A high-purity hydrogen production device with adsorption purification and palladium membrane purification

Abstract

This application provides a high-purity hydrogen preparation device with adsorption purification and palladium membrane purification. All components are integrated into a rigid cabinet, eliminating external cascaded high-pressure pipelines, reducing leakage points, improving system rigidity and safety, and facilitating explosion-proof and pressure vessel certification. The device employs a three-section structure: gas-liquid separator – adsorption purification unit – high-temperature palladium membrane. The adsorption unit uses a molecular sieve + palladium catalyst composite filling, combining deep dehydration and catalytic deoxygenation functions, providing a dry, oxygen-free pre-protection environment for the palladium membrane, significantly extending its service life. The pressure-stabilizing isolation section forms a "pressure-stabilizing isolation zone," effectively absorbing pressure fluctuations during switching and preventing damage to the palladium membrane due to pressure alternation. An integrated protection circuit quickly evacuates the palladium membrane cavity in case of abnormal shutdown or gas supply interruption, physically blocking air contact and completely eliminating the risk of high-temperature oxidation.

Description

Technical Field

[0001] This invention relates to the field of hydrogen production technology, and more specifically, to a high-purity hydrogen production apparatus with adsorption purification and palladium membrane purification functions. Background Technology

[0002] Existing high-purity hydrogen production systems are typically physically divided into two independently operating units: one is a pre-processing unit responsible for electrolytic hydrogen production and PSA initial purification, and the other is a separate post-processing unit for deep palladium membrane purification. Connecting these two units on-site via external high-pressure pipelines, flanges, or joints has the following drawbacks: Poor safety: External pipeline connections are prone to air infiltration due to pressure fluctuations, forming flammable and explosive mixtures, posing a risk of explosion and fire; at the same time, the infiltrated oxygen and water vapor will accelerate the oxidation of the palladium film and shorten its service life. Severe damage from pressure fluctuations: The front-end process generates periodic pressure fluctuations during switching and regeneration. The back-end palladium membrane unit lacks coordinated control and is subjected to pressure shocks for a long time, which can easily lead to fatigue tearing or structural deformation of the palladium membrane. Controlling the split and protecting against lag: The separate equipment is controlled independently, and communication delays occur in emergency situations, causing the palladium film to be exposed to air at high temperatures, increasing the risk of oxidation. The dispersed structure makes certification difficult: external piping increases the number of leakage points, the system has poor rigidity, and it is difficult to pass the stringent explosion-proof and pressure vessel certifications.

[0003] Therefore, we have made improvements and proposed a high-purity hydrogen preparation device with adsorption purification and palladium membrane purification. Summary of the Invention

[0004] This invention provides a high-purity hydrogen preparation device with adsorption purification and palladium membrane purification, including an integrated rigid cabinet and integrated within the integrated rigid cabinet: a front-end hydrogen production and dehydration assembly, a middle adsorption purification unit, a tail-end high-temperature palladium membrane purification unit, and a protection assembly; The outlet of the front-end hydrogen production and dehydration assembly is connected to the inlet of the central adsorption and purification unit. The outlet of the central adsorption and purification unit is connected to the inlet of the tail-end high-temperature palladium membrane purification unit through a voltage-stabilizing isolation pipe section, forming a three-section series integrated structure. The protection assembly includes a protection circuit connected to the tail-end high-temperature palladium membrane purification unit.

[0005] As a preferred technical solution of this application, the front-end hydrogen production and dehydration assembly includes a hydrogen production device and a gas-liquid separator connected to the wet hydrogen output end of the hydrogen production device. The gas-liquid separator is equipped with a wire mesh demister. The gas-liquid separator integrates a float level gauge and a solenoid valve. The float level gauge and the solenoid valve constitute a first-level automated physical dehydration unit. The wet hydrogen output end of the hydrogen production equipment is connected in sequence to the gas-liquid separator by pressure sensor three, one-way valve one, pressure sensor two, and radiator two.

[0006] As a preferred technical solution of this application, the gas-liquid separator is further connected to a second safety valve and a third solenoid valve, with the second safety valve and the third solenoid valve connected in parallel and connected to a water seal.

[0007] As a preferred technical solution of this application, the front-end hydrogen production and dehydration assembly further includes a water tank. The water tank is connected to the water inlet of the hydrogen production equipment by a manual ball valve, a safety valve, a water pump, a pressure sensor, a conductivity transmitter, and a flow meter. The water outlet of the hydrogen production equipment is connected to the water tank to form a water electrolysis transmission circuit.

[0008] As a preferred technical solution of this application, a manual ball valve 2 is connected between the water pump 1 and the pressure sensor 1. The manual ball valve 2 is connected to a drain end. The drain end is connected to a solenoid valve 4. The solenoid valve 4 is connected to a water seal device. The water seal device is connected to the solenoid valve 2, and the water seal device is also connected to a vent end.

[0009] As a preferred technical solution of this application, the central adsorption purification unit is a pressure swing adsorption device, including a drying tower one and a drying tower two connected in parallel, both of which are filled with a composite medium of molecular sieve and palladium catalyst. The drying tower 1 is connected to solenoid valve 5 and solenoid valve 6, the drying tower 2 is connected to solenoid valve 7 and solenoid valve 8, solenoid valve 5 and solenoid valve 7 are connected to the gas-liquid separator through a pipeline; solenoid valve 6 and solenoid valve 8 are connected to the water seal device through a pipeline. The drying tower 1 is connected to pressure sensor 4 and one-way valve 2. One-way valve 3 is connected between one-way valve 2 and pressure sensor 4. The drying tower 2 is connected to pressure sensor 5 and one-way valve 5. One-way valve 4 is connected between one-way valve 5 and pressure sensor 5. Manual needle valve 1 is connected between one-way valve 4 and one-way valve 3. One-way valve 2, manual needle valve 1 and one-way valve 5 are connected to each other.

[0010] As a preferred technical solution of this application, the pressure stabilizing isolation pipe section includes a back pressure valve, a pressure reducing valve, a one-way valve, and a pressure sensor connected in series between the manual needle valve and the tail-end high-temperature palladium membrane purification unit.

[0011] As a preferred technical solution of this application, the tail-end high-temperature palladium membrane purification unit includes a palladium membrane tube one and a palladium membrane tube two, and a temperature transmitter two is connected between the palladium membrane tube one and the pressure sensor six. The palladium membrane tube 1 and the water seal are connected in sequence by a check valve 7, a solenoid valve 10, a manual needle valve 2, a float flow meter, and a check valve 8.

[0012] As a preferred technical solution of this application, a temperature transmitter is connected between the palladium membrane tube 1 and the palladium membrane tube 2. The palladium membrane tube 2 is provided with a hydrogen discharge end, and a pressure sensor 7, a one-way valve 9, a solenoid valve 12, a dew point meter and a one-way valve 10 are connected in sequence between the palladium membrane tube 2 and the hydrogen discharge end; the solenoid valve 12 is also connected to the water seal and the vent end. A solenoid valve thirteen is connected between the pressure sensor seven and the one-way valve nine. The palladium diaphragm tube one is also connected to a solenoid valve eleven. The solenoid valve thirteen is connected to the solenoid valve eleven and is connected to the protection circuit.

[0013] As a preferred technical solution of this application, the protection circuit includes a vacuum pump, which is connected to solenoid valve thirteen and solenoid valve eleven, and the vacuum pump is also connected to a vacuum port.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows: In the scheme of this application: 1. All components in this application are integrated into a single rigid cabinet, eliminating external cascaded high-pressure pipelines, reducing leakage points, improving system rigidity and safety, and facilitating explosion-proof and pressure vessel certification; 2. Through the three-section structure of "gas-liquid separator - adsorption purification unit - high temperature palladium membrane", the adsorption unit adopts molecular sieve + palladium catalyst composite filling, which has both deep dehydration and catalytic deoxygenation functions, providing a dry and oxygen-free pre-protection environment for the palladium membrane, significantly extending its service life. 3. The installation of the pressure stabilizing isolation section can form a "pressure stabilizing isolation zone", effectively absorbing pressure fluctuations caused by switching and preventing the palladium membrane from being damaged due to pressure alternation; 4. An integrated protection circuit quickly evacuates the palladium membrane chamber in case of abnormal shutdown or gas supply interruption, physically blocking air contact and completely eliminating the risk of high-temperature oxidation. Attached Figure Description

[0015] Figure 1 A schematic diagram of the high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification provided in this application; Figure 2 A schematic diagram of the water tank, hydrogen production equipment, and gas-liquid separator provided in this application; Figure 3 A partial schematic diagram of the high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification provided in this application; Figure 4 This is a schematic diagram of drying tower one and drying tower two provided in this application.

[0016] The image shows: 1. Integrated rigid cabinet; 101. Hydrogen leak sensor 1; 102. Exhaust fan; 2. Hydrogen production equipment; 3. Water tank; 301. Manual ball valve 1; 302. Safety valve 1; 303. Water pump 1; 304. Manual ball valve 2; 305. Pressure sensor 1; 306. Conductivity transmitter; 307. Flow meter 1; 308. Drain end; 309. Water pump 2; 310. Radiator 1; 311. Filter 1; 312. Filter 2; 313. Hydrogen leak sensor 2; 314. Temperature transmitter 1; 315. Float level gauge 1; 316. Oxygen exhaust fan; 317. Oxygen exhaust end; 318. Water supply end; 319. Solenoid valve 1; 4. Gas-liquid separator; 401. Radiator II; 402. Pressure sensor II; 403. Check valve I; 404. Pressure sensor III; 405. Solenoid valve II; 406. Safety valve II; 407. Solenoid valve III; 5. Water seal device; 501. Solenoid valve four; 502. Vent end; 6. Drying Tower 1; 601. Drying Tower 2; 602. Pressure Sensor 4; 603. Check Valve 2; 604. Check Valve 3; 605. Pressure Sensor 5; 606. Check Valve 4; 607. Check Valve 5; 608. Manual Needle Valve 1; 609. Back Pressure Valve; 610. Drain End; 611. Solenoid Valve 5; 612. Solenoid Valve 6; 613. Solenoid Valve 7; 614. Solenoid Valve 8; 615. Solenoid Valve 9; 616. Pressure Reducing Valve; 617. Check Valve 6; 618. Pressure Sensor 6; 7. Palladium membrane tube 1; 701. Palladium membrane tube 2; 702. Temperature transmitter 2; 703. Check valve 7; 704. Solenoid valve 10; 705. Manual needle valve 2; 706. Float flowmeter; 707. Check valve 8; 708. Temperature transmitter 3; 709. Solenoid valve 11; 710. Pressure sensor 7; 711. Check valve 9; 712. Solenoid valve 12; 713. Dew point meter; 714. Check valve 10; 715. Hydrogen discharge end; 716. Solenoid valve 13; 8. Vacuum pump; 801. Vacuum port. Detailed Implementation

[0017] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.

[0018] It should be noted that, unless otherwise specified, the embodiments and features and technical solutions in the present invention can be combined with each other.

[0019] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0020] Example 1, please refer to Figures 1-4 A high-purity hydrogen production device with adsorption purification and palladium membrane purification includes an integrated rigid cabinet 1 and integrated within the integrated rigid cabinet 1: a front-end hydrogen production and dehydration assembly, a middle adsorption purification unit, a tail-end high-temperature palladium membrane purification unit, and a protection assembly. The outlet of the front-end hydrogen production and dehydration assembly is connected to the inlet of the central adsorption purification unit. The outlet of the central adsorption purification unit is connected to the inlet of the tail-end high-temperature palladium membrane purification unit through a pressure-stabilizing isolation pipe section, forming a three-section series integrated structure. The setting of the pressure-stabilizing isolation pipe section can buffer and stabilize the gas pressure output by the central unit, providing stable working conditions for the tail-end high-temperature palladium membrane purification unit which is sensitive to pressure fluctuations, and protecting the expensive palladium membrane. The protection assembly includes a protection circuit connected to the tail-end high-temperature palladium membrane purification unit.

[0021] The integrated rigid cabinet 1 also integrates an exhaust fan 102 and a hydrogen leak sensor 101. The integrated rigid cabinet 1 integrates an exhaust fan 102 and a hydrogen leak sensor 101 to form an active safety monitoring system. Once the hydrogen leak sensor 101 detects a hydrogen leak, it can link the exhaust fan to force ventilation and dilute the hydrogen, and trigger an alarm or shutdown, which significantly improves the intrinsic safety level of the device and meets strict explosion-proof and safety standards. Furthermore, the front-end hydrogen production and dehydration assembly includes a hydrogen production device 2 and a gas-liquid separator 4 connected to the wet hydrogen output end of the hydrogen production device 2. The gas-liquid separator 4 is equipped with a wire mesh demister and integrates a float level gauge 2 and a solenoid valve 2 405. The float level gauge 2 and the solenoid valve 2 405 constitute a first-level automated physical dehydration unit. The wet hydrogen produced by the hydrogen production device 2 first enters the gas-liquid separator 4 and undergoes preliminary gas-liquid separation using the wire mesh demister to remove most of the liquid water. The linkage control between the float level gauge 2 and the solenoid valve 2 405 enables the automatic discharge of condensate in the gas-liquid separator 4.

[0022] The hydrogen production equipment 2 is preferably a PEM electrolyzer hydrogen production unit, which can be replaced with an alkaline electrolyzer hydrogen production unit according to the actual hydrogen production needs, and is suitable for high-flow hydrogen production scenarios. This application uses a PLC for control, but it can also use a dedicated embedded integrated microcontroller customized based on the ARM architecture for control. Pressure sensor 404, check valve 403, pressure sensor 402, and radiator 401 are connected sequentially between the wet hydrogen output end of hydrogen production equipment 2 and gas-liquid separator 4. The radiator 401 installed on the wet hydrogen output pipeline can reduce the gas temperature, promote water vapor condensation, and improve the dehydration efficiency of gas-liquid separator 4. Pressure sensors 402 and 404 are used to monitor the hydrogen production outlet pressure. Check valve 403 prevents gas or liquid from flowing back into hydrogen production equipment 2. Together, they constitute the basic monitoring and protection unit to ensure the stability and safety of the gas production side. Furthermore, the gas-liquid separator 4 is also connected to a second safety valve 406 and a third solenoid valve 407. The second safety valve 406 and the third solenoid valve 407 are connected in parallel and connected to a water seal 5. The second safety valve 406 is set up for the gas-liquid separator 4 as a mechanical redundancy for overpressure protection. The third solenoid valve 407 provides a controlled exhaust / exhaust pipeline, both of which are connected to the water seal 5. This ensures that whether the second safety valve 406 is activated or the exhaust is actively performed, the gas is wet-treated by the water seal 5 and can be discharged more safely. Furthermore, the front-end hydrogen production and dehydration assembly also includes a water tank 3. The water tank 3 is connected to the water inlet of the hydrogen production equipment 2 by a manual ball valve 301, a safety valve 302, a water pump 303, a pressure sensor 305, a conductivity transmitter 306, and a flow meter 307. The water outlet of the hydrogen production equipment 2 is connected to the water tank 3 to form a water electrolysis transmission circuit. The water tank 3 and the hydrogen production equipment 2 constitute a circulating water circuit. The water pump 303 provides power, the flow meter 307 and the pressure sensor 305 monitor the water supply status, the conductivity transmitter 306 monitors the water quality online, and the safety valve 302 and the manual ball valve 301 provide safety isolation functions. The water tank 3 is equipped with a filtration unit, which includes a second water pump 309 connected to the water tank 3, a first radiator 310 connected to the second water pump 309, a first filter 311 connected to the first radiator 310, a second filter 312 connected to the first filter 311, and the second filter 312 connected to the water tank 3. The second water pump 309, the first radiator 310, the first filter 311, and the second filter 312 can circulate, cool, and purify the water in the water tank 3. The water tank 3 is equipped with a hydrogen leak sensor 313, a temperature transmitter 314, a float level gauge 315, an oxygen extraction fan 316, and a solenoid valve 319. The oxygen extraction fan 316 is connected to an oxygen discharge end 317, and the solenoid valve 319 is connected to a water supply end 318. The hydrogen leak sensor 313 monitors possible hydrogen leakage during water circulation. The temperature transmitter 314 and the float level gauge 315 monitor the water temperature and level. The oxygen extraction fan 316 can discharge the oxygen accumulated in the electrolyzed water to ensure safety. The solenoid valve 319 enables automatic water replenishment. Furthermore, a manual ball valve 304 is connected between the water pump 303 and the pressure sensor 305. The manual ball valve 304 is connected to a drain end 308. The drain end 308 is connected to a solenoid valve 501. The solenoid valve 501 is connected to a water seal device 5. The water seal device 5 is connected to a solenoid valve 405. The water seal device 5 is also connected to a vent end 502.

[0023] Furthermore, the centrally located adsorption purification unit is a pressure swing adsorption device, including a drying tower 6 and a drying tower 601 connected in parallel. Both the drying tower 6 and the drying tower 601 are filled with a composite medium of molecular sieve and palladium catalyst, which physically lies between the gas-liquid separator 4 and the palladium membrane tube 7 and the palladium membrane tube 701, serving as a second key water removal barrier to prevent high-humidity gas from washing away the core components in the downstream section. Drying tower 6 is connected to solenoid valve 5 611 and solenoid valve 612, and drying tower 2 601 is connected to solenoid valve 7 613 and solenoid valve 8 614. Solenoid valve 5 611 and solenoid valve 7 613 are connected to gas-liquid separator 4 through a pipeline; solenoid valve 612 and solenoid valve 8 614 are connected to water seal device 5 through a pipeline. By controlling the switching combination of solenoid valve 5 611, solenoid valve 612, solenoid valve 7 613 and solenoid valve 8 614, the working state of drying tower 6 and drying tower 2 601 can be flexibly switched, such as adsorption, regeneration, pressure equalization, etc., and the regeneration waste gas is guided to water seal device 5 for safe treatment. Drying tower 601 is connected to pressure sensor 4 602 and check valve 2 603. Check valve 3 604 is connected between check valve 2 603 and pressure sensor 4 602. Drying tower 601 is connected to pressure sensor 5 605 and check valve 5 607. Check valve 5 607 is connected to pressure sensor 5 605 and check valve 4 606. Manual needle valve 1 608 is connected between check valve 4 606 and check valve 3 604. Check valve 2 603, manual needle valve 1 608, and check valve 5 607 are connected. Pressure sensor 4 Pressure sensor 602 and pressure sensor 605 monitor the pressure of the two drying towers respectively, which are important parameters for controlling the PSA cycle steps. Check valves 603, 604, 606, and 607 form a unidirectional gas flow path, ensuring that the process gas and regeneration gas flow in the designed direction and preventing cross-contamination. Manual needle valve 608 can be used to finely adjust the pressure equalization rate between drying tower 6 and drying tower 601. Check valve 603 is also connected to solenoid valve 615, which is connected to vent valve 610.

[0024] Furthermore, the pressure-stabilizing isolation section includes a back pressure valve 609, a pressure reducing valve 616, a one-way valve 617, and a pressure sensor 618 connected in series between the manual needle valve 608 and the high-temperature palladium membrane purification unit at the tail end. The back pressure valve 609 provides a stable adsorption back pressure; the pressure reducing valve 616 reduces the pressure to a range suitable for palladium membrane purification; the one-way valve 617 prevents gas backflow; and the pressure sensor 618 monitors the gas pressure. The pressure-stabilizing isolation section effectively isolates the pressure difference between the two sections and provides stable and controllable gas intake conditions for the high-temperature palladium membrane purification unit at the tail end.

[0025] Furthermore, the tail-end high-temperature palladium membrane purification unit includes palladium membrane tube 1 7 and palladium membrane tube 2 701. A temperature transmitter 2 702 is connected between palladium membrane tube 1 7 and pressure sensor 618. Using palladium membrane tube 1 7 and palladium membrane tube 2 701 as the final purification components, hydrogen gas with extremely high purity can be produced by utilizing the unique dissolution-diffusion mechanism of hydrogen in palladium alloy. Temperature transmitter 2 702 monitors the inlet temperature, because the permeability of palladium membrane is very sensitive to temperature, and this parameter is crucial for controlling and optimizing purification efficiency. A one-way valve 703, a solenoid valve 704, a manual needle valve 705, a float flowmeter 706, and a one-way valve 707 are connected sequentially between the palladium membrane tube 7 and the water seal device 5. The solenoid valve 704 controls the opening and closing of the product gas flow path; the manual needle valve 705 is used to finely adjust the product gas back pressure or flow rate; the float flowmeter 706 displays the instantaneous flow rate of product hydrogen; the one-way valves 703 and 707 ensure the correct gas flow direction. This design facilitates the monitoring and regulation of the production of high-purity hydrogen. Furthermore, a temperature transmitter 708 is connected between palladium membrane tube 1 7 and palladium membrane tube 2 701. Palladium membrane tube 2 701 is equipped with a hydrogen discharge end 715, and pressure sensor 710, check valve 9 711, solenoid valve 12 712, dew point meter 713 and check valve 10 714 are sequentially connected between palladium membrane tube 2 701 and hydrogen discharge end 715. Solenoid valve 12 712 is also connected to water seal 5 and vent end 502. After the product gas of palladium membrane tube 2 701 is pressure measured by pressure sensor 710 and guided by check valve 9 711, the flow direction is controlled by solenoid valve 12 712. Dew point meter 713 monitors the dew point of the final product gas online, which is a key quality indicator for determining the purity of hydrogen. The final product gas is output from hydrogen discharge end 715, or switched to water seal 5 / vent end 502 by solenoid valve 12 712 for unqualified gas discharge or system purging. A solenoid valve 716 is connected between pressure sensor 710 and check valve 911. Palladium diaphragm tube 7 is also connected to solenoid valve 709. Solenoid valve 716 is connected to solenoid valve 709 and is connected to the protection circuit.

[0026] The protection circuit includes a vacuum pump 8, which is connected to solenoid valve 13 716 and solenoid valve 11 709. The vacuum pump 8 is also connected to a vacuum port 801. When the equipment is abnormally powered off or shut down for protection, the vacuum pump 8 can start the evacuation chamber to physically block the path of air to palladium membrane tube 1 7 and palladium membrane tube 2 701. This fundamentally eliminates the hardware pain point of extremely long dew point recovery period caused by high-temperature oxidation damage to palladium membrane tube 1 7 and palladium membrane tube 2 701.

[0027] All internal pipeline connections, airtightness tests, and PLC bottom-level interlocking actions in this application are packaged and debugged in the integrated rigid cabinet 1 during the factory manufacturing stage. After the equipment is delivered to the site, the engineers only need to connect the pure water, power supply, and end hydrogen output pipeline to start the machine, which saves the complex pipeline splicing, weld flaw detection, and joint debugging cycle between multiple controllers at the project site for separate equipment. The integrated design without external cascaded pipelines gives the entire preparation device physical rigidity, which not only reduces hydrogen leakage points, but also enables it to cope with harsh environments such as impact loads, and greatly reduces the structural threshold for explosion-proof review and export certification. Based on a pressure-following closed-loop hardware architecture, the underlying main controller can automatically perform stepless current adjustment on the front-end hydrogen production equipment 2 according to the slight fluctuations in the terminal hydrogen pressure. This flexible adjustment mechanism of "producing gas on demand" avoids thermal stress fatigue and energy waste caused by frequent hard start-stop of the equipment. This device uses a dual-tower structure of "molecular sieve + palladium catalyst" to handle most of the "coarse filtration and pre-deoxygenation" work, so that the more expensive palladium membrane tube 1 7 and palladium membrane tube 2 701 are only responsible for the final "ultra-low dew point fine adjustment". This physically reduces the cleaning frequency and replacement probability of palladium membrane tube 1 7 and palladium membrane tube 2 701, thus reducing the hardware maintenance cost of the entire system throughout its life cycle.

[0028] Example 2 further optimizes the high-purity hydrogen preparation device with adsorption purification and palladium membrane purification provided in Example 1. Specifically, drying tower 6 and drying tower 601 can be replaced with a TSA purification device with heating regeneration, and water and impurity removal can be achieved by thermal desorption.

[0029] Example 3 further optimizes the high-purity hydrogen preparation device with adsorption purification and palladium membrane purification provided in the above examples. Specifically, the protection circuit can be replaced by: expelling oxygen by filling in inert gas when the machine is shut down.

[0030] The high-purity hydrogen preparation device with adsorption purification and palladium membrane purification provided by this invention is used as follows: Step 1: System Startup and Preprocessing Water intake and circulation: Open the water supply end 318 of water tank 3, and add water to the set level of float level gauge 315 through solenoid valve 319. Start water pump 309, and the cooling water flows back to water tank 3 through radiator 310, filter 311, and filter 312 to complete the water filtration and circulation. Hydrogen production start-up: Start the hydrogen production equipment 2. Water pump 303 delivers pure water from water tank 3 to hydrogen production equipment 2. Manual ball valve 301, safety valve 302 and conductivity transmitter 306 monitor the inlet water quality and flow rate. Primary dehydration: Wet hydrogen gas is output from hydrogen production equipment 2, cooled by radiator 2 401, and then enters gas-liquid separator 4. The wire mesh demister, float level gauge 2 405 and solenoid valve 2 407 in the separator constitute a primary automated physical dehydration unit to separate liquid water. Step 2: Adsorption purification in the middle stage: Hydrogen gas that has undergone primary dehydration enters drying tower 6 and drying tower 2 601. Drying tower 6 and drying tower 2 601 undergo alternating adsorption and regeneration through solenoid valve group solenoid valve 5 611, solenoid valve 612, solenoid valve 7 613 and solenoid valve 8 614. The molecular sieve and palladium catalyst composite medium fills the tower to remove moisture and trace impurities, serving as a second purification barrier. Pressure stabilization control: The adsorbed hydrogen gas passes through the pressure stabilization isolation pipe section, and then passes through the back pressure valve 609, pressure reducing valve 616 and pressure sensor 618 in sequence to stabilize the input pressure to the high-temperature palladium membrane purification unit at the tail end. Step 3: High-temperature palladium membrane purification and hydrogen production output at the tail end: Hydrogen gas enters palladium membrane tube 1 7 and palladium membrane tube 2 701. A heating plate is installed between palladium membrane tube 1 7 and palladium membrane tube 2 701. During operation, the temperature is heated to 370-390℃ to provide a high-temperature environment. Under the high-temperature environment, hydrogen gas selectively permeates through the palladium membrane to obtain hydrogen gas with extremely high purity. The operating status of palladium diaphragm tube 1 and palladium diaphragm tube 2 701 is monitored in real time by temperature transmitter 2 702, temperature transmitter 3 708 and pressure sensor 7 710. The purified high-purity hydrogen is output through the hydrogen exhaust terminal 715; the dew point meter 713 monitors the hydrogen purity in real time. Step 4: System Protection and Shutdown Stop the operation of hydrogen production unit 2; In the event of an abnormal power outage or malfunction shutdown, the protection assembly should be activated immediately: Option A Vacuum Protection: Start vacuum pump 8, and draw a vacuum through solenoid valve 11 709 and solenoid valve 13 716 to physically block air from contacting the high-temperature palladium film tube and prevent oxidation; Option B: Inert gas protection: Inert gas is introduced to expel oxygen from the system through a protection circuit, thus preventing the palladium film from oxidizing. Venting and depressurization: Residual gas in the system can be discharged through the water seal 5 and each vent end 502 and vent end 610.

[0031] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection, an electrical connection, or a connection that allows communication between them; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0032] Obviously, the embodiments described above are merely some embodiments of the present invention, not all embodiments. The accompanying drawings show preferred embodiments of the present invention, but do not limit the patent scope of the present invention. The present invention can be implemented in many different forms; rather, these embodiments are provided to provide a more thorough and complete understanding of the disclosure of the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing specific embodiments, or make equivalent substitutions for some of the technical features. Any equivalent structures made using the content of this specification and drawings, directly or indirectly applied to other related technical fields, are similarly within the patent protection scope of this invention.

Claims

1. A high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification functions, characterized in that, Includes an integrated rigid cabinet (1) and integrated within the integrated rigid cabinet (1): front-end hydrogen production and dehydration assembly, central adsorption purification unit, tail-end high-temperature palladium membrane purification unit and protection assembly; The outlet of the front-end hydrogen production and dehydration assembly is connected to the inlet of the central adsorption and purification unit. The outlet of the central adsorption and purification unit is connected to the inlet of the tail-end high-temperature palladium membrane purification unit through a voltage-stabilizing isolation pipe section, forming a three-section series integrated structure. The protection assembly includes a protection circuit connected to the tail-end high-temperature palladium membrane purification unit.

2. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 1, characterized in that, The front-end hydrogen production and dehydration assembly includes a hydrogen production device (2) and a gas-liquid separator (4) connected to the wet hydrogen output end of the hydrogen production device (2). The gas-liquid separator (4) is equipped with a wire mesh demister. The gas-liquid separator (4) integrates a float level gauge and a solenoid valve (405). The float level gauge and the solenoid valve (405) constitute a first-level automated physical dehydration unit. The wet hydrogen output end of the hydrogen production equipment (2) is connected in sequence to the gas-liquid separator (4) by pressure sensor three (404), one-way valve one (403), pressure sensor two (402) and radiator two (401).

3. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 2, characterized in that, The gas-liquid separator (4) is also connected to a second safety valve (406) and a third solenoid valve (407). The second safety valve (406) and the third solenoid valve (407) are connected in parallel and are connected to a water seal (5).

4. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 3, characterized in that, The front-end hydrogen production and dehydration assembly also includes a water tank (3). The water tank (3) is connected to the water inlet of the hydrogen production equipment (2) by a manual ball valve (301), a safety valve (302), a water pump (303), a pressure sensor (305), a conductivity transmitter (306), and a flow meter (307). The water outlet of the hydrogen production equipment (2) is connected to the water tank (3) to form a water electrolysis transmission circuit.

5. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 4, characterized in that, A manual ball valve 2 (304) is connected between the water pump 1 (303) and the pressure sensor 1 (305). The manual ball valve 2 (304) is connected to a drain end (308). The drain end (308) is connected to a solenoid valve 4 (501). The solenoid valve 4 (501) is connected to a water seal device (5). The water seal device (5) is connected to the solenoid valve 2 (405). The water seal device (5) is also connected to a vent end (502).

6. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 5, characterized in that, The central adsorption purification unit is a pressure swing adsorption device, including a first drying tower (6) and a second drying tower (601) connected in parallel. Both the first drying tower (6) and the second drying tower (601) are filled with a composite medium of molecular sieve and palladium catalyst. The drying tower one (6) is connected to solenoid valve five (611) and solenoid valve six (612), and the drying tower two (601) is connected to solenoid valve seven (613) and solenoid valve eight (614). Solenoid valve five (611) and solenoid valve seven (613) are connected to the gas-liquid separator (4) through a pipeline; solenoid valve six (612) and solenoid valve eight (614) are connected to the water seal device (5) through a pipeline. The drying tower 1 (6) is connected to pressure sensor 4 (602) and check valve 2 (603). Check valve 3 (604) is connected between check valve 2 (603) and pressure sensor 4 (602). The drying tower 2 (601) is connected to pressure sensor 5 (605) and check valve 5 (607). Check valve 4 (606) is connected between check valve 5 (607) and pressure sensor 5 (605). Manual needle valve 1 (608) is connected between check valve 4 (606) and check valve 3 (604). Check valve 2 (603), manual needle valve 1 (608) and check valve 5 (607) are connected to each other.

7. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 6, characterized in that, The pressure stabilizing isolation pipe section includes a back pressure valve (609), a pressure reducing valve (616), a one-way valve (617), and a pressure sensor (618) connected in series between a manual needle valve (608) and a high-temperature palladium membrane purification unit at the tail end.

8. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 7, characterized in that, The tail-end high-temperature palladium membrane purification unit includes palladium membrane tube one (7) and palladium membrane tube two (701), and a temperature transmitter two (702) is connected between palladium membrane tube one (7) and pressure sensor six (618). The palladium membrane tube (7) and the water seal (5) are connected in sequence by a check valve (703), a solenoid valve (704), a manual needle valve (705), a float flowmeter (706), and a check valve (707).

9. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 8, characterized in that, A temperature transmitter (708) is connected between palladium membrane tube 1 (7) and palladium membrane tube 2 (701). The palladium membrane tube 2 (701) is provided with a hydrogen discharge end (715). A pressure sensor (710), a one-way valve (711), a solenoid valve (712), a dew point meter (713), and a one-way valve (714) are connected in sequence between the palladium membrane tube 2 (701) and the hydrogen discharge end (715). The solenoid valve (712) is also connected to the water seal (5) and the vent end (502). The pressure sensor 7 (710) is connected to the one-way valve 9 (711) by a solenoid valve 13 (716), and the palladium diaphragm tube 1 (7) is also connected to a solenoid valve 11 (709). The solenoid valve 13 (716) is connected to the solenoid valve 11 (709) and is connected to the protection circuit.

10. The high-purity hydrogen preparation apparatus with adsorption purification and palladium membrane purification according to claim 9, characterized in that, The protection circuit includes a vacuum pump (8), which is connected to solenoid valve thirteen (716) and solenoid valve eleven (709), and the vacuum pump (8) is also connected to a vacuum port (801).

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