Anode material for adipic acid monoester electrolysis and preparation method thereof

Abstract

The invention discloses an anode material for adipic acid monoester electrolysis and a preparation method of the anode material, the electrode solves the key problems that a platinum layer is easy to fall off, the catalytic activity is low, the organic matter poisoning resistance is poor and the like of a traditional titanium platinum-plated electrode through multi-scale interface strengthening and nano structure regulation and control; the preparation method comprises the following core steps: constructing a porous ZrO2-TiO2 composite oxide layer on the surface of a titanium substrate by adopting a micro-arc oxidation-hydrothermal composite process, and generating platinum nanoparticles in situ to pre-fill pores, so that the anchoring effect of a platinum layer is remarkably enhanced; depositing a platinum / carbon nano tube (Pt / CNT) composite catalyst layer on the surface of the oxide layer through a pulse-ultrasonic synergistic electroplating technology, wherein the carbon nano tube is used as a conductive framework to inhibit platinum agglomeration; through vacuum annealing and electrochemical activation treatment, the interface bonding force and active site exposure are further optimized; the electrode shows excellent performance in an adipic acid monoester electrolysis system, and efficient electrocatalytic conversion from adipic acid monomethyl ester to dimethyl sebacate is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of metal electrode materials and organic electrochemical synthesis, in particular to an anode material for electrolysis of adipic acid monoester and a preparation method thereof. Background Art

[0002] Dimethyl sebacate is a key intermediate in the synthesis of nylon, plasticizers, and biodiesel. Traditionally, dimethyl sebacate is produced by the esterification reaction of sebacic acid. This traditional method requires esterification, neutralization, and distillation, and is significantly affected by the production and price of sebacic acid. In recent years, electrochemical oxidation has become a research hotspot due to its green, efficient, and highly controllable characteristics, but its industrial application is limited by the performance bottleneck of electrode materials. Although the currently widely used titanium-based platinum-plated electrodes have high conductivity and corrosion resistance, the interfacial bonding between the platinum layer and the titanium substrate is weak due to the difference in thermal expansion coefficients. The platinum layer is easily peeled off during electrolysis. The platinum particles formed by the traditional direct current electroplating process are coarse, with a low specific surface area and insufficient density of catalytic active sites, resulting in low current efficiency. During the electrolysis process, organic intermediates are adsorbed on the electrode surface, causing severe passivation. Frequent shutdowns for cleaning are required, affecting continuous production. Although the existing improved technology has partially improved the uniformity of the coating, it has failed to fundamentally solve the core problems such as insufficient platinum-titanium interface bonding strength, difficulty in precise control of nano-scale active sites, and weak resistance to organic poisoning, which seriously restricts the industrialization process of electrochemical synthesis of dimethyl sebacate. Summary of the Invention

[0003] The present invention discloses an anode material for the electrolysis of monoadipate. This electrode solves the key problems of traditional titanium-plated platinum electrodes, such as easy detachment of the platinum layer, low catalytic activity, and poor resistance to organic poisoning, through multi-scale interface strengthening and nanostructure regulation. The preparation of an anode material for the electrolysis of monoadipate according to the present invention includes the following core steps: constructing a porous ZrO2-TiO2 composite oxide layer on the surface of a titanium substrate using a micro-arc oxidation-hydrothermal composite process, and in situ generating platinum nanoparticles to pre-fill the pores, significantly enhancing the anchoring effect of the platinum layer; depositing a platinum / carbon nanotube (Pt / CNT) composite catalytic layer on the surface of the oxide layer using a pulse-ultrasonic coordinated electroplating technique, with the carbon nanotubes acting as a conductive skeleton to inhibit platinum agglomeration; and further optimizing the interfacial bonding force and active site exposure through vacuum annealing and electrochemical activation treatment. The electrode exhibits excellent performance in the monoadipate electrolysis system, achieving efficient electrocatalytic conversion of monomethyl adipate to dimethyl sebacate.

[0004] To achieve the above object, the present invention provides the following technical solutions: The present invention provides an anode material for electrolysis of adipic acid monoester, which is composed of a three-level functionalized structure, including: The titanium substrate is pretreated by alkaline washing, degreasing and acid etching to form a rough surface at the micron level using industrial pure titanium as a support carrier, which is then washed with NaOH and etched with hydrochloric acid to enhance the mechanical bonding of the interface. The porous ZrO2-TiO2 composite oxide layer is obtained by micro-arc oxidation-hydrothermal composite treatment. The porous ZrO2-TiO2 composite oxide layer is generated by micro-arc oxidation in an electrolyte containing phosphate and zirconate. The thickness is 10-15μm and the pore size is 100-500nm. The ZrO2 nanocrystals are uniformly embedded in the TiO2 matrix, with a porosity of 35-40%. It has both high hardness and acid resistance. The platinum / carbon nanotube composite catalytic layer is deposited on the surface of the porous ZrO2-TiO2 composite oxide layer by pulse electroplating. Through pulse-ultrasonic synergistic electroplating deposition, platinum particles with an average particle size of 10~20nm are loaded on the surface of carboxylated CNTs and in the pores of the porous ZrO2-TiO2 composite oxide layer, forming a three-dimensional conductive network, which significantly improves the catalytic activity and resistance to organic adsorption.

[0005] The present invention also provides a method for preparing the anode material for electrolysis of adipic acid monoester according to claim 1 or 2, comprising the following steps: S01, titanium substrate pretreatment, immerse the 2mm titanium plate in a NaOH solution with a concentration of 8-12% and treat it at 70-90°C for 1-2 hours to remove the surface oxide film; use acetone ultrasonic cleaning for 10-20 minutes to remove organic pollutants; then immerse it in a 20-40% hydrochloric acid solution at 60°C for etching for 2 hours to obtain the pretreated titanium substrate; S02, micro-arc oxidation-hydrothermal composite treatment: the pretreated titanium substrate is placed in an electrolyte containing Na3PO4 and K2ZrF6, and treated with a bipolar pulse power supply for 15 minutes to generate a porous ZrO2-TiO2 composite oxide layer; the oxidized titanium substrate is placed in a hydrothermal reaction solution containing H2PtCl6 and reducing sugars, and reacted at 160-200°C for 4-8 hours, and platinum nanoparticles with an average particle size of 10-20nm are in situ generated in the pores of the porous ZrO2-TiO2 composite oxide layer, with a filling rate of more than 85% and an interfacial bonding strength increased to 20-30MPa; S03, pulse electroplating of a platinum / carbon nanotube composite catalytic layer: placing the titanium substrate obtained in step S02 in an electroplating solution containing H2PtCl6, carboxylated carbon nanotubes, sodium dodecyl sulfate, and cerium nitrate; using a pulse current mode, a forward current density of 15-25 mA / cm², a pulse width of 8-12 ms; a reverse current density of 3-7 mA / cm², a pulse width of 1-3 ms; an electroplating temperature of 45-55°C, and a time of 60-120 minutes; applying ultrasonic assisted dispersion at a frequency of 35-45 kHz throughout the process; the ultrasonic cavitation effect promotes uniform dispersion of CNTs, and the pulse current inhibits abnormal growth of platinum particles; ultimately forming a three-dimensional composite layer with platinum particles having a particle size of 10-20 nm, a specific surface area of ​​30-50 m² / g, and a coating bonding strength of 25-30 MPa; S04, post-treatment and activation: In a mixed gas of Ar and H2, the three-dimensional composite layer is annealed at 550~650℃ for 1.5~2.5 hours to eliminate internal stress and form strong Pt-CNT interface coupling; in a 0.1~1.0M H2SO4 solution, cyclic voltammetry activation is carried out for 10~30 times at a scan rate of 30~70mV / s to remove surface oxides and expose highly active crystal faces to obtain an anode material for the electrolysis of monoadipate.

[0006] Furthermore, in step S02, the concentration of Na3PO4 in the electrolyte is 0.1-0.5 M, and the concentration of K2ZrF6 is 0.02-0.06 M. The conditions for the bipolar pulse power treatment are: forward 300-400 V, reverse 60-80 V, and frequency 400-600 Hz.

[0007] Furthermore, in the hydrothermal reaction solution of step S02, the reducing sugar concentration is 0.04-0.08 M, the molar ratio of H₂PtCl₂ to the reducing sugar is 1:1.5-2.5, and the reducing sugar is one of glucose, fructose, and sucrose. The hydrothermal reaction solution also contains CTAB at a concentration of 0.1-0.3 M, and the solvent is a mixed solution of ethanol and water, wherein the volume ratio of ethylene glycol to water is 1:1.

[0008] Furthermore, in step S03, the electroplating solution is an electroplating solution containing 10-15 g / L H2PtCl6, 0.3-0.6 g / L carboxylated carbon nanotubes, 1-4 g / L sodium dodecyl sulfate and 0.2-0.5 g / L cerium nitrate.

[0009] Furthermore, in step S04, the volume ratio of Ar and H2 is 90:10-95:5, the heating rate of annealing is 5-10°C / min, and after annealing, the electrode is naturally cooled to room temperature under the protection of argon.

[0010] The present invention also provides an application of the anode material for electrolysis of adipic acid monoester as described above in organic electrochemical synthesis, wherein the application includes the following conditions: Electrode configuration: the anode is the composite platinum-plated electrode according to claim 1, and the cathode is a titanium mesh or graphite electrode; Electrolyte system: monoadipate as the reaction substrate, with a concentration of 0.5~2.0M; supporting electrolyte is one of triethylamine, triethylenediamine or diethylamine, with a concentration of 0.1~0.5M; Electrolysis parameters: current density 100~200mA / cm², temperature 50~65℃, electrolysis time 8~16 hours.

[0011] A circulating flow electrolytic cell is used during the electrolysis process with a flow rate of 0.5~2.0L / min.

[0012] Compared with the prior art, the present invention has the following beneficial effects: The anode material for the electrolysis of monoadipate of the present invention consists of a three-level functionalized structure: a pretreated titanium substrate is used as a supporting carrier, pure titanium is used for alkaline washing with NaOH and acid etching with hydrochloric acid to form a micron-scale rough surface, thereby enhancing the mechanical bonding of the interface; a porous ZrO2-TiO2 composite oxide layer is generated in an electrolyte containing phosphate and zirconate by a micro-arc oxidation process, with a thickness of 10-15 μm and a pore size of 100-500 nm, wherein ZrO2 nanocrystals are uniformly embedded in the TiO2 matrix, with a porosity of 35-40%, and having both high hardness and acid resistance; a platinum / carbon nanotube (Pt / CNT) composite catalytic layer is deposited by pulse-ultrasonic coordinated electroplating, with platinum particles having an average particle size of 10-20 nm, which are loaded on the surface of carboxylated CNTs and in the pores of the oxide layer to form a three-dimensional conductive network, thereby significantly improving the catalytic activity and resistance to organic adsorption. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 This is an SEM image of the ZrO2-TiO2 composite oxide layer prepared in Example 1; Figure 2 This is the SEM image of the Pt / CNT composite layer prepared in Example 1. DETAILED DESCRIPTION

[0014] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention. Example 1

[0015] (1) Pretreatment of titanium substrate: immerse a 2 mm thick pure titanium plate in a 10% NaOH solution at 80 °C for 1 hour to remove the surface oxide film; ultrasonically clean the plate with acetone for 10 minutes to remove organic pollutants; then etch the plate in a 37% hydrochloric acid solution at 60 °C for 2 hours to form a micron-scale rough surface, thus obtaining the pretreated titanium substrate. (2) Micro-arc oxidation-hydrothermal composite treatment: In an electrolyte containing 0.2M Na3PO4 and 0.05M K2ZrF6, a bipolar pulse power supply (forward voltage 400V / 10ms, reverse voltage 80V / 2ms, frequency 500Hz) was used for 15 minutes to form a porous ZrO2-TiO2 composite oxide layer such as Figure 1 The oxidized titanium substrate was placed in a hydrothermal reaction solution containing 0.1M H2PtCl6, 0.05M glucose, and 0.1M CTAB in a 1:1 ethylene glycol / water (volume ratio) mixture at 180°C in an autoclave for 6 hours. Platinum nanoparticles with an average particle size of 10-20nm were in situ generated within the pores of the oxide layer. The filling rate reached 90%, and the interfacial bonding strength was increased to 28MPa. (3) Pulse electroplating of Pt / CNT composite layer: 15g / L H2PtCl6·6H2O, 0.5g / L carboxylated CNT, 2g / LSDS, 0.2g / L cerium nitrate, 50mL / L ethylene glycol were used as the electroplating solution. The pulse current mode was adopted, with a forward current density of 20mA / cm², a pulse width of 10ms, a reverse current density of 5mA / cm², a pulse width of 2ms, an electroplating temperature of 50℃, and a time of 90 minutes. Ultrasonic dispersion with a frequency of 40kHz was applied throughout the process to finally form an electroplated Pt / CNT composite layer. Platinum particles were loaded on the surface of the carboxylated CNT and in the pores of the oxide layer to form a three-dimensional nanoflower structure. The average particle size of the platinum particles was 12~16nm, the specific surface area was 45m² / g, and the coating bonding strength was 28MPa. Figure 2 shown.

[0016] (4) Post-treatment and activation: Annealing was performed at 600°C for 2 hours in an Ar / H2 mixed gas (volume ratio 95:5). Cyclic voltammetry activation was performed 20 times in a 0.5M H2SO4 solution at a scan rate of 50 mV / s. The anode material (titanium-based composite platinum-plated electrode) for the electrolysis of adipic acid monoester was obtained.

[0017] (5) Electrolysis applications: Using the titanium-based composite platinum-plated electrode prepared above as the anode and a titanium mesh cathode, continuous electrolysis was performed for 10 hours in an electrolyte system consisting of 1.0M monoadipate, methanol, and 0.2M triethylamine at a current density of 150mA / cm², a temperature of 60°C, and an electrolyte flow rate of 1.0L / min. The results showed an 85% selectivity for synthesized dimethyl sebacate and an 80% feedstock conversion rate. After 1000 hours of continuous operation, the platinum loss rate was only 0.8%.

[0018] The SEM images of the prepared ZrO2-TiO2 composite oxide layer are shown in Figure 1 As shown in the figure, the electron microscope scanning image of porous ZrO2-TiO2 nanotubes shows that they have a tubular structure and are evenly distributed. The SEM image of the Pt / CNT composite layer is shown in the figure. Figure 2 As shown, the formation of three-dimensional nanoflower structures of platinum nanoparticles. Example 2

[0019] The electrode preparation method is the same as Example 1 Electrolysis applications: Using the titanium-based composite platinum-plated electrode prepared above as the anode and a titanium mesh cathode, continuous electrolysis was performed for 10 hours in an electrolyte system consisting of 1.0M monoadipate, methanol, and 0.2M diethylamine at a current density of 150mA / cm², a temperature of 60°C, and an electrolyte flow rate of 1.0L / min. The results showed an 83% selectivity for synthesized dimethyl sebacate and a 77% feedstock conversion rate. After 1000 hours of continuous operation, the platinum loss rate was 1.5%. Example 3

[0020] The difference from Example 1 is the different platinum content, as follows: During the hydrothermal reduction stage, the H2PtCl6 concentration dropped to 0.05 M, and the H2PtCl6·6H2O concentration in the plating solution dropped to 10 g / L; The results of the micro-arc oxidation-hydrothermal composite treatment: platinum nanoparticles with an average particle size of 15-20nm were generated in situ within the pores of the oxide layer; the filling rate reached 85%, and the interfacial bonding strength was 26MPa; Pulse electroplating results for a Pt / CNT composite layer: The resulting Pt / CNT composite layer features platinum particles loaded onto the surface of the carboxylated CNTs and within the pores of the oxide layer, forming a three-dimensional nanoflower structure. The average particle size is 17-20 nm, the specific surface area is 38 m² / g, and the coating has a bonding strength of 25 MPa.

[0021] Electrolysis applications: Using the titanium-based composite platinum-plated electrode prepared above as the anode and a titanium mesh cathode, continuous electrolysis was performed for 10 hours in an electrolyte system consisting of 1.0M monoadipate, methanol, and 0.2M triethylamine at a current density of 150mA / cm², a temperature of 60°C, and an electrolyte flow rate of 1.0L / min. The results showed an 82% selectivity for synthesized dimethyl sebacate and a 78% feedstock conversion rate. After 1000 hours of continuous operation, the platinum loss rate was 1.2%. Example 4

[0022] The difference from Example 1 is that the micro-arc oxidation time and annealing temperature are different, as follows: The micro-arc oxidation time was extended to 20 minutes and the annealing temperature was increased to 700 °C.

[0023] The results of the micro-arc oxidation-hydrothermal composite treatment showed that platinum nanoparticles with an average particle size of 18-20 nm were generated in situ within the pores of the oxide layer; the filling rate reached 87%, and the interfacial bonding strength was 26 MPa; Results of pulse electroplating of a Pt / CNT composite layer: The resulting Pt / CNT composite layer consists of platinum particles loaded onto the surface of the carboxylated CNTs and within the pores of the oxide layer, forming a three-dimensional nanoflower structure. The average particle size is 16-19 nm, the specific surface area is 40 m² / g, and the coating has a bonding strength of 27 MPa.

[0024] Electrolysis applications: Using the titanium-based composite platinum-plated electrode prepared above as the anode and a titanium mesh cathode, continuous electrolysis was performed for 10 hours in an electrolyte system consisting of 1.0M monoadipate, methanol, and 0.2M triethylamine at a current density of 150mA / cm², a temperature of 60°C, and an electrolyte flow rate of 1.0L / min. The results showed an 80% selectivity for synthesized dimethyl sebacate and a 78% feedstock conversion rate. The electrode exhibited no coating cracking after 1000 hours of continuous operation. Example 5

[0025] The difference from Example 1 lies in the difference in pulse current density and annealing temperature, as follows: The pulse current density was increased to 25 mA / cm² in the forward direction and 7 mA / cm² in the reverse direction, and the annealing temperature was 650°C.

[0026] The results of micro-arc oxidation-hydrothermal composite treatment: platinum nanoparticles with an average particle size of 10~20nm were in situ generated in the pores of the oxide layer; the filling rate reached 90%, and the interfacial bonding strength was increased to 28MPa.

[0027] Pulse electroplating results for a Pt / CNT composite layer: The resulting Pt / CNT composite layer features platinum particles loaded onto the surface of the carboxylated CNTs and within the pores of the oxide layer, forming a three-dimensional nanoflower structure. The average particle size is 15-18 nm, the specific surface area reaches 42 m² / g, and the coating has a bonding strength of 27 MPa.

[0028] Electrolysis applications: Using the titanium-based composite platinum-plated electrode prepared above as the anode and a titanium mesh cathode, continuous electrolysis was conducted for 10 hours in an electrolyte system consisting of 1.0M monoadipate, methanol, and 0.2M triethylamine at a current density of 150mA / cm², a temperature of 60°C, and an electrolyte flow rate of 1.0L / min. The results showed a selectivity of 82% for synthesized dimethyl sebacate and a feedstock conversion rate of 79%. The electrode voltage fluctuation was less than 4% after 800 hours. Example 6

[0029] The difference from Example 1 is that the concentrations of Na3PO4 and K2ZrF6 in the electrolyte are different, as follows: The concentrations of Na3PO4 and K2ZrF6 in the electrolyte are 0.3M and 0.1M, respectively.

[0030] The results of the micro-arc oxidation-hydrothermal composite treatment showed that platinum nanoparticles with an average particle size of 12-16 nm were generated in situ within the pores of the oxide layer; the filling rate reached 89% and the interfacial bonding strength was 28 MPa; Pulse electroplating results for a Pt / CNT composite layer: The resulting Pt / CNT composite layer features platinum particles loaded onto the carboxylated CNT surface and within the pores of the oxide layer, forming a three-dimensional nanoflower structure. The average particle size is 13-17 nm, the specific surface area reaches 43 m² / g, and the coating has a bonding strength of 27 MPa.

[0031] Electrolysis applications: Using the titanium-based composite platinum-plated electrode prepared above as the anode and a titanium mesh cathode, continuous electrolysis was performed for 10 hours in an electrolyte system consisting of 1.0 M monoadipate, methanol, and 0.2 M triethylamine at a current density of 150 mA / cm², a temperature of 60°C, and an electrolyte flow rate of 1.0 L / min. The results showed a selectivity of 79% for synthesized dimethyl sebacate and a feedstock conversion rate of 75%. After 1000 hours of continuous operation, the electrode experienced a platinum loss of 1%.

[0032] The comparative analysis of Examples 1-6 is shown in Table 1.

[0033] Table 1 Comparative analysis of Examples 1-6

[0034] This invention utilizes a micro-arc oxidation-hydrothermal composite process to construct a porous ZrO2-TiO2 layer and a platinum / CNT composite catalytic layer. The process parameters are flexibly adjustable, adapting to high current density and high-temperature conditions. The electrode achieves a DMS selectivity of 80%-88% and a lifespan exceeding 1000 hours (with a platinum loss rate of less than 1.5%) in industrial electrolysis, combining high catalytic efficiency with long-term stability. By flexibly adjusting the process parameters and adapting to different electrolyte systems, it provides a highly efficient and durable electrode solution for green electrochemical synthesis.

[0035] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0036] It should be noted that the above content merely illustrates the technical idea of ​​the present invention and cannot be used to limit the scope of protection of the present invention. For ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications all fall within the scope of protection of the claims of the present invention.

Claims

1. An anode material for electrolysis of adipic acid monoester, characterized in that: The invention comprises a titanium substrate whose surface has been degreased by alkali washing and roughened by acid etching, a porous ZrO2-TiO2 composite oxide layer obtained by micro-arc oxidation-hydrothermal composite treatment, and a platinum / carbon nanotube composite catalytic layer deposited on the surface of the porous ZrO2-TiO2 composite oxide layer by pulse electroplating; the porous ZrO2-TiO2 composite oxide layer has a thickness of 10-15 μm and a pore diameter of 100-500 nm, platinum nanoparticles are loaded in the pores of the porous ZrO2-TiO2 composite oxide layer and on the surface of the carbon nanotubes, the particle diameter of the platinum nanoparticles is 10-30 nm, and the thickness of the platinum / carbon nanotube composite catalytic layer is 3-5 nm.

2. The anode material for electrolysis of adipic acid monoester according to claim 1, characterized in that: The carbon nanotube content in the platinum / carbon nanotube composite catalytic layer is 5-15 wt %.

3. A method for preparing an anode material for electrolysis of adipic acid monoester according to claim 1 or 2, characterized in that: The following steps are included: S01, titanium substrate pretreatment, immerse the titanium plate in a NaOH solution with a concentration of 8-12% and treat it at 70-90°C for 1-2 hours to remove the surface oxide film; Use acetone ultrasonic cleaning for 10 to 20 minutes to remove organic pollutants; Then, the titanium substrate was immersed in a 20-40% hydrochloric acid solution at 60°C for etching for 2 hours to obtain a pretreated titanium substrate; S02, micro-arc oxidation-hydrothermal composite treatment: the pretreated titanium substrate is placed in an electrolyte containing Na3PO4 and K2ZrF6 and treated with a bipolar pulse power supply for 15 minutes to form a porous ZrO2-TiO2 composite oxide layer; the oxidized titanium substrate is placed in a hydrothermal reaction solution containing H2PtCl6 and reducing sugars and reacted at 160-200°C for 4-8 hours to in-situ generate platinum nanoparticles in the pores of the porous ZrO2-TiO2 composite oxide layer; S03. Pulse electroplating of a platinum / carbon nanotube composite catalyst layer: placing the titanium substrate obtained in step S02 in an electroplating solution containing H2PtCl6, carboxylated carbon nanotubes, sodium dodecyl sulfate, and cerium nitrate; using a pulse current mode with a forward current density of 15-25 mA / cm² and a pulse width of 8-12 ms; a reverse current density of 3-7 mA / cm² and a pulse width of 1-3 ms; an electroplating temperature of 45-55°C and a time of 60-120 minutes; and applying ultrasonic wave-assisted dispersion throughout the process to obtain a three-dimensional composite layer; S04, post-treatment and activation: In a mixed gas of Ar and H2, the three-dimensional composite layer is annealed at 550-650°C for 1.5-2.5 hours; in a 0.1-1.0 M H2SO4 solution, cyclic voltammetry activation is performed for 10-30 times at a scan rate of 30-70 mV / s to obtain an anode material for the electrolysis of adipic acid monoester.

4. The method for preparing an anode material for electrolysis of adipic acid monoester according to claim 1, characterized in that: In step S02, in the electrolyte, the concentration of Na3PO4 is 0.1~0.5M, and the concentration of K2ZrF6 is 0.02~0.06M.

5. The method for preparing an anode material for electrolysis of adipic acid monoester according to claim 1, characterized in that: In the hydrothermal reaction solution of step S02, the concentration of the reducing sugar is 0.04~0.08M, the molar ratio of H2PtCl6 to the reducing sugar is 1:1.5~2.5, and the reducing sugar is one of glucose, fructose, and sucrose.

6. The method for preparing an anode material for electrolysis of adipic acid monoester according to claim 1, characterized in that: In step S03, the electroplating solution contains 10-15 g / L H2PtCl6, 0.3-0.6 g / L carboxylated carbon nanotubes, 1-4 g / L sodium lauryl sulfate, and 0.2-0.5 g / L cerium nitrate.

7. The method for preparing an anode material for electrolysis of adipic acid monoester according to claim 1, characterized in that: In step S03, the ultrasonic frequency is 35-45 kHz.

8. The method for preparing an anode material for electrolysis of adipic acid monoester according to claim 1, characterized in that: In step S04, the volume ratio of Ar and H2 is 90:10-95:5, the annealing heating rate is 5-10°C / min, and after annealing, the electrode is naturally cooled to room temperature under argon protection.

9. Use of the anode material for electrolysis of adipic acid monoester according to claim 1 or 2 in organic electrochemical synthesis, characterized in that: The application includes the following conditions: Electrode configuration: the anode is the composite platinum-plated electrode according to claim 1, and the cathode is a titanium mesh or graphite electrode; Electrolyte system: monoadipate as the reaction substrate, concentration of 0.5~2.0M; The supporting electrolyte is one of triethylamine, triethylenediamine or diethylamine, with a concentration of 0.1~0.5M; Electrolysis parameters: current density 100~200mA / cm², temperature 50~65℃, electrolysis time 8~16 hours.

10. Use of an anode material for electrolysis of adipic acid monoester according to claim 9 in organic electrochemical synthesis, characterized in that: A circulating flow electrolytic cell is used during the electrolysis process with a flow rate of 0.5~2.0L / min.

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