Preparation of ultrafine nano-sponge platinum system and process method thereof

Abstract

This invention relates to the field of electrochemical technology, and more particularly to a system for preparing ultrafine nano-platinum sponges and a process method thereof. The system includes a main body comprising a reaction vessel. The reaction vessel has a raw material module and a batching module at its feed end, and a hydrazine hydrate module at its feed end. Multiple nitrogen modules are installed within the main body. A cooling water module and a heating oil module are connected to the reaction vessel. A catalyst drying module is also connected to the reaction vessel. The nitrogen modules include several nitrogen storage tanks. This invention successfully prepares fine-particle electrocatalysts by reducing chloroplatinic acid with a specific reducing agent, effectively overcoming the performance shortcomings of catalysts prepared by traditional methods, and providing strong support for improving the efficiency of hydrogen production through proton exchange membrane water electrolysis.

Description

Technical Field

[0001] This invention relates to the field of electrochemical technology, and in particular to a process for preparing an ultrafine nano-sponge platinum system and a method thereof. Background Technology

[0002] Hydrogen energy is a green and clean energy source that is being increasingly used. How to produce hydrogen is key to its utilization. Acidic water electrolyzers can electrolyze water to convert electrical energy into hydrogen energy, and hydrogen fuel cells are an important application of hydrogen energy. These two clean energy conversion systems are crucial for hydrogen energy utilization. For these devices to achieve high performance and high energy conversion efficiency, highly active and stable catalysts are essential. Micro- and nano-platinum particles (platinum black) possess excellent electrocatalytic performance and good corrosion resistance, making them core catalyst materials for acidic water electrolyzers and hydrogen fuel cells. Therefore, a simple, low-cost method for preparing platinum nanocrystals with high yield of the target product is of great significance for the application of hydrogen energy.

[0003] Currently, the main method for platinum preparation in China is the repeated precipitation of ammonium chloroplatinate. This method produces platinum with low purity, which cannot meet the requirements of modern scientific development. Abroad, high-purity platinum is mostly produced using physical metallurgical methods, such as single crystal pulling. These methods involve significant investment and complex operation. Furthermore, the waste liquid and impurities generated during the extraction of high-purity platinum are generally treated and discharged, resulting in the waste of small amounts of crude platinum contained in the waste liquid and impurities, and also causing environmental pollution. In the preparation of catalysts for electrolyzers used in proton exchange membrane water electrolysis to produce hydrogen, electrocatalysts can reduce overpotential by more than 400mV, playing a crucial role. In platinum particle production, how to prepare fine-particle, high-specific-surface-area catalysts is currently a research hotspot. Traditional catalyst preparation methods often struggle to precisely control the size and specific surface area of ​​catalyst particles, resulting in larger catalyst particles with smaller specific surface areas, which cannot fully meet the high-performance catalyst requirements of water electrolyzers, thus limiting the improvement of water electrolysis efficiency. Summary of the Invention

[0004] To address some of the problems existing in the prior art, this invention provides a system for preparing ultrafine nano-sponge platinum. By using a specific reducing agent to reduce chloroplatinic acid, a fine-particle electrocatalyst can be successfully prepared, effectively solving the performance deficiencies of catalysts prepared by traditional methods and providing strong support for improving the efficiency of hydrogen production by proton exchange membrane water electrolysis.

[0005] To achieve the above objectives, the present invention provides a system for preparing ultrafine nano-sized platinum sponges, comprising a system body, the system body including a reaction vessel, a raw material module and a batching module being configured at the feed end of the reaction vessel, a hydrazine hydrate module being configured at the feed end of the reaction vessel, multiple nitrogen modules being configured within the system body, a cooling water module and a heating oil module being connected to the reaction vessel, a catalyst drying module being connected to the reaction vessel, and the nitrogen modules including several nitrogen storage tanks.

[0006] As a further improvement of the present invention, in order to enable users to flexibly select the type and combination of reducing agents according to specific process requirements, realize the reuse of reducing agents or anti-sticking treatment, and further improve resource utilization efficiency and product quality, the raw material module includes several groups of raw material storage tanks arranged in parallel with the reactor. The raw material storage tanks are divided into polytetrafluoroethylene storage tanks, isopropanol storage tanks, ethanol storage tanks, propionaldehyde storage tanks, acetaldehyde storage tanks, formaldehyde storage tanks, ethylene glycol storage tanks and hydrogen storage tanks. Each group of raw material storage tanks is connected to a main raw material transport pipeline, which is connected to the feed end of the reactor through the main raw material transport pipeline. In addition to the main raw material transport pipeline, the polytetrafluoroethylene storage tank and the isopropanol storage tank are also provided with raw material transport branch pipelines, which are connected to the catalyst drying module through the raw material transport branch pipelines. The propionaldehyde storage tank, acetaldehyde storage tank, formaldehyde storage tank and ethylene glycol storage tank are all equipped with main nitrogen pipelines in cooperation with the nitrogen module.

[0007] As a further improvement of the present invention, in order to ensure the purity and stability of the raw materials, nitrogen protection effectively prevents the oxidation and deterioration of the raw materials during transportation, improving the quality and consistency of the catalyst. The batching module includes several sets of batching and storage tanks arranged in parallel with the reactor. The batching and storage tanks are divided into chloroplatinic acid storage tanks and sodium borohydride storage tanks. The chloroplatinic acid storage tank is connected to a chloroplatinic acid feeding tank via a pipeline, and the sodium borohydride storage tank is connected to a sodium borohydride feeding tank via a pipeline. A main nitrogen supply pipeline is provided between the chloroplatinic acid storage tank and the sodium borohydride storage tank and the nitrogen storage tank. A nitrogen transport branch pipeline is connected between the main nitrogen supply pipeline and the chloroplatinic acid feeding tank and the sodium borohydride feeding tank. The nitrogen transport branch pipeline includes a main blowing pipeline, an auxiliary blowing pipeline, and a backflush pipeline.

[0008] As a further improvement of the present invention, in order to achieve a continuous and stable supply of chloroplatinic acid and sodium borohydride, both the chloroplatinic acid storage tank and the sodium borohydride storage tank are equipped with main discharge pipelines. The chloroplatinic acid storage tank is connected to the chloroplatinic acid feeding tank through the main discharge pipeline, and the sodium borohydride storage tank is connected to the sodium borohydride feeding tank through the main discharge pipeline. Both the chloroplatinic acid feeding tank and the sodium borohydride feeding tank are equipped with feeding pipelines. The chloroplatinic acid feeding tank is connected to the reaction vessel through the feeding pipeline, and the sodium borohydride feeding tank is connected to the reaction vessel through the feeding pipeline.

[0009] As a further improvement of the present invention, in order to achieve precise feeding and avoid the uncertainty of manual operation, the hydrazine hydrate module includes a hydrazine hydrate storage tank connected to the reactor. The hydrazine hydrate storage tank is connected to a hydrazine hydrate transport pipeline, through which the hydrazine hydrate is quantitatively fed into the reactor.

[0010] As a further improvement of the present invention, in order to realize the recycling of cooling water, reduce water consumption, and maintain a low-pressure environment in the reaction system, the cooling water module includes a raw water main pipeline, which is connected to a condenser and a vacuum assembly. The condenser is equipped with a first raw water transport pipeline, which is used to exchange heat with the reactor. The vacuum assembly includes a water supply pipeline connected to the raw water main pipeline, which is connected to a process water tank. A filter is installed at the front end of the process water tank and connected to the water supply pipeline. The process water tank is equipped with a vacuum pump, a water supply receiving pipeline, and a water supply transport pipeline. The process water tank receives the treated water from the reactor and the catalyst drying module through the water supply receiving pipeline, and then, after being processed by the vacuum pump and the process water tank, it is transported into the reactor through the water supply transport pipeline for cooling and heat exchange.

[0011] As a further improvement of the present invention, in order to provide a uniform and controllable heat source for the reactor, the heating oil module includes a heat transfer oil tank. The heat transfer oil tank is provided with an oil inlet pipe and an oil outlet pipe at both ends. The heat transfer oil tank transports the heat transfer oil into the reactor through the oil inlet pipe and then recovers it through the oil outlet pipe.

[0012] As a further improvement of the present invention, in order to achieve thorough mixing and real-time monitoring of the reaction liquid, avoid liquid leakage, and improve reaction safety, the reaction vessel is equipped with a mixing and stirring impeller inside, and a stepper motor is installed at the top of the reaction vessel. Ultrasonic level gauges and reaction temperature detectors are also installed on both sides of the reaction vessel, and a water-proof and ventilated membrane layer is also installed inside the reaction vessel.

[0013] As a further improvement of the present invention, in order to effectively control the crystallization process of the catalyst, avoid particle sintering, simplify the preparation process of the PEM electrode, and improve production efficiency, the catalyst drying module includes a filtration drying chamber. The filtration drying chamber is connected to the discharge end of the reactor via a pipeline. The filtration drying chamber is also equipped with a return pipeline connected to the reactor. The filtration drying chamber is connected to a cooling water module via a pipeline. An electric heating drying furnace is connected to the discharge end of the filtration drying chamber. A spiral cooling bed is connected to the discharge end of the electric heating drying furnace. The bed is connected to a catalyst finished product storage tank via pipelines. The catalyst finished product storage tank is connected to a catalyst feeding tank via pipelines. A negative pressure return pipeline is also provided between the catalyst feeding tank and the catalyst finished product storage tank. A mixing agitator is connected to the catalyst feeding tank. The catalyst feeding tank also includes a carbon powder storage tank and a carbon powder feeding tank, which are connected to each other via pipelines. The carbon powder feeding tank is connected to the mixing agitator. A spraying machine is connected to the discharge end of the mixing agitator. A hot press and a cold press are subsequently installed after the spraying machine.

[0014] One of the beneficial effects of this invention is reflected in the following aspects:

[0015] Full-process automation and integration: Through the integrated design of the reactor and modules for reducing agents, ingredients, and hydrazine hydrate, fully automated control is achieved from raw material input to catalyst formation. The nitrogen module, through the cooperation of multiple gas storage tanks and the main nitrogen pipeline, provides an inert gas protective environment for the reactor, preventing raw material oxidation. At the same time, the closed-loop circulation system of the cooling water module and the heating oil module precisely controls the reaction temperature, significantly improving the stability and consistency of the preparation process.

[0016] Precise control of process conditions: The raw material module supports the selective use of various reducing agents such as formaldehyde and acetaldehyde, and achieves flexible feeding through a combination of main and branch pipelines; the batching module ensures precise batching of chloroplatinic acid and sodium borohydride through a nitrogen purging system, preventing agglomeration. The mixing and stirring blades inside the reactor work in conjunction with the ultrasonic level gauge to achieve thorough mixing and real-time monitoring of the reaction liquid, further optimizing the reaction conditions.

[0017] Product quality and production efficiency improved: The catalyst drying module effectively controls the catalyst crystallization process and avoids particle sintering through staged drying in a filter drying chamber and an electric heating drying oven, combined with rapid cooling by a spiral cooling bed. Meanwhile, the integrated design of the carbon powder mixing and spraying machine simplifies the PEM electrode preparation process.

[0018] This invention also provides a process for preparing an ultrafine nano-sponge platinum system, the process comprising the following steps:

[0019] Step 1: Select suitable raw materials from ethanol storage tanks, propionaldehyde storage tanks, acetaldehyde storage tanks, formaldehyde storage tanks, ethylene glycol storage tanks, and hydrogen storage tanks according to process requirements; the reducing agent can be one or a combination of two of formaldehyde, acetaldehyde, propionaldehyde, ethylene glycol, ethanol, and hydrogen.

[0020] Step 2: Take out the required amount of chloroplatinic acid from the chloroplatinic acid storage tank and transport it to the reactor through the chloroplatinic acid feed tank; at the same time, take out sodium borohydride from the sodium borohydride storage tank as needed and transport it to the reactor through the sodium borohydride feed tank.

[0021] Step 3: Feed the hydrazine hydrate from the storage tank into the reactor via the hydrazine hydrate transport pipeline in a measured quantity;

[0022] Step 4: Nitrogen gas is introduced into each storage tank and reaction vessel through the nitrogen storage tank in the nitrogen module, via the main nitrogen pipeline and nitrogen transport branch pipeline, to ensure that the system is an inert gas environment and prevent oxidation.

[0023] Step 5: According to the process requirements, select appropriate raw materials and transport them to the reactor through the main raw material transport pipeline. The polytetrafluoroethylene storage tank and the isopropanol storage tank are connected to the catalyst drying module through the raw material transport branch pipeline for anti-sticking or modification in subsequent processing.

[0024] Step 6: The reactor is equipped with mixing and stirring blades, and the speed is precisely controlled by a top stepper motor. Ultrasonic level gauges are installed on both sides of the reactor to monitor the level of the reactants in real time. At the same time, the reaction temperature detector continuously monitors the reaction temperature to ensure that the reaction is carried out under optimal conditions.

[0025] Step 7: Using the heating oil module, the reactor is uniformly heated through a circulation system consisting of a heat transfer oil tank, an inlet oil pipe, and an outlet oil pipe. The temperature is controlled within the range of 100-150℃. The reactor is kept at the set temperature for 2-5 hours to ensure that the reaction proceeds fully and high-quality catalyst particles are generated.

[0026] Step 8: Multiple nitrogen modules are introduced into the reactor and some storage tanks through the main nitrogen pipeline to create an inert atmosphere and prevent the raw materials and products from being oxidized during the reaction.

[0027] Step Nine: After the reaction is complete, the reactor is rapidly cooled using a cooling water module. The main raw water pipeline delivers cooling water to the condenser, which is connected to the reactor via the first raw water transport pipeline. The vacuum assembly, through the water supply pipeline, process water tank, vacuum pump, and other components, recovers and processes the treated water from the reactor and catalyst drying module, and recycles it for cooling.

[0028] Step 10: The reaction product enters the filtration and drying chamber through the discharge end of the reactor, where impurities are removed by a precision filtration device to ensure the purity of the catalyst; the filtered catalyst is then dried in an electric heating drying oven to remove residual moisture.

[0029] Step 11: Mix the dried finished catalyst with carbon powder, isopropanol solution and polytetrafluoroethylene solution in a mixer to form a stable catalyst slurry; use a spraying machine to spray the catalyst slurry onto the Nafion membrane to form a uniform PEM electrode layer.

[0030] Step 12: Add a carbon paper diffusion layer to the PEM electrode to assemble a complete membrane electrode assembly. Test the water electrolysis catalytic performance of the assembled membrane electrode and record the current density data at different voltages.

[0031] Another beneficial effect of the present invention is:

[0032] Flexible and precise raw material selection: Step 1 offers a variety of reducing agents to choose from, which can be flexibly combined according to process requirements to meet different reaction conditions and improve the diversity of product performance.

[0033] The process control is meticulous and comprehensive: Steps two through five ensure the accurate delivery of raw materials to the reactor, while nitrogen is used to create an inert environment to prevent oxidation and ensure the smooth progress of the reaction. Step six utilizes mixing impellers, ultrasonic level gauges, and reaction temperature detectors to precisely control stirring, material level, and temperature during the reaction process, ensuring the reaction proceeds under optimal conditions and improving product quality.

[0034] Stable and reliable reaction conditions: Steps seven and eight precisely control the reaction temperature and atmosphere through the heating oil module and multiple nitrogen modules to ensure a full and stable reaction and generate high-quality catalyst particles.

[0035] Highly efficient and environmentally friendly cooling and water treatment: The cooling water module in step nine achieves rapid cooling, while simultaneously recovering and treating the treated water from the reactor and catalyst drying module, allowing for recycling, reducing costs, and being environmentally friendly.

[0036] The product processing is complete and of high quality: Steps 10 to 12 involve filtering, drying, mixing, spraying, assembling, and performance testing of the reaction products, forming a complete production process that ensures the purity and performance stability of the catalyst, ultimately yielding high-quality membrane electrode assemblies that meet the needs of water electrolysis catalysis applications.

[0037] In operation, this invention first selects suitable raw materials from polytetrafluoroethylene (PTFE), isopropanol, ethanol, propionaldehyde, acetaldehyde, formaldehyde, ethylene glycol, and hydrogen storage tanks according to process requirements. Simultaneously, the required amounts of chloroplatinic acid and sodium borohydride are taken from chloroplatinic acid and sodium borohydride storage tanks, respectively, and transported to the reaction vessel via corresponding feeding tanks. Furthermore, hydrazine hydrate is quantitatively fed from the hydrazine hydrate storage tank to the reaction vessel via a hydrazine hydrate transport pipeline.

[0038] Subsequently, using the nitrogen storage tank in the nitrogen module, nitrogen is introduced into each storage tank and reaction vessel through the main nitrogen pipeline and nitrogen transport branch pipeline to ensure that the system is an inert gas environment and prevent the raw materials and products from being oxidized during the reaction.

[0039] Inside the reactor, the mixing impeller is precisely controlled by a top stepper motor to ensure thorough mixing of the reactants. Simultaneously, a reaction temperature detector continuously monitors the reaction temperature, and an ultrasonic level gauge monitors the material level in real time, ensuring the reaction proceeds under optimal conditions.

[0040] Using a heating oil module, the reactor is uniformly heated through a circulation system consisting of a heat-conducting oil tank, an inlet oil pipeline, and an outlet oil pipeline. The temperature is controlled within the range of 100-150℃. The reactor is kept at the set temperature for 2-5 hours to ensure that the reaction proceeds fully and high-quality catalyst particles are generated.

[0041] After the reaction is complete, the reactor is rapidly cooled using a cooling water module. The reaction products then enter a filtration and drying chamber, where impurities are removed by a precision filtration device, and finally dried in an electrically heated drying oven.

[0042] Finally, the dried finished catalyst was mixed with carbon powder, isopropanol solution, and polytetrafluoroethylene solution in a mixer to form a stable catalyst slurry, which was then sprayed onto a Nafion membrane to form a PEM electrode layer. A carbon paper diffusion layer was added to the PEM electrode, and the assembly was then processed by hot and cold presses to form a complete membrane electrode assembly. The water electrolysis catalytic performance was then tested, and the current density data at different voltages were recorded. Attached Figure Description

[0043] To facilitate understanding by those skilled in the art, the present invention will be further described below with reference to the accompanying drawings:

[0044] Figure 1 This is a structural diagram of the present invention.

[0045] Figure 2 This is sub-view A of the present invention.

[0046] Figure 3 This is sub-view B of the present invention.

[0047] Figure 4 This is a flowchart for the raw materials module.

[0048] Figure 5 This is a flowchart of chloroplatinic acid in the raw materials module.

[0049] Figure 6 This is the overall flowchart for the raw materials module.

[0050] Figure 7 This is a flowchart for cooling water.

[0051] Figure 8 This is a flowchart for heating oil.

[0052] Figure 9 This is sub-flowchart A for the catalyst drying module.

[0053] Figure 10 This is sub-flowchart B for the catalyst drying module.

[0054] The components include: 1. Reactor; 101. Mixing and stirring impeller; 102. Stepper motor; 103. Ultrasonic level gauge; 104. Reaction temperature detector; 2. Raw material module; 201. Raw material storage tank; 202. Polytetrafluoroethylene storage tank; 203. Isopropanol storage tank; 204. Ethanol storage tank; 205. Propionaldehyde storage tank; 206. Acetaldehyde storage tank; 207. Formaldehyde storage tank; 208. Ethylene glycol storage tank; and 209. Hydrogen storage tank. 210 Raw material transport main pipeline, 211 Raw material transport branch pipeline, 3 Batching module, 301 Chloroplatinic acid storage tank, 302 Sodium borohydride storage tank, 303 Chloroplatinic acid feeding tank, 304 Sodium borohydride feeding tank, 305 Main nitrogen feeding pipeline, 4 Hydrazine hydrate module, 401 Hydrazine hydrate storage tank, 402 Hydrazine hydrate transport pipeline, 5 Nitrogen module, 501 Nitrogen storage tank, 502 Main nitrogen pipeline, 5 03 Main blowing pipeline, 504 Auxiliary blowing pipeline, 505 Backflush pipeline, 506 Nitrogen transport branch pipeline, 6 Cooling water module, 601 Raw water main pipeline, 602 Condenser, 603 Vacuum assembly, 604 First raw water transport pipeline, 605 Makeup water pipeline, 606 Process water tank, 607 Makeup water receiving pipeline, 608 Makeup water transport pipeline, 7 Heating oil module, 701 Heat transfer oil tank, 702 Oil inlet pipeline, 703 Oil outlet pipeline, 8 Catalyst drying module, 801 Filter drying chamber, 802 Return material pipeline, 803 Electric heating drying oven, 804 Spiral cooling bed, 805 Catalyst finished product storage tank, 806 Catalyst feeding tank, 807 Negative pressure return material pipeline, 808 Mixer, 809 Carbon powder storage tank, 810 Carbon powder feeding tank, 811 Sprayer, 9 Main unloading pipeline, 10 Feeding pipeline. Detailed Implementation

[0055] To enable those skilled in the art to better understand the technical solutions in this application, the following description is provided in conjunction with the appendix. Figures 1-10The present invention will be further described below. The following embodiments are only used to illustrate the technical solutions of the present invention more clearly, and should not be used to limit the scope of protection of the present invention.

[0056] like Figures 1-10 The system shown is a system for preparing ultrafine nano-sized platinum sponges, comprising a system body, which includes a reaction vessel 1. The feed end of the reaction vessel 1 is equipped with a raw material module 2 and a batching module 3. The feed end of the reaction vessel 1 is also equipped with a hydrazine hydrate module 4. The system body is equipped with multiple nitrogen modules 5. The reaction vessel 1 is also connected to a cooling water module 6 and a heating oil module 7. The reaction vessel 1 is connected to a catalyst drying module 8. The nitrogen modules 5 include several nitrogen storage tanks 501.

[0057] The raw material module 2 includes several groups of raw material storage tanks 201 arranged parallel to the reaction vessel 1. The raw material storage tanks 201 are divided into polytetrafluoroethylene storage tank 202, isopropanol storage tank 203, ethanol storage tank 204, propionaldehyde storage tank 205, acetaldehyde storage tank 206, formaldehyde storage tank 207, ethylene glycol storage tank 208, and hydrogen storage tank 209. Each group of raw material storage tanks 201 is connected to a main raw material transport pipeline 210, and the raw material transport pipeline... Pipeline 210 is connected to the feed end of reactor 1; in addition to the main raw material transport pipeline 210, the polytetrafluoroethylene storage tank 202 and isopropanol storage tank 203 are also provided with a raw material transport branch pipeline 211, which is connected to the catalyst drying module 8 through the raw material transport branch pipeline 211; the propionaldehyde storage tank 205, acetaldehyde storage tank 206, formaldehyde storage tank 207 and ethylene glycol storage tank 208 are all equipped with a main nitrogen pipeline 502 in cooperation with the nitrogen module 5.

[0058] The batching module 3 includes several batching and storage tanks arranged parallel to the reactor 1. The batching and storage tanks are divided into a chloroplatinic acid storage tank 301 and a sodium borohydride storage tank 302. The chloroplatinic acid storage tank 301 is connected to a chloroplatinic acid feeding tank 303 via a pipeline, and the sodium borohydride storage tank 302 is connected to a sodium borohydride feeding tank 304 via a pipeline. A main nitrogen supply pipeline 305 is provided between the chloroplatinic acid storage tank 301 and the sodium borohydride storage tank 302 and the nitrogen storage tank 501. A nitrogen transport branch pipeline 506 is connected between the main nitrogen supply pipeline 305 and the chloroplatinic acid feeding tank 303 and the sodium borohydride feeding tank 304. The nitrogen transport branch pipeline 506 includes a main blowing pipeline 503, an auxiliary blowing pipeline 504, and a backflush pipeline 505.

[0059] Both the chloroplatinic acid storage tank 301 and the sodium borohydride storage tank 302 are equipped with main discharge pipelines 9. The chloroplatinic acid storage tank 301 is connected to the chloroplatinic acid feeding tank 303 through the main discharge pipeline 9, and the sodium borohydride storage tank 302 is connected to the sodium borohydride feeding tank 304 through the main discharge pipeline 9. Both the chloroplatinic acid feeding tank 303 and the sodium borohydride feeding tank 304 are equipped with feeding pipelines 10. The chloroplatinic acid feeding tank 303 is connected to the reaction vessel 1 through the feeding pipeline 10, and the sodium borohydride feeding tank 304 is connected to the reaction vessel 1 through the feeding pipeline 10.

[0060] The hydrazine hydrate module 4 includes a hydrazine hydrate storage tank 401 connected to the reactor 1. The hydrazine hydrate storage tank 401 is connected to a hydrazine hydrate transport pipeline 402, through which hydrazine hydrate is quantitatively fed into the reactor 1.

[0061] The cooling water module 6 includes a raw water main pipeline 601, which is connected to a condenser 602 and a vacuum assembly 603. The condenser 602 is equipped with a first raw water transport pipeline 604, which is used to exchange heat with the reactor 1. The vacuum assembly 603 includes a water supply pipeline 605 connected to the raw water main pipeline 601. The water supply pipeline 605 is connected to a process water tank 606. The process water tank 606 has a filter at its front end, which is connected to the water supply pipeline 605. The process water tank 606 is equipped with a vacuum pump, a water supply receiving pipeline 607, and a water supply transport pipeline 608. The process water tank 606 receives the processed water from the reactor 1 and the catalyst drying module 8 through the water supply receiving pipeline 607, and then, after being processed by the vacuum pump and the process water tank 606, it is transported into the reactor 1 through the water supply transport pipeline 608 for cooling and heat exchange.

[0062] The heating oil module 7 includes a heat transfer oil tank 701. The heat transfer oil tank 701 is provided with an oil inlet pipe 702 and an oil outlet pipe 703 at both ends. The heat transfer oil tank 701 transports the heat transfer oil into the reaction vessel 1 through the oil inlet pipe 702 and then recovers it through the oil outlet pipe 703.

[0063] The reactor 1 is equipped with a mixing and stirring blade 101 inside, and a stepper motor 102 is installed on the top of the reactor 1. An ultrasonic level gauge 103 and a reaction temperature detector 104 are also installed on both sides of the reactor 1. A water-proof and ventilated membrane layer is also installed inside the reactor 1.

[0064] The catalyst drying module 8 includes a filtration drying chamber 801, which is connected to the discharge end of the reactor 1 via a pipeline. The filtration drying chamber 801 also has a return pipeline 802 connected to the reactor 1. The filtration drying chamber 801 is connected to a cooling water module 6 via a pipeline. An electric heating drying furnace 803 is connected to the discharge end of the filtration drying chamber 801. A spiral cooling bed 804 is connected to the discharge end of the electric heating drying furnace 803. The spiral cooling bed 804 is connected to a catalyst finished product storage tank 805 via a pipeline. The catalyst finished product storage tank 805 is connected to... A catalyst feeding tank 806 is connected and configured, and a negative pressure return pipeline 807 is also provided between the catalyst feeding tank 806 and the catalyst finished product storage tank 805. A mixing agitator 808 is connected to the catalyst feeding tank 806. The catalyst feeding tank 806 also includes a carbon powder storage tank 809 and a carbon powder feeding tank 810. The carbon powder storage tank 809 and the carbon powder feeding tank 810 are connected by a pipeline. The carbon powder feeding tank 810 is connected to the mixing agitator 808. A spraying machine 811 is connected to the discharge end of the mixing agitator 808. A hot press and a cold press are configured after the spraying machine 811.

[0065] A process for preparing an ultrafine nano-sponge platinum system, the process comprising the following steps:

[0066] Step 1: Select suitable raw materials from ethanol storage tank 204, propionaldehyde storage tank 205, acetaldehyde storage tank 206, formaldehyde storage tank 207, ethylene glycol storage tank 208, and hydrogen storage tank 209 according to process requirements; the reducing agent can be one or a combination of two of formaldehyde, acetaldehyde, propionaldehyde, ethylene glycol, ethanol, and hydrogen.

[0067] Step 2: Take out the required amount of chloroplatinic acid from the chloroplatinic acid storage tank 301 and transport it to the reactor 1 through the chloroplatinic acid feeding tank 303; at the same time, take out sodium borohydride from the sodium borohydride storage tank 302 as needed and transport it to the reactor 1 through the sodium borohydride feeding tank 304.

[0068] Step 3: Feed hydrazine hydrate from storage tank 401 into reactor 1 via hydrazine hydrate transport pipeline 402 in a measured amount;

[0069] Step 4: Nitrogen gas is introduced into each storage tank and reaction vessel 1 through the nitrogen storage tank 501 in nitrogen module 5, the main nitrogen pipeline 502 and the nitrogen transport branch pipeline 506 to ensure that the system is an inert gas environment and prevent oxidation.

[0070] Step 5: According to the process requirements, select appropriate raw materials and transport them to the reactor 1 through the main raw material transport pipeline 210. The polytetrafluoroethylene storage tank 202 and the isopropanol storage tank 203 are connected to the catalyst drying module 8 through the raw material transport branch pipeline 211 for anti-sticking or modification in subsequent processing.

[0071] Step 6: The reactor 1 is equipped with a mixing and stirring blade 101, and the rotation speed is precisely controlled by the top stepper motor 102. Ultrasonic level gauges 103 are installed on both sides of the reactor 1 to monitor the level of the reactants in real time. At the same time, the reaction temperature detector 104 continuously monitors the reaction temperature to ensure that the reaction is carried out under the best conditions.

[0072] Step 7: Using the heating oil module 7, the reaction vessel 1 is uniformly heated through the circulation system consisting of the heat transfer oil tank 701, the oil inlet pipe 702 and the oil outlet pipe 703. The temperature is controlled within the range of 100-150℃. The reaction vessel 1 is kept at the set temperature for 2-5 hours to ensure that the reaction proceeds fully and high-quality catalyst particles are generated.

[0073] Step 8: Multiple nitrogen modules 5 introduce nitrogen into the reactor 1 and some storage tanks through the main nitrogen pipeline 502 to create an inert atmosphere and prevent the raw materials and products from being oxidized during the reaction.

[0074] Step 9: After the reaction is completed, the reactor 1 is rapidly cooled by the cooling water module 6. The raw water main pipeline 601 delivers cooling water to the condenser 602, which is connected to the reactor 1 through the first raw water transport pipeline 604; the vacuum assembly 603 recovers and processes the treated water from the reactor 1 and the catalyst drying module 8 through the water supply pipeline 605, the process water tank 606, the vacuum pump, and other components, and recycles it for cooling.

[0075] Step 10: The reaction product enters the filtration and drying chamber 801 through the discharge end of the reactor 1. Impurities are removed by a precision filtration device to ensure the purity of the catalyst. The filtered catalyst enters the electric heating drying oven 803 for drying to remove residual moisture.

[0076] Step 11: The dried finished catalyst is mixed with carbon powder, isopropanol solution and polytetrafluoroethylene solution in a mixer 808 to form a stable catalyst slurry; the catalyst slurry is sprayed onto the Nafion membrane using a sprayer 811 to form a uniform PEM electrode layer.

[0077] Step 12: Add a carbon paper diffusion layer to the PEM electrode to assemble a complete membrane electrode assembly. Test the water electrolysis catalytic performance of the assembled membrane electrode and record the current density data at different voltages.

[0078] In operation, this invention first selects suitable raw materials from ethanol storage tank 204, propionaldehyde storage tank 205, acetaldehyde storage tank 206, formaldehyde storage tank 207, ethylene glycol storage tank 208, and hydrogen storage tank 209 according to process requirements. Simultaneously, the required amounts of chloroplatinic acid and sodium borohydride are taken from chloroplatinic acid storage tank 301 and sodium borohydride storage tank 302, respectively, and transported to reactor 1 via corresponding feed tanks. Furthermore, hydrazine hydrate is quantitatively fed from hydrazine hydrate storage tank 401 to reactor 1 via hydrazine hydrate transport pipeline 402.

[0079] Subsequently, using the nitrogen storage tank 501 in the nitrogen module 5, nitrogen is introduced into each storage tank and the reaction vessel 1 through the main nitrogen pipeline 502 and the nitrogen transport branch pipeline 506 to ensure that the system is an inert gas environment and prevent the raw materials and products from being oxidized during the reaction.

[0080] Inside the reactor 1, the mixing impeller 101 is precisely controlled by a top stepper motor 102 to ensure thorough mixing of the reactants. Simultaneously, a reaction temperature detector 104 continuously monitors the reaction temperature, and an ultrasonic level gauge 103 monitors the material level in real time, ensuring the reaction proceeds under optimal conditions.

[0081] Using the heating oil module 7, the reaction vessel 1 is uniformly heated through a circulation system consisting of the heat transfer oil tank 701, the oil inlet pipe 702, and the oil outlet pipe 703. The temperature is controlled within the range of 100-150℃. The reaction vessel 1 is kept at the set temperature for 2-5 hours to ensure that the reaction proceeds fully and high-quality catalyst particles are generated.

[0082] After the reaction is complete, the reactor 1 is rapidly cooled by the cooling water module 6. The reaction product then enters the filtration and drying chamber 801, where impurities are removed by a precision filtration device, and is then dried in the electric heating drying oven 803.

[0083] Finally, the dried finished catalyst was mixed with carbon powder, isopropanol solution, and polytetrafluoroethylene solution in a mixer 808 to form a stable catalyst slurry, which was then sprayed onto a Nafion membrane to form a PEM electrode layer. A carbon paper diffusion layer was added to the PEM electrode, and the assembly was then processed by a hot press and a cold press to form a complete membrane electrode assembly. The water electrolysis catalytic performance was then tested, and the current density data at different voltages were recorded. Example 1

[0084] Weigh 2.63 g of chloroplatinic acid, 6 mL of formaldehyde, and 3 g of potassium hydroxide. Dissolve them in water and pour the solution into a high-pressure reactor. Set the internal reaction temperature of the high-pressure reactor to 100°C. Using the heating oil module 7, the reactor 1 is uniformly heated through a circulation system consisting of a heat-conducting oil tank 701, an oil inlet pipe 702, and an oil outlet pipe 703. The temperature is maintained at 100°C and the reaction continues for 2 hours at 100°C. After the reaction, the reactor 1 is rapidly cooled by the cooling water module 6. The reaction product then enters the filtration and drying chamber 801, where impurities are removed by a precision filter and the product is dried in an electric heating drying oven 803. The dried catalyst is mixed with carbon powder, isopropanol solution, and polytetrafluoroethylene solution in a mixer 808 to form a stable catalyst slurry. This slurry is then sprayed onto a Nafion membrane to form a PEM electrode layer, achieving a maximum performance of 1 A / cm² and a voltage of 2.3 V. Example 2

[0085] Weigh 2.63 g of chloroplatinic acid, 6 mL of formaldehyde, and 3 g of potassium hydroxide. Dissolve them in water and pour the solution into a high-pressure reactor. Set the internal reaction temperature of the high-pressure reactor to 120°C. Using the heating oil module 7, the reactor 1 is uniformly heated through a circulation system consisting of a heat-conducting oil tank 701, an oil inlet pipe 702, and an oil outlet pipe 703. Maintain the temperature at 120°C and continue the reaction at 120°C for 2 hours. After the reaction, the reactor 1 is rapidly cooled by the cooling water module 6. The reaction product then enters the filtration and drying chamber 801, where impurities are removed by a precision filter and the product is dried in an electric heating drying oven 803. The dried catalyst is mixed with carbon powder, isopropanol solution, and polytetrafluoroethylene solution in a mixer 808 to form a stable catalyst slurry. This slurry is then sprayed onto a Nafion membrane to form a PEM electrode layer, achieving a maximum performance of 1.1 A / cm² and a voltage of 2.25 V. Example 3

[0086] Weigh 2.63 g of chloroplatinic acid, 6 mL of formaldehyde, and 3 g of potassium hydroxide. Dissolve them in water and pour the solution into a high-pressure reactor. Set the internal reaction temperature of the high-pressure reactor to 130°C. Using the heating oil module 7, the reactor 1 is uniformly heated through a circulation system consisting of a heat-conducting oil tank 701, an oil inlet pipe 702, and an oil outlet pipe 703. Maintain the temperature at 130°C and continue the reaction at 130°C for 2 hours. After the reaction, the reactor 1 is rapidly cooled by the cooling water module 6. The reaction product then enters the filtration and drying chamber 801, where impurities are removed by a precision filter and the product is dried in an electric heating drying oven 803. The dried catalyst is mixed with carbon powder, isopropanol solution, and polytetrafluoroethylene solution in a mixer 808 to form a stable catalyst slurry. This slurry is then sprayed onto a Nafion membrane to form a PEM electrode layer, achieving a maximum performance of 1.15 A / cm² and a voltage of 2.2 V.

[0087] This invention is not limited to the above embodiments. Based on the technical solutions disclosed in this invention, those skilled in the art can make some substitutions and modifications to some of the technical features without creative effort, and these substitutions and modifications are all within the protection scope of this invention.

Claims

1. A system for preparing ultrafine nano-sized platinum sponges, comprising a system body, characterized in that, The system body includes a reactor (1), and the feed end of the reactor (1) is equipped with a raw material module (2) and a batching module (3). The feed end of the reactor (1) is also equipped with a hydrazine hydrate module (4). The system body is equipped with multiple nitrogen modules (5). The reactor (1) is also connected to a cooling water module (6) and a heating oil module (7). The reactor (1) is connected to a catalyst drying module (8). The nitrogen module (5) includes several nitrogen storage tanks (501). The raw material module (2) includes several groups of raw material storage tanks (201) arranged in parallel with the reactor (1). The raw material storage tanks (201) are divided into polytetrafluoroethylene storage tank (202), isopropanol storage tank (203), ethanol storage tank (204), propionaldehyde storage tank (205), acetaldehyde storage tank (206), formaldehyde storage tank (207), ethylene glycol storage tank (208), and hydrogen storage tank (209). Each group of raw material storage tanks (201) is connected to a main raw material transport pipeline (210) and transported through the main raw material transport pipeline. The pipeline (210) is connected to the feed end of the reactor (1); the polytetrafluoroethylene storage tank (202) and the isopropanol storage tank (203) are provided with a raw material transport branch pipeline (211) in addition to the main raw material transport pipeline (210), and are connected to the catalyst drying module (8) through the raw material transport branch pipeline (211); the propionaldehyde storage tank (205), acetaldehyde storage tank (206), formaldehyde storage tank (207) and ethylene glycol storage tank (208) are all provided with a main nitrogen pipeline (502) in cooperation with the nitrogen module (5); The batching module (3) includes several batching and storage tanks arranged in parallel with the reactor (1). The batching and storage tanks are divided into a chloroplatinic acid storage tank (301) and a sodium borohydride storage tank (302). The chloroplatinic acid storage tank (301) is connected to a chloroplatinic acid feeding tank (303) through a pipeline. The sodium borohydride storage tank (302) is connected to a sodium borohydride feeding tank (304) through a pipeline. A nitrogen feeding main pipeline (305) is provided between the chloroplatinic acid storage tank (301) and the sodium borohydride storage tank (302) and the nitrogen storage tank (501). A nitrogen transport branch pipeline (506) is provided between the nitrogen feeding main pipeline (305) and the chloroplatinic acid feeding tank (303) and the sodium borohydride feeding tank (304). The hydrazine hydrate module (4) includes a hydrazine hydrate storage tank (401) connected to the reactor (1). The hydrazine hydrate storage tank (401) is connected to a hydrazine hydrate transport pipeline (402), and the hydrazine hydrate transport pipeline (402) feeds a quantitative amount of hydrazine hydrate into the reactor (1). The cooling water module (6) includes a raw water main pipeline (601), which is connected to a condenser (602) and a vacuum assembly (603). The condenser (602) is equipped with a first raw water transport pipeline (604) and exchanges heat with the reactor (1) through the first raw water transport pipeline (604). The vacuum assembly (603) includes a water supply pipeline (605) connected to the raw water main pipeline (601), and the water supply pipeline (605) is connected to a process water tank (606). The heating oil module (7) includes a heat transfer oil tank (701), and an oil inlet pipe (702) and an oil outlet pipe (703) are respectively provided at both ends of the heat transfer oil tank (701). The reactor (1) is equipped with a mixing and stirring blade (101) inside, and a stepper motor (102) is installed on the top of the reactor (1). An ultrasonic level gauge (103) and a reaction temperature detector (104) are also installed on both sides of the reactor (1). The catalyst drying module (8) includes a filtration drying chamber (801), which is connected to the discharge end of the reactor (1) via a pipeline. The filtration drying chamber (801) also has a return pipeline (802) connected to the reactor (1). The filtration drying chamber (801) is connected to a cooling water module (6) via a pipeline. An electric heating drying furnace (803) is connected to the discharge end of the filtration drying chamber (801). A spiral cooling bed (804) is connected to the discharge end of the electric heating drying furnace (803). The spiral cooling bed (804) is connected to a catalyst finished product storage tank (805) via a pipeline. The catalyst finished product storage tank (805) is connected to... A catalyst feeding tank (806) is connected and a negative pressure return pipeline (807) is also provided between the catalyst feeding tank (806) and the catalyst finished product storage tank (805). A mixing agitator (808) is connected to the catalyst feeding tank (806). The catalyst feeding tank (806) also includes a carbon powder storage tank (809) and a carbon powder feeding tank (810). The carbon powder storage tank (809) and the carbon powder feeding tank (810) are connected by a pipeline. The carbon powder feeding tank (810) is connected to the mixing agitator (808). A spraying machine (811) is connected to the discharge end of the mixing agitator (808). A hot press and a cold press are provided after the spraying machine (811).

2. The system for preparing ultrafine nano-sponge platinum according to claim 1, characterized in that, The nitrogen transport branch pipeline (506) includes a main blowing pipeline (503), an auxiliary blowing pipeline (504), and a backflush pipeline (505); Both the chloroplatinic acid storage tank (301) and the sodium borohydride storage tank (302) are equipped with a main discharge pipeline (9). The chloroplatinic acid storage tank (301) is connected to the chloroplatinic acid feeding tank (303) through the main discharge pipeline (9). The sodium borohydride storage tank (302) is connected to the sodium borohydride feeding tank (304) through the main discharge pipeline (9). Both the chloroplatinic acid feeding tank (303) and the sodium borohydride feeding tank (304) are equipped with a feeding pipeline (10). The chloroplatinic acid feeding tank (303) is connected to the reactor (1) through the feeding pipeline (10). The sodium borohydride feeding tank (304) is connected to the reactor (1) through the feeding pipeline (10).

3. The system for preparing ultrafine nano-sponge platinum according to claim 1, characterized in that, The process water tank (606) is equipped with a filter at the front end and connected to the water supply pipeline (605). The process water tank (606) is equipped with a vacuum pump, a water supply receiving pipeline (607) and a water supply transport pipeline (608). The process water tank (606) receives the processed water from the reactor (1) and the catalyst drying module (8) through the water supply receiving pipeline (607), and then transports it into the reactor (1) for cooling and heat exchange after being processed by the vacuum pump and the process water tank (606) through the water supply transport pipeline (608).

4. The system for preparing ultrafine nano-sponge platinum according to claim 1, characterized in that, The heat transfer oil tank (701) transports heat transfer oil into the reactor (1) through the oil inlet pipe (702) and then recovers it through the oil outlet pipe (703).

5. The system for preparing ultrafine nano-sponge platinum according to claim 1, characterized in that, The interior of the reactor (1) is also provided with a water-proof and ventilated membrane layer.

6. The process for preparing ultrafine nano-sized platinum sponges according to claim 1, characterized in that, The process includes the following steps: Step 1: Based on process requirements, select suitable raw materials as reducing agents from ethanol storage tank (204), propionaldehyde storage tank (205), acetaldehyde storage tank (206), formaldehyde storage tank (207), ethylene glycol storage tank (208), and hydrogen storage tank (209); the reducing agent is one or a combination of two of formaldehyde, acetaldehyde, propionaldehyde, ethylene glycol, ethanol, and hydrogen. Step 2: Take out the required amount of chloroplatinic acid from the chloroplatinic acid storage tank (301) and transport it to the reactor (1) through the chloroplatinic acid feed tank (303); at the same time, take out sodium borohydride from the sodium borohydride storage tank (302) as needed and transport it to the reactor (1) through the sodium borohydride feed tank (304). Step 3: Feed hydrazine hydrate from the storage tank (401) into the reactor (1) via the hydrazine hydrate transport pipeline (402) in a measured amount; Step 4: Nitrogen gas is introduced into each storage tank and reaction vessel (1) through the nitrogen storage tank (501) in the nitrogen module (5), the main nitrogen pipeline (502) and the nitrogen transport branch pipeline (506) to ensure that the system is an inert gas environment and prevent oxidation; Step 5: According to the process requirements, select appropriate raw materials and transport them to the reactor (1) through the main raw material transport pipeline (210). The polytetrafluoroethylene storage tank (202) and the isopropanol storage tank (203) are connected to the catalyst drying module (8) through the raw material transport branch pipeline (211) for anti-sticking or modification in subsequent processing. Step 6: The reactor (1) is equipped with mixing and stirring blades (101), and the speed is precisely controlled by the top stepper motor (102). Ultrasonic level gauges (103) are installed on both sides of the reactor (1) to monitor the level of the reactants in real time. At the same time, the reaction temperature detector (104) continuously monitors the reaction temperature to ensure that the reaction is carried out under the best conditions. Step 7: Using the heating oil module (7), the reactor (1) is uniformly heated through the circulation system consisting of the heat transfer oil tank (701), the oil inlet pipe (702) and the oil outlet pipe (703). The temperature is controlled within the range of 100-150℃. The reactor (1) is kept at the set temperature for 2-5 hours to ensure that the reaction proceeds fully and high-quality catalyst particles are generated. Step 8: Multiple nitrogen modules (5) introduce nitrogen into the reactor (1) and some storage tanks through the main nitrogen pipeline (502) to create an inert atmosphere and prevent the raw materials and products from being oxidized during the reaction. Step 9: After the reaction is completed, the reactor (1) is rapidly cooled by the cooling water module (6); the raw water main pipeline (601) transports the cooling water to the condenser (602), and connects it to the reactor (1) through the first raw water transport pipeline (604); the vacuum assembly (603) recovers and processes the processed water of the reactor (1) and the catalyst drying module (8) through the water supply pipeline (605), the process water tank (606), and the vacuum pump, and recirculates it for cooling; Step 10: The reaction product enters the filtration and drying chamber (801) through the discharge end of the reactor (1), where impurities are removed by a precision filtration device to ensure the purity of the catalyst; the filtered catalyst enters the electric heating drying oven (803) for drying to remove residual moisture; Step 11: The dried finished catalyst is mixed with carbon powder, isopropanol solution and polytetrafluoroethylene solution in a mixer (808) to form a stable catalyst slurry; the catalyst slurry is sprayed onto the Nafion membrane using a sprayer (811) to form a uniform PEM electrode layer. Step 12: Add a carbon paper diffusion layer to the PEM electrode to assemble a complete membrane electrode assembly. Test the water electrolysis catalytic performance of the assembled membrane electrode and record the current density data at different voltages.

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