular montmorillonite-loaded zero-valent nano-iron electrode material. When used as a granular electrode in a three-dimensional electrode system, the montmorillonite-loaded zero-valent nano-iron electrode material exhibits an ideal removal effect on organic matter while significantly reducing iron ion leaching.

Description

Technical Field

[0001] The present invention relates to the technical field of material preparation, and in particular to a montmorillonite-loaded zero-valent nano-iron electrode material and a preparation method and application thereof. Background Art

[0002] Electrochemical catalytic oxidation technology has the advantages of high efficiency in in-situ generation of oxidizing species, small footprint, easy operation and management, and has become a potential treatment solution for effectively removing organic pollutants from wastewater.

[0003] Nano-zero-valent iron (nZVI) is a metal material with high catalytic activity, low cost and easy availability. Compared with metals such as Pd and Ag, it has considerable economic benefits. Composite materials loaded with nano-zero-valent iron are often used as electrodes in electrochemical catalytic oxidation systems.

[0004] In existing technologies, nano-zero-valent iron-loaded composite materials are typically used as cathodes and are relatively effective in removing organic pollutants. However, the high amount of iron ions leached into the solution after the reaction makes secondary pollution a major limitation in the application and development of this technology. Summary of the Invention

[0005] (1) Purpose of the invention

[0006] The present invention provides a montmorillonite-loaded zero-valent nano-iron electrode material, a preparation method and an application thereof. When the montmorillonite-loaded zero-valent nano-iron electrode material is used as a particle electrode in a three-dimensional electrode system, it not only has an ideal removal effect on organic matter, but also can greatly reduce the amount of iron ion leaching. (2) Summary of the invention

[0008] In one aspect, the present invention provides a method for preparing a montmorillonite-loaded zero-valent nano-iron electrode material, comprising:

[0009] A reducing agent solution is added dropwise to a mixed solution containing an iron source and a montmorillonite carrier to react to obtain a montmorillonite-supported zero-valent nano-iron material, wherein the ratio of the iron source to the montmorillonite carrier in the mixed solution is 0.0005 to 0.004 mol / g, wherein the iron source is calculated as a molar amount of divalent iron ions and the montmorillonite carrier is calculated as a mass amount;

[0010] The obtained montmorillonite-loaded zero-valent nano-iron material, a binder, and water are mixed to obtain a clay-like solid;

[0011] The clay-like solid is granulated and calcined to obtain a granular montmorillonite-loaded zero-valent nano-iron electrode material.

[0012] Preferably, the montmorillonite carrier is montmorillonite doped with biochar, and the mass content of the biochar in the montmorillonite carrier is 3 to 20%.

[0013] Preferably, the mass content of the biochar in the montmorillonite carrier is 3-7%.

[0014] Specifically, the iron source is selected from at least one of FeSO4, FeCl2, and Fe(NO3)2;

[0015] The concentration of the iron source in the mixed solution is 0.004 to 0.035 mol / L based on the molar amount of iron ions;

[0016] The reducing agent is selected from at least one of NaBH4 and KBH4;

[0017] In terms of molar amount, the amount of the reducing agent is 3.5 to 4 times that of the iron source.

[0018] Specifically, the specific conditions of the reaction include:

[0019] Carry out under inert atmosphere and stirring conditions;

[0020] The reaction temperature is room temperature;

[0021] The reaction time is 0.5 to 1 hour.

[0022] Specifically, the binder is selected from at least one of pseudo-boehmite, magnesium phosphate, and aluminum phosphate;

[0023] The binder accounts for 9-17% of the total mass of the binder and the montmorillonite-loaded zero-valent nano-iron material.

[0024] Specifically, the specific conditions of the calcination include:

[0025] Calcination temperature is 400-450°C;

[0026] The calcination time is 2.5 to 3 hours.

[0027] In another aspect, the present invention provides a montmorillonite-loaded zero-valent nano-iron electrode material prepared by any of the above-mentioned preparation methods.

[0028] In another aspect, the present invention provides the use of the montmorillonite-loaded zero-valent nano-iron electrode material prepared by any of the preparation methods described above in the field of electrochemical catalytic oxidation of organic compounds.

[0029] Specifically, the montmorillonite-loaded zero-valent nano-iron electrode material is used as a particle electrode in a three-dimensional electrode.

[0030] (3) Beneficial effects

[0031] The above technical solution of the present invention has the following beneficial technical effects:

[0032] The present invention provides a montmorillonite-loaded zero-valent nano-iron electrode material, a preparation method thereof, and an application thereof. By using montmorillonite to load nano-zero-valent iron and controlling the loading amount of the nano-zero-valent iron, the prepared montmorillonite-loaded zero-valent nano-iron electrode material, when used as a three-dimensional electrode particle electrode, can ensure a good organic matter removal rate and greatly reduce the amount of iron ion leaching, thereby avoiding the problem of secondary pollution easily generated by the nano-zero-valent iron electrode material and being green and friendly to the environment.

[0033] By doping the montmorillonite with a certain proportion of biochar, the nano-zero-valent iron is evenly distributed between the carrier layers, along its edges, and on its surface. It also exhibits excellent mechanical strength, excellent acid and alkali resistance, and a high oxygen evolution overpotential. Furthermore, the addition of biochar and the nano-zero-valent iron loading accelerate the electron mass transfer efficiency of the particle electrode in the three-dimensional electrode system, reducing the charge and discharge resistance of the solution and facilitating the oxidative degradation of pollutants during the reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 X-ray diffraction patterns of montmorillonite and MMT(5%C) / nZVI (powder) provided in Example 1;

[0035] Figure 2 This is an electron microscope image of montmorillonite;

[0036] Figure 3 The electron micrograph of MMT (5% C) / nZVI (powder) provided in Example 1;

[0037] Figure 4 This is an electron micrograph of the material provided in step 1 of Example 4;

[0038] Figure 5 Cyclic voltammetry scanning curves of two-dimensional electrode system and three-dimensional electrode system;

[0039] Figure 6 Fitting curves of different scan rates and peak current for cyclic voltammetry tests of two-dimensional electrode system and three-dimensional electrode system;

[0040] Figure 7 Comparison of electron transfer rates in a two-dimensional electrode system and a three-dimensional electrode system constructed using the electrode materials provided in Examples 1 to 25;

[0041] Figure 8 Comparison diagram of the fitted charge and discharge resistance in the three-dimensional electrode systems constructed using the electrode materials provided in Examples 1 to 25, respectively;

[0042] Figure 9 A comparison of the removal effects of ciprofloxacin in wastewater by electrode systems constructed with MMT / nZVI / GF and MMT(5%C) / nZVI materials respectively;

[0043] Figure 10 This is a comparison chart of the amount of iron ion leaching in the solution after the reaction of the electrode system constructed with MMT / nZVI / GF and MMT (5% C) / nZVI materials as electrodes. DETAILED DESCRIPTION

[0044] To make the objectives, technical solutions, and advantages of the present invention more clearly understood, the present invention will be further described in detail below in conjunction with specific embodiments and with reference to the accompanying drawings. It should be understood that these descriptions are merely exemplary and are not intended to limit the scope of the present invention. In addition, in the following description, descriptions of well-known structures and technologies are omitted to avoid unnecessary confusion of the concepts of the present invention.

[0045] An embodiment of the present invention provides a method for preparing a montmorillonite-loaded zero-valent nano-iron electrode material, comprising:

[0046] Step 1: Adding a reducing agent solution dropwise to a mixed solution containing an iron source and a montmorillonite carrier to react to obtain a montmorillonite-supported zero-valent nano-iron material, wherein the ratio of the iron source to the montmorillonite carrier in the mixed solution is 0.0005 to 0.004 mol / g, wherein the iron source is calculated as a molar amount of divalent iron ions and the montmorillonite carrier is calculated as a mass amount;

[0047] Step 2: mixing the obtained montmorillonite-loaded zero-valent nano-iron material, a binder, and water to obtain a clay-like solid;

[0048] Step 3: Granulate and calcine the clay-like solid to obtain granular montmorillonite-loaded zero-valent nano-iron electrode material.

[0049] Specifically, in step 2, based on the total mass of the montmorillonite-loaded zero-valent nano-iron material, the binder, and water, the amount of water used is preferably 19-25% wt;

[0050] Specifically, before granulation in step 3, mud kneading and layering are performed, wherein the mud kneading time is preferably 8 to 15 minutes;

[0051] Specifically, the montmorillonite carrier is montmorillonite doped with biochar, and the mass content of the biochar in the montmorillonite carrier is 3 to 20%; preferably, the mass content of the biochar in the montmorillonite carrier is 3 to 7%, so as to ensure that when the obtained material is used as a granular electrode, the removal effect of ciprofloxacin can reach more than 90%, and the iron ion leaching amount can be as low as 0.87 mg / L or less.

[0052] Specifically, the iron source is selected from at least one of FeSO4, FeCl2, and Fe(NO3)2;

[0053] Specifically, the concentration of the iron source in the mixed solution is 0.004 to 0.035 mol / L, calculated as the molar amount of iron ions;

[0054] Specifically, the reducing agent is selected from at least one of NaBH4 and KBH4;

[0055] Specifically, the amount of the reducing agent used is 3.5 to 4 times that of the iron source on a molar basis.

[0056] Optionally, the solvent of the mixed solution containing the iron source and the montmorillonite carrier is a mixture of ethanol and water, preferably, the volume ratio of ethanol to water is 2 to 3:1.

[0057] Optionally, the reducing agent concentration in the reducing agent solution is 0.08 to 0.7 mol / L. The solvent of the reducing agent solution is deionized water. Preferably, the dripping speed is 25 to 35 drops / min.

[0058] Optionally, the specific conditions of the reaction include:

[0059] Under inert atmosphere and stirring conditions, the inert atmosphere refers to an atmosphere such as argon and nitrogen;

[0060] The reaction temperature is room temperature, which in the present invention refers to 20-28°C;

[0061] The reaction time is 0.5 to 1 hour.

[0062] The binder is selected from at least one of pseudo-boehmite, magnesium phosphate, and aluminum phosphate;

[0063] The binder accounts for 9-17% of the total mass of the binder and the montmorillonite-loaded zero-valent nano-iron material, preferably 15%, which can ensure both the stability of the material and the activity of the catalyst.

[0064] Preferably, the specific conditions of the calcination include:

[0065] Calcination temperature is 400-450°C;

[0066] The calcination time is 2.5 to 3 hours. One embodiment of the present invention provides a method for preparing a shaped particle electrode material by using a montmorillonite-loaded zero-valent nano-iron material, comprising the following steps:

[0067] Step 1: Preparation of montmorillonite (MMT) / biochar (C) montmorillonite-loaded zero-valent nano-iron material;

[0068] Step 2: dry-mixing the prepared montmorillonite-loaded zero-valent nano-iron material with a binder, and then wet-mixing with deionized water until it becomes a clay-like consistency;

[0069] Step 3: Place the clay-like mixed material in a vacuum clay mill for multiple clay milling, place it in a simple plodder to make long strips, and then granulate it using a pelletizer;

[0070] Step 4: The prepared particles were placed in a tubular furnace and calcined at 450° C. for 3 h under a nitrogen atmosphere to form the particles.

[0071] The preparation method of the granular electrode material provided by the present invention comprises wet mixing, drying, and calcining to form a certain amount of nano-zero-valent iron and an inorganic binder, biochar with a specific doping ratio and montmorillonite loaded with a certain amount of nano-zero-valent iron and pseudo-boehmite. This not only enables the nano-zero-valent iron to be successfully and evenly loaded on the carrier, but also exhibits relatively excellent electrochemical properties, thereby effectively improving the electrocatalytic oxidation performance of the material in a three-dimensional electrode system, reducing the amount of iron leaching in the solution, and avoiding the occurrence of secondary pollution.

[0072] In an optional embodiment, the specific conditions for calcining the particles into shape include:

[0073] The mixture was dried at 40-50°C for 60-90 min under an inert atmosphere, and then calcined at 450°C for 3 h under an inert atmosphere.

[0074] The specific surface area of ​​the granular montmorillonite loaded zero-valent nano-iron electrode material prepared in the embodiment of the present invention can reach 84m 2 / g, and the pore volume can reach 0.18cm 3 / g.

[0075] Preferably, the particle size of the granular montmorillonite-loaded zero-valent nano-iron electrode material is 3 to 5 mm.

[0076] Within this particle size range, the particle electrode can achieve centrifugal rotation at a speed of 400 to 450 r / min with the magnetic stirrer.

[0077] The montmorillonite-loaded zero-valent nano-iron electrode material prepared by the preparation methods provided in the above embodiments of the present invention can be used in the field of electrochemical catalytic oxidation of organic compounds.

[0078] An embodiment of the present invention provides a three-dimensional electrode system, including an anode, a cathode, and a granular electrode located between the anode and the cathode, wherein the granular electrode is a granular montmorillonite-loaded zero-valent nano-iron electrode material prepared in the above embodiment, and both the cathode and the anode are graphite plate-like carbon-based materials.

[0079] The following are specific embodiments of the present invention:

[0080] In the embodiment of the present invention:

[0081] The pseudo-boehmite was purchased from MacLean Company and was model P871910.

[0082] The biochar used in each example was produced by carbonizing washed wheat straw at 500°C for 4 h under a nitrogen atmosphere;

[0083] Other raw materials are conventional commercially available products.

[0084] Example 1

[0085] Preparation of granular montmorillonite-loaded zero-valent nano-iron electrode materials:

[0086] Step 1: Take 600 ml of a mixed liquid with a FeSO4·7H2O concentration of 0.0167 mol / L, wherein the solvent used in the mixed liquid is a mixture of anhydrous ethanol and deionized water in a volume ratio of 3:1); add 5 g of a montmorillonite carrier (the montmorillonite carrier used is a mixture of commercially available montmorillonite and biochar, and the biochar doping ratio in the montmorillonite carrier is 5% wt) to the above mixed liquid, stir continuously for 3 hours, and then add 100 ml of a 0.35 mol / L NaBH4 solution at a rate of 25-35 drops / min in a three-necked flask continuously purged with nitrogen. After the addition is completed, react for 30 minutes to obtain a montmorillonite-supported nano-zero-valent iron material, recorded as MMT(5%C) / nZVI (powder);

[0087] Step 2: The prepared montmorillonite-supported nano-zero-valent iron material was dried in a vacuum drying oven at 80°C for 6 hours to obtain a dried montmorillonite-supported nano-zero-valent iron material. The dried montmorillonite-supported nano-zero-valent iron material was passed through a 75-mesh sieve and dry-mixed with pseudo-boehmite, where the pseudo-boehmite content was 15% by weight. After uniform mixing, 5.2 mL of deionized water was added until the mixture formed a clay-like consistency. The mixture was then repeatedly kneaded in a vacuum slurry mill for 10 minutes. The mixture was then extruded into strips using a simple plodder. The pellets were then formed into granules with a particle size of approximately 3-5 mm using a pelletizer. The granules were then calcined in a tube furnace at 450°C for 3 hours to form the resulting material, designated MMT(5%C) / nZVI.

[0088] Comparative Example 1

[0089] This embodiment provides a granular montmorillonite-loaded zero-valent nano-iron electrode material, the preparation method of which includes:

[0090] The preparation method of montmorillonite-loaded zero-valent nano-iron in step 1 is basically the same as that in the embodiment, except that the montmorillonite carrier is not doped with biochar, and the prepared material is recorded as MMT / nZVI.

[0091] Step 2: 2.5 g of the prepared MMT / nZVI was added to 2.5 mL of polytetrafluoroethylene (PTFE), 29 mL of deionized water, 1 mL of iso-n-butanol, and 0.3 g of carbon black in a beaker and stirred. A small amount of ethanol was added during stirring and the mixture was sonicated for 30 minutes to achieve uniformity. Graphite felt (GF) was soaked in acetone for 4 hours, then rinsed with deionized water and dried at 105°C. GF was added to the mixture and sonicated for 30 minutes, stirring constantly to ensure uniform loading on both sides of the graphite felt electrode. The remaining mixed solution in the beaker was evenly applied to the electrode using a pipette. This entire process was performed under a nitrogen atmosphere. The loaded electrode was first dried in natural conditions for 2 hours, then in a vacuum drying oven for 24 hours. Subsequently, the sample was calcined in a tube furnace at 365°C for 60 minutes under nitrogen. This sample is designated as MMT / nZVI / GF.

[0092] Example 2-25

[0093] Examples 2-25 respectively provide a granular montmorillonite-loaded zero-valent nano-iron electrode material, and the preparation method thereof is basically the same as that of Example 1. The differences are shown in Table 1.

[0094] Table 1 Preparation conditions of Examples 1-25

[0095]

[0096]

[0097] Among them, the material obtained in Example 4 is recorded as MMT / nZVI.

[0098] The montmorillonite-loaded zero-valent nano-iron provided in each embodiment was characterized:

[0099] X-ray diffractometer (XRD) was used to observe the changes in elements in the material before and after loading. The MMT (5% C) / nZVI (powder) provided in Example 1 was used as a typical representative. Figure 1 It can be found that nano-zero-valent iron was successfully loaded onto the montmorillonite carrier (montmorillonite / biochar) without being oxidized. The morphologies of unloaded montmorillonite MMT, MMT (5% C) / nZVI (powder), and MMT / nZVI (powder) were observed and analyzed using scanning electron microscopy (SEM). MMT (5% C) / nZVI was also used as a typical representative. Figures 2-4It can be clearly observed that the montmorillonite without nano-zero-valent iron loading exhibits a distinct layered structure with uneven edges. The montmorillonite with or without biochar successfully loaded with nano-zero-valent iron. The biochar-doped nano-zero-valent iron is evenly distributed between the carrier layers and along the edges, indicating that the addition of biochar facilitates the dispersion of nZVI, resulting in a relatively uniform distribution on the carrier. A specific surface area analyzer was used to measure the pore parameters of MMT, MMT(5%C) / nZVI, and MMT / nZVI, again using MMT(5%C) / nZVI as a representative example (see Table 2).

[0100] Table 2 Pore structure parameters of particle electrodes

[0101]

[0102] The electrochemical performance of the granular montmorillonite-loaded zero-valent nano-iron electrode material provided in each embodiment was tested:

[0103] Electrochemical performance tests were performed using cyclic voltammetry. The test methods included:

[0104] A platinum metal disk electrode was used as the working electrode, a platinum sheet was used as the auxiliary electrode, and a saturated calomel electrode was used as the reference electrode. The electrode materials provided in each embodiment were used as particle electrodes to form a three-dimensional electrode system (no third electrode in the two-dimensional system, and other conditions were the same as the three-dimensional electrode system). The electrode potential was set to -0.2 to 0.6 V, and scanned from -0.2 V to the negative potential direction at a certain scanning speed. After the corresponding potential reached 0.6 V, the scanning direction was changed, and the same speed was used to scan back to the initial potential of -0.2 V. The scanning rates were set to 50, 100, 150, 200, 250, and 300 mV / s, respectively, and this scanning was repeated multiple times.

[0105] See also Figures 5-7 After adding the particle electrode, the peak value of the response current has obvious changes due to the different biochar doping ratios and the nano zero-valent iron loading. The current peak values ​​of different systems are linearly fitted at different scanning rates, and the size of the obtained k value can well represent the size of the electron mass transfer rate in the system. The electrode material provided by the embodiment of the present invention has relatively excellent electron mass transfer performance. Different charge transfer resistances are analyzed using electrochemical impedance spectroscopy, see Figure 8Taking Example 1 as a typical example, when the biochar doping amount is 3-7%, the system has a smaller solution charge and discharge resistance, which is more conducive to the reaction. A three-dimensional electrode system was constructed using the granular montmorillonite-loaded zero-valent nano-iron electrode material provided in each example as the granular electrode and a graphite plate as the cathode and anode. A two-dimensional electrode system was constructed using the MMT / nZVI / GF material prepared in Comparative Example 1 as the cathode and a graphite plate as the anode. The constructed three-dimensional system and two-dimensional system were respectively subjected to experiments on the removal of the antibiotic ciprofloxacin in water and the determination of the amount of iron leaching. The specific method for constructing the system and the specific steps of the experiment include:

[0106] Construction and experimental methods of three-dimensional electrode systems, including:

[0107] The experiment was carried out under the following conditions: a constant temperature magnetic stirrer was set at 400 r / min, room temperature was 25 ℃, a graphite plate (60 × 30 × 5 mm) was used as cathode and anode respectively, a spacing of 60 mm was set between the positive and negative electrodes, and the positive and negative electrodes were inserted 30 mm below the liquid level. A DC power supply was used to apply an applied voltage of 2 V, and the power supply was connected to the positive and negative electrodes with a red and black wire clamp. The electrolyte solution was 0.05 mol / L Na2SO4. In a 400 mL beaker, the basic control factors were kept constant, the initial pH value of the regulating solution was 3, 5 g / L of the material provided in each embodiment was added to the solution, 150 mL of a 10 mg / L ciprofloxacin aqueous solution was respectively added to the reaction system, and the concentration of ciprofloxacin was determined by spectrophotometry after 180 min. The iron ion leaching amount was determined by o-phenanthroline spectrophotometry. Each experiment was repeated twice.

[0108] The construction of the two-dimensional electrode system is similar to that of the three-dimensional electrode system, except that the MMT / nZVI / GF material prepared in Comparative Example 1 is used as the cathode, the graphite plate is used as the anode, and no other particulate materials are added to the electrolyte solution.

[0109] The three-dimensional system constructed with the materials provided in Example 1 is a typical example. Figure 9 and Figure 10 As shown in the figure, the electrode systems assembled by MMT (5% C) / nZVI and MMT / nZVI / GF have ideal removal effects on ciprofloxacin, but the iron ion leaching amount of MMT (5% C) / nZVI in the three-dimensional electrode system is significantly reduced, with the lowest being only 0.87 mg / L.

[0110] In summary, the electrode material prepared in the experimental example of the present invention has greater mechanical strength and good electrochemical properties. Compared with the nano-zero-valent iron-loaded composite cathode material, it can not only remove antibiotics in sewage equally effectively and achieve efficient degradation of pollutants, but also has less secondary pollution to the environment.

[0111] It should be understood that the above-described specific embodiments of the present invention are merely illustrative or illustrative of the principles of the present invention and do not constitute limitations of the present invention. Therefore, any modifications, equivalent substitutions, improvements, etc. made without departing from the spirit and scope of the present invention should be included within the scope of protection of the present invention. In addition, the appended claims are intended to cover all variations and modifications that fall within the scope and metes and bounds of the appended claims, or equivalents thereof.

Claims

1. A method for preparing a montmorillonite-loaded zero-valent nano-iron electrode material, characterized in that: include: A reducing agent solution is dropwise added to a mixed solution containing an iron source and a montmorillonite carrier to react to obtain a montmorillonite-loaded zero-valent iron material, wherein the ratio of the iron source to the montmorillonite carrier in the mixed solution is 0.0005 to 0.004 mol / g, wherein the iron source is calculated as a molar amount of divalent iron ions and the montmorillonite carrier is calculated as a mass amount. The montmorillonite carrier is montmorillonite doped with biochar, and the mass content of the biochar in the montmorillonite carrier is 3 to 20%, and the biochar is generated by carbonizing straw. The obtained montmorillonite-loaded zero-valent nano-iron material, a binder, and water are mixed to obtain a clay-like solid; The clay-like solid is granulated and calcined to obtain a granular montmorillonite-loaded zero-valent nano-iron electrode material.

2. The preparation method according to claim 1, characterized in that The mass content of the biochar in the montmorillonite carrier is 3-7%.

3. The preparation method according to claim 1, wherein: The iron source is selected from at least one of FeSO4, FeCl2, and Fe(NO3)2; The concentration of the iron source in the mixed solution is 0.004-0.035 mol / L based on the molar amount of iron ions; The reducing agent is selected from at least one of NaBH4 and KBH4; In terms of molar amount, the amount of the reducing agent is 3.5 to 4 times that of the iron source.

4. The preparation method according to claim 1, characterized in that The specific conditions of the reaction include: Carry out under inert atmosphere and stirring conditions; The reaction temperature is room temperature; The reaction time is 0.5~1h.

5. The preparation method according to claim 1, wherein: The binder is selected from at least one of pseudo-boehmite, magnesium phosphate, and aluminum phosphate; The binder accounts for 9-17% of the total mass of the binder and the montmorillonite-loaded zero-valent nano-iron material.

6. The preparation method according to claim 5, characterized in that: The specific conditions of the calcination include: Calcination temperature is 400~450℃; The calcination time is 2.5~3h.

7. The montmorillonite-loaded zero-valent nano-iron electrode material prepared by the preparation method according to any one of claims 1 to 6.

8. Use of the montmorillonite-loaded zero-valent nano-iron electrode material prepared by the preparation method according to any one of claims 1 to 6 in the field of electrochemical catalytic oxidation of organic compounds.

9. The use according to claim 8, characterized in that The montmorillonite-loaded zero-valent nano-iron electrode material is used as a particle electrode in a three-dimensional electrode.

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