Electrocatalysts, methods of making and using the same

Abstract

The present application relates to the field of catalyst, discloses a kind of electrocatalyst and its preparation method and application.The electrocatalyst includes metal active component, oxide carrier component and optional activated carbon, and the loss rate of metal active component of the electrocatalyst is less than 0.3wt% after being soaked in 10wt% 60 DEG C hydrochloric acid for 24h.The method for preparing electrocatalyst includes: impregnating carrier with impregnation solution containing binder and metal active component precursor, and then sequentially drying and calcining, and the carrier is selected from oxide carrier and / or activated carbon.The application also discloses the application of electrocatalyst as described above in three-dimensional electrocatalytic oxidation treatment of organic amine wastewater.The application also discloses the application of binder in reducing the loss rate of metal active component of electrocatalyst.The electrocatalyst of the present application can quickly and effectively reduce COD in organic amine wastewater under the action of current, and has stable performance, efficient operation, suitable for long-period operation, and great potential for development.

Description

Technical Field

[0001] This invention relates to the field of catalysts, and more specifically to electrocatalysts, their preparation methods, and applications. Background Technology

[0002] Organic amines are important chemical raw materials with wide applications in pharmaceuticals, leather tanning, rubber, petroleum, detergents, and synthetic dyes. Industrial wastewater from organic amine production has a high total nitrogen content and contains substances that are difficult to biodegrade and inhibit biodegradation; it cannot be directly discharged into natural water bodies without treatment. Currently, there is no good solution for treating this type of wastewater. Three-dimensional electro-oxidation, as a high-concentration organic wastewater treatment technology, uses air or pure oxygen as an oxidant under normal temperature and pressure conditions. With the synergistic effect of a microcurrent applied between the electrode plates and an electrocatalyst, nitrogen-containing organic pollutants in the liquid phase can be oxidized into CO2, N2, water, inorganic acids, or small-molecule organic compounds, thereby purifying the water. This is a green, energy-saving, and environmentally friendly wastewater treatment technology. The three-dimensional electro-oxidation reactor mainly includes a power source, reactor, anode and cathode plates, and electrocatalyst. Among these, the electrocatalyst is a key component of the three-dimensional electro-oxidation reaction and is crucial for improving reaction efficiency. Therefore, developing highly active and stable electrocatalysts is of great significance.

[0003] CN103241807A discloses a composite particle electrode for use in a bipolar three-dimensional electrode reactor and its preparation method. The composite particle electrode includes activated carbon particles and porous ceramic ring particles, wherein the activated carbon particles account for 60-70 wt% of the total particle electrode, and the porous ceramic ring particles account for 30-40 wt% of the total particle electrode. Different metal active components are loaded on the activated carbon particles and the porous ceramic ring particles respectively. The preparation includes (1) particle and particle pretreatment, (2) impregnation adsorption, (3) heat treatment, and (4) calcination activation. This invention has the characteristics of simple preparation method, low investment, easy industrialization, and high effective space utilization of electrolytic cells. It can be used for the pretreatment of high-concentration recalcitrant organic pollutants to improve the biodegradability of sewage, and can also be used for the deep treatment of low-concentration sewage in sewage treatment plants. However, this method will cause organic matter to adhere to the catalyst surface under long-term energization, affecting catalytic activity.

[0004] CN104925913A relates to a catalytic particle electrode for the simultaneous removal of recalcitrant organic matter and ammonia nitrogen from wastewater, its preparation method, and its application. The electrode comprises activated carbon from fruit shells with a particle size of 1mm-5mm and a metal component supported thereon, the metal component comprising 0.8wt%-2.5wt% of the total mass of the activated carbon. This particle catalytic electrode packing material features high catalytic activity, low cost and availability, simple preparation, high COD and ammonia nitrogen degradation and removal efficiency, high effluent mineralization, low energy consumption per unit COD, and continuous use. It is suitable for treating recalcitrant wastewater containing high concentrations of organic pollutants and high ammonia nitrogen. However, this method, with prolonged energization, causes the active component to detach from the activated carbon from the fruit shells, leading to deactivation of the electrocatalyst. Summary of the Invention

[0005] The purpose of this invention is to overcome the problem of unstable catalyst activity in the prior art, and to provide an electrocatalyst, its preparation method and application.

[0006] To achieve the above objectives, the first aspect of the present invention provides an electrocatalyst comprising a metal active component, an oxide support component, and optionally activated carbon, wherein the loss rate of the metal active component after the electrocatalyst is soaked in 10 wt% hydrochloric acid at 60°C for 24 h is less than 0.3 wt%.

[0007] A second aspect of the present invention provides a method for preparing an electrocatalyst, the method comprising: impregnating a support with an impregnation solution containing a binder and a precursor of a metal active component, and then sequentially drying and calcining the support, wherein the support is selected from oxide supports and / or activated carbon.

[0008] A third aspect of the present invention provides an electrocatalyst prepared by the above method.

[0009] The fourth aspect of the present invention provides an application of the electrocatalyst described above in the three-dimensional electrocatalytic oxidation treatment of organic amine wastewater.

[0010] The fifth aspect of the present invention provides the use of binders in reducing the loss rate of the metallic active components of electrocatalysts.

[0011] The electrocatalyst of this invention can rapidly and effectively reduce COD in organic amine wastewater under the action of current (in a three-dimensional electrocatalytic oxidation process). It has stable performance, high efficiency, and is suitable for long-term operation, and has great development potential.

[0012] The electrocatalyst of this invention was filled between the anode and cathode of a fixed-bed reactor. After continuous treatment for 600 hours at room temperature, atmospheric pressure, and a residence time of 30 minutes, a high COD removal rate was achieved while the loss rate of active components was less than 0.3 wt%. The electrocatalytic oxidation reaction of this invention can operate under low current and voltage conditions, has low energy consumption, and can effectively reduce the organic matter content of organic amine wastewater over a long period. The electrocatalyst of this invention is stable in the organic amine environment, thus this invention achieves good technical results. Detailed Implementation

[0013] The following provides a detailed description of specific embodiments of the present invention. It should be understood that the specific embodiments described herein are for illustrative and explanatory purposes only and are not intended to limit the invention. Furthermore, the endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values; these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of various ranges, the endpoint values ​​of various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0014] The present invention provides an electrocatalyst, characterized in that the electrocatalyst comprises a metal active component, an oxide support component and optional activated carbon, wherein the loss rate of the metal active component after the electrocatalyst is soaked in 10 wt% hydrochloric acid at 60°C for 24 h is less than 0.3 wt%, preferably less than 0.006 wt%, and more preferably less than 0.003 wt%.

[0015] According to the present invention, there is no particular limitation on the content of the metal active component in the electrocatalyst, but preferably, the content of the metal active component in the electrocatalyst, calculated as metal element, is 1-8 wt%, for example, 1.4 wt%, 1.8 wt%, 2.6 wt%, 3.4 wt%, 3.8 wt%, 4.5 wt%, 5.5 wt%, 6.5 wt%, 7.5 wt%, 8 wt%, or any value between the above values.

[0016] According to the present invention, the total content of the oxide support component and activated carbon in the electrocatalyst can be 92-99 wt%.

[0017] According to the present invention, the metal active component can be a metal or its oxide commonly used in electrocatalysts in the art, but preferably, the metal active component is selected from at least one of Group IB, Group VIII, Group IIA, Group VIB, Group VA, Group IIB, Group VB, Group IVA, Group VIIB metals and their oxides. More preferably, the metal active component is selected from at least one of Cu, Fe, Ca, W, Bi, Zn, Co, Cr, V, Ni, Sn, Mn and their oxides.

[0018] More preferably, the active metal component is Cu and Zn, and the weight ratio of Cu to Zn is 0.15-7, such as 0.15, 0.51, 0.81, 1.1, 1.51, 2.1, 2.51, 3.1, 3.51, 4.1, 4.51, 5.1, 5.51, 6.1, 6.51, 7 or any value between the above values.

[0019] More preferably, the active metal component is W and Co, and the weight ratio of W to Co is 1-7, such as 1.2, 2.1, 2.4, 3.1, 3.51, 4.1, 4.51, 5.1, 5.51, 6.1, 6.51, 7 or any value between the above values.

[0020] More preferably, the active metal components are Ni and Sn, and the weight ratio of Ni to Sn is 0.9-7, such as 1.3, 2.1, 2.51, 3.1, 3.51, 4.1, 4.51, 5.1, 5.51, 6.1, 6.51, 7 or any value between the above values.

[0021] More preferably, the active metal components are Cu, Ni and Sn, and the weight ratio of Cu, Ni and Sn is 1:1-3:1-7, most preferably 1:1-2:2-4.

[0022] More preferably, the active metal component is W and Sn, and the weight ratio of W to Sn is 1-7, such as 1.2, 1.8, 2.2, 2.4, 3.1, 3.5, 4.1, 4.5, 5.1, 5.5, 6.1, 6.5, 7 or any value between the above values.

[0023] The preferred embodiments described above, which select metal active components, can further improve the effect of the electrocatalyst in terms of COD removal rate in wastewater.

[0024] According to the present invention, the support oxide component can be an inorganic oxide commonly used in solid catalysts in the art, but preferably, the oxide support component is selected from alumina and / or silicon dioxide.

[0025] According to the present invention, the activated carbon can be any existing activated carbon used in electrocatalysts. Preferably, the activated carbon has a particle size in the range of 3-100 mm and a specific surface area of ​​600-1200 m². 2 / g.

[0026] According to a particularly preferred embodiment of the present invention, the electrocatalyst comprises a metal active component, alumina, and activated carbon. The content of the metal active component, calculated as a metal element, is 1-8 parts by weight (e.g., 1.5, 2.5, 3.5, 4.5, 5.5, 6.5, 7.5, 8, or any value between the above values) relative to 100 parts by weight of activated carbon, and the content of alumina is 1-3 parts by weight (e.g., 1, 1.2, 1.5, 1.8, 2, 2.5, 3, or any value between the above values).

[0027] The present invention also provides a method for preparing an electrocatalyst, characterized in that the method comprises: impregnating a support with an impregnation solution containing a binder and a precursor of a metal active component, and then drying and calcining the support in sequence, wherein the support is selected from oxide supports and / or activated carbon, preferably activated carbon.

[0028] In this invention, in order to further improve the stability of the electrocatalyst, the amount of binder relative to 100 parts by weight of the carrier is preferably 1-3 (such as 1, 1.2, 1.5, 1.8, 2, 2.5, 3 or any value between the above values) parts by weight, more preferably 1-2 parts by weight.

[0029] In this invention, relative to 100 parts by weight of the carrier, the amount of the metal active component precursor, calculated as metal element, can be 1-8 (e.g., 1.5, 2.5, 3.5, 4.5, 5.5, 6.5, 7.5, 8 or any value between the above) parts by weight.

[0030] In this invention, the metal active component precursor can be a substance commonly used in the art for preparing electrocatalysts. However, preferably, the metal active component precursor is selected from at least one of Group IB, Group VIII, Group IIA, Group VIB, Group VA, Group IIB, Group VB, Group IVA, and Group VIIB metal precursors. More preferably, the metal active component precursor is selected from at least one of Cu, Fe, Ca, W, Bi, Zn, Co, Cr, V, Ni, Sn, and Mn precursors. The metal active component precursor can be selected from common substances that can provide metal active components, and can be salts of metal active components, such as chlorides, sulfates, nitrates, organic acid salts (acetates), etc. For example, the Cu precursor can be selected from at least one of CuCl2, Cu(NO3)2, and CuSO4. The Co precursor can be selected from at least one of CoCl2, CoSO4, and Co(CH3COO)2. The Ni precursor can be selected from at least one of NiSO4, NiCl2, and Ni(NO3)2. The Fe precursor can be selected from at least one of FeSO4, FeCl2, and Fe(NO3)2. The Zn precursor can be selected from at least one of ZnSO4, ZnCl2, and Zn(NO3)2. The Ca precursor can be selected from at least one of CaSO4, CaCl2, and Ca(NO3)2. The Sn precursor can be selected from at least one of SnSO4, SnCl2, and Sn(NO3)2.

[0031] More preferably, the metal active component precursor is a Cu precursor and a Zn precursor, and the amount of both is such that the weight ratio of Cu to Zn is 0.15-7, such as 0.15, 0.51, 0.81, 1.1, 1.51, 2.1, 2.51, 3.1, 3.51, 4.1, 4.51, 5.1, 5.51, 6.1, 6.51, 7 or any value between the above values.

[0032] More preferably, the metal active component precursor is a W precursor and a Co precursor, and the amount of both is such that the weight ratio of W to Co is 1-7, such as 1.2, 2.1, 2.4, 3.1, 3.51, 4.1, 4.51, 5.1, 5.51, 6.1, 6.51, 7 or any value between the above values.

[0033] More preferably, the metal active component precursor is a Ni precursor and a Sn precursor, and the amount of both is such that the weight ratio of Ni to Sn is 0.9-7, such as 1.3, 2.1, 2.51, 3.1, 3.51, 4.1, 4.51, 5.1, 5.51, 6.1, 6.51, 7 or any value between the above values.

[0034] More preferably, the metal active component precursor is a Cu precursor, a Ni precursor and a Sn precursor, and the amount of the three is such that the weight ratio of Cu, Ni and Sn is 1:1-3:1-7, and most preferably 1:1-2:2-4.

[0035] More preferably, the metal active component precursor is a W precursor and a Sn precursor, and the amount of both is such that the weight ratio of W to Sn is 1-7, such as 1.2, 1.8, 2.2, 2.4, 3.1, 3.5, 4.1, 4.5, 5.1, 5.5, 6.1, 6.5, 7 or any value between the above values.

[0036] In this invention, the oxide support can be an inorganic oxide commonly used in the art for preparing solid catalysts, but is preferably selected from alumina and / or silica. The particle size of the oxide support can be in the range of 3-100 mm.

[0037] In this invention, the particle size of the activated carbon is preferably in the range of 3-100 mm, and the specific surface area is preferably 600-1200 m². 2 / g.

[0038] In a preferred embodiment of the present invention, the binder is selected from inorganic colloids and has a particle size of 1-100 nm. In a more preferred embodiment, the binder is selected from at least one of boehmite, aluminum sol, aluminum phosphate, titanium sol, silica sol, and water glass.

[0039] In this invention, the pH value of the impregnation solution is preferably 7.5-9, thereby further improving the stability of the inorganic colloid and ensuring thorough mixing of the inorganic colloid with the active metal component. To promote the formation of the binder colloid, acid is added to dissolve the binder, and then the pH value is adjusted with alkali to promote the formation of the colloid in the solution. For example, boehmite is dissolved in an acid solution (such as nitric acid with a concentration of 25-35 wt%) to form a solution, which is then mixed with the precursor solution and adjusted to a weakly alkaline state with an alkali solution to form an impregnation solution with a stable colloid.

[0040] In this invention, impregnation can be carried out by equal volume impregnation or excessive impregnation, and the impregnation time can be 6-24 hours.

[0041] In this invention, there are no particular restrictions on the drying conditions, which may include: a drying temperature of 70-90°C and a drying time of 12-80 hours.

[0042] In this invention, the calcination conditions may include: an inert atmosphere, a calcination temperature of 480-900℃, and a calcination time of 3-7 hours. The inert atmosphere may be provided by an inert gas and / or nitrogen. The preferred calcination temperature is 600-750℃. The preferred calcination time is 3.5-5.5 hours.

[0043] The present invention also provides an electrocatalyst prepared by the method described above.

[0044] Furthermore, the present invention also provides the application of the electrocatalyst described above in the three-dimensional electrocatalytic oxidation treatment of organic amine wastewater.

[0045] In this invention, the range of organic amines is relatively wide, including aliphatic amines, alcoholic amines, amides, alicyclic amines, aromatic amines, naphthyl amines, and other amines. The number of carbon atoms can be 1-20, specifically including but not limited to: monomethylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethanolamine, 3-propanolamine, triethylamine, ethylenediamine, cyclopropylamine, propylamine, dipropylamine, tripropylamine, isopropylamine, 1,2-propanediamine, diisopropylamine, 1,2-dimethylpropylamine, 2-propenylamine, sec-butylamine, n-butylamine, di-n-butylamine, isobutylamine, 1,4-propanediamine, diisopropyl ... -One or more of the following: butylene diamine, morpholine, diisobutylamine, diethylenetriamine, hexamethylenetetramine, hexylamine, 2-ethylhexylamine, hexamethylenediamine, monoethanolamine, diethanolamine, isopropanolamine, hexamethyleneimine, diisopropanolamine, triisopropanolamine, piperazine, N,N-methyldiethanolamine, N,N-diethylethanolamine, m-phenylenediamine, triethylenediamine, triethylenediamine, cycloethyleneimine, cyclohexylamine, 1-naphthylamine, 2-naphthylamine, aniline, diphenylamine, benzidine, o-methylaniline, m-methylaniline, p-methylaniline, o-phenylenediamine, and p-phenylenediamine.

[0046] In this invention, there are no particular restrictions on the content of organic amines in the wastewater. Preferably, the organic amine wastewater has a COD of 1000-50000 mg / L and a total nitrogen (TN) content of 10000-30000 mg / L. The COD test method is "HJ / T 399-2007 Determination of Chemical Oxygen Demand in Water - Rapid Digestion Spectrophotometric Method". The total nitrogen test method is "GBT 11894-89 Determination of Total Nitrogen in Water".

[0047] The specific operation of treating organic amine wastewater by three-dimensional electrocatalytic oxidation using the aforementioned electrocatalyst can be carried out in a conventional manner. For example, specific application methods may include, but are not limited to: filling the positive and negative electrodes with the aforementioned electrocatalyst, and passing current through the electrodes to react the organic amine wastewater with an oxygen-containing oxidant.

[0048] The oxygen-containing oxidant can be oxygen, air, oxygen-enriched air, or oxygen-deficient air. The amount of oxygen used is preferably 1-2 times the mass of oxygen required based on the original wastewater COD value. The electrode can be any conductive electrode, preferably a DSA electrode, such as an electrode with a rhodium-iridium coating on the upper surface of a titanium plate as the anode and a stainless steel plate as the cathode. The electrocatalyst fills the space between the positive and negative electrodes. The voltage between the electrode plates can be 1-10V, preferably 2-5V. The reaction temperature is preferably room temperature. The reaction pressure is preferably atmospheric pressure. The residence time of the organic amine wastewater can be 10-120 minutes, preferably 25-45 minutes.

[0049] This invention also provides the application of binders in reducing the loss rate of the metal active components of electrocatalysts. The specific types of binders, the metal active components of the electrocatalyst, the support, the preparation method, etc., can be as described above and will not be repeated here. The loss rate preferably refers to the loss rate of the metal active components after immersion in 10wt% hydrochloric acid at 60°C for 24 hours.

[0050] The present invention will be further illustrated below by way of examples, but these examples in no way limit the scope of the present invention.

[0051] Examples 1-15

[0052] The precursor of the metal active component was dissolved in water to form solution A; a binder solution (obtained by adding 1.5 parts by weight of 30 wt% nitric acid to 1.5 parts by weight of pseudoboehmite) was stirred thoroughly to form solution B; solutions A and B were mixed, and the pH was adjusted to 7.5 to obtain an impregnation solution; the resulting mixture was then impregnated in equal volumes onto irregularly shaped activated carbon (specific surface area of ​​800 m²) with a diameter of 3-100 mm at room temperature. 2 / g), impregnated overnight; dried at 80℃ for 4 hours; calcined in a muffle furnace at 700℃ for 4 hours under nitrogen protection to obtain the electrocatalyst. The amounts of active component precursor, binder and support are used to adjust the content of each component in the obtained electrocatalyst as shown in Table 1.

[0053] The precursors for Cu, W, Zn, Co, Sn, and Ni are CuCl2, Na2WO4, ZnCl2, CoCl2, SnCl2, and NiCl2, respectively.

[0054] Table 1

[0055]

[0056]

[0057] Examples 17-18

[0058] The electrocatalyst was prepared according to the method of Example 10, except that the support was replaced with γ-alumina (purchased from Sinopharm Reagent) and silica (purchased from Sinopharm Reagent), respectively.

[0059] Examples 19-21

[0060] The electrocatalyst was prepared according to the method of Example 10, except that the binder solution was replaced with titanium sol (purchased from Sinopharm Reagent), silica sol (purchased from Sinopharm Reagent), and water glass (purchased from Sinopharm Reagent), respectively.

[0061] Examples 22-23

[0062] The electrocatalyst was prepared according to the method of Example 10, except that the amount of binder used was 1 and 3 parts by weight, respectively.

[0063] Examples 24-25

[0064] The electrocatalyst was prepared according to the method of Example 10, except that the calcination temperatures were 480°C and 900°C, respectively.

[0065] Comparative Example 1

[0066] The electrocatalyst was prepared according to the method of Example 10, except that the metal active component was mixed with boehmite and water to obtain an impregnation solution.

[0067] Comparative Example 2

[0068] The electrocatalyst was prepared according to the method of Example 10, except that the binder solution was not used, and the activated carbon was directly impregnated with solution A.

[0069] Test Example 1

[0070] The performance of the electrocatalysts obtained in the above embodiments and comparative examples was evaluated under the following process conditions:

[0071] Raw materials: Prepare an aqueous solution of aniline, using simulated raw water with a COD of 25000 ml / L, and adjust the pH to 4;

[0072] Wastewater retention time: 30 minutes;

[0073] Fixed-bed reactor volume: 1000 ml;

[0074] An electrode with a rhodium-iridium coating (rhodium-iridium molar ratio of 1:1.5) on the upper surface of a titanium plate is used as the anode, and a stainless steel plate is used as the cathode.

[0075] Electrocatalyst loading amount: 500g, with no electrocatalyst added as a blank control and activated carbon used as a replacement electrocatalyst as a positive control;

[0076] Apply 2.4V to the electrode terminals;

[0077] Air is used as the oxidant, and the aeration rate is 60 ml / min;

[0078] Reaction temperature: Room temperature (approximately 25°C);

[0079] Reaction pressure: Atmospheric pressure;

[0080] COD removal rate = (COD before reaction - COD after reaction) / COD before reaction × 100%;

[0081] Loss rate of active component = (content of active component in electrocatalyst before reaction - content of active component in electrocatalyst after reaction) / content of active component in electrocatalyst before reaction × 100%;

[0082] The test method for COD before and after the reaction is "HJ / T 399-2007 Determination of Chemical Oxygen Demand in Water - Rapid Digestion Spectrophotometric Method";

[0083] The test method for the content of active components is GB / T 11894-89 Determination of Total Nitrogen in Water.

[0084] The test procedure for the loss rate of active components under acid treatment is as follows:

[0085] 20g of electrocatalyst was immersed in 100g of 10wt% hydrochloric acid solution and reacted at 60℃ for 24 hours with stirring. The mixture was then filtered, the solid was dried, and the metal content was determined by ICP analysis. The loss rate of active components was calculated as: (Weight of metal before acid treatment - Weight of metal after acid treatment) / Weight of metal before acid treatment × 100%.

[0086] The evaluation results are shown in Table 2.

[0087] Table 2

[0088]

[0089]

[0090] Comparing Examples 10 with Examples 17-18, Examples 10 with Examples 19-21, Examples 10 with Examples 22-23, and Examples 10 with Examples 24-25, it can be seen that using activated carbon as a carrier, using boehmite as a binder, controlling the amount of binder within the preferred range, and controlling the calcination temperature within the preferred range can yield electrocatalysts with better performance.

[0091] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various specific technical features in any suitable manner. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately. However, these simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A method for preparing an electrocatalyst, characterized in that, The method includes: impregnating a carrier with an impregnation solution containing a binder and a precursor of a metal active component, and then drying and calcining the carrier in sequence, wherein the carrier is selected from activated carbon; The impregnation solution has a stable colloid; The metal active component precursor is a W precursor and a Co precursor, and the amount of both is such that the weight ratio of W to Co is 1:1-7. The loss rate of the metal active component of the electrocatalyst after immersion in 10 wt% hydrochloric acid at 60°C for 24 hours was less than 0.003 wt%. The calcination conditions include: an inert atmosphere, a calcination temperature of 480-900℃, and a calcination time of 3-7 hours; The amount of the binder relative to 100 parts by weight of the carrier is 1-3 parts by weight, and the amount of the metal active component precursor, calculated as metal element, is 1-8 parts by weight.

2. The method according to claim 1, wherein, The activated carbon has a particle size in the range of 3-100 mm and a specific surface area of ​​600-1200 m². 2 / g.

3. The method according to claim 1, wherein, The binder is selected from inorganic colloids with a particle size in the range of 1-100 nm.

4. The method according to claim 1, wherein, The binder is selected from at least one of boehmite, aluminum sol, aluminum phosphate, titanium sol, silica sol, and water glass.

5. The method according to any one of claims 1-4, wherein, The pH value of the impregnation solution is 7.5-9; And / or, the impregnation time is 6-24 hours.

6. The method according to claim 1, wherein, The drying conditions include: a drying temperature of 70-90℃ and a drying time of 12-80h.

7. The method according to claim 1, wherein, The roasting temperature is 600-750℃; And / or, the roasting time is 3.5-5.5h.

8. An electrocatalyst prepared by the method according to any one of claims 1-7.

9. The application of the electrocatalyst according to claim 8 in the three-dimensional electrocatalytic oxidation treatment of organic amine wastewater.

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