Hydrogen purification device

Abstract

The utility model discloses a kind of hydrogen purification devices, it includes 2 or more parallel hydrogen purification units, raw material main pipeline, purified hydrogen pipeline and relaxation separation tail gas pipeline, the hydrogen purification unit includes metal hollow fiber membrane assembly, heating component, the upper flange with gas outlet for discharging purified hydrogen, the intermediate flange with heat exchange jacket, and the shell with lower flange, the upper flange with gas outlet, the intermediate flange with heat exchange jacket and the shell with lower flange are connected airtight by nut, the shell with lower flange is located in the heating component. By adopting the hydrogen purification device of the utility model, crude hydrogen raw gas is first passed through heat exchange jacket before being purified using metal hollow fiber membrane assembly, heat exchange is carried out using heat exchange jacket, preheating of raw gas can be achieved, energy efficiency is improved, while helping to maintain system thermal balance, reducing equipment depreciation and operating risk caused by temperature fluctuation, enhancing the safety of the device.

Description

Technical Field

[0001] This utility model belongs to the field of hydrogen purification technology, and in particular relates to a purification device for ultrapure hydrogen. Background Technology

[0002] Industrial byproducts from coking, refining, and other chemical industries contain hydrogen, which has high utilization value. Furthermore, due to the rapid development of hydrogen energy, the market demand for high-purity fuel hydrogen is increasing daily, and my country possesses abundant and inexpensive hydrogen resources from coking and refining industries. However, the composition of byproduct hydrogen resources is complex, and the separation and purification process is cumbersome, requiring several pretreatment steps before entering a pressure swing adsorption (PSA) unit for further separation and purification. If producing high-purity fuel hydrogen, due to stringent impurity requirements, multiple cycles within the PSA unit are needed to meet the fuel hydrogen's specifications. Therefore, the required equipment investment, energy consumption, and maintenance costs are substantial.

[0003] In addition, electronic specialty gases are one of the key raw materials in the semiconductor chip industry, known as the "industrial life" of the semiconductor industry, and play a vital role. Among them, high-purity hydrogen with a purity of 99.9999% to 99.9999999% (6N to 9N) is a special gas in electronic specialty gases and has significant applications in the epitaxial wafer preparation process of the semiconductor chip industry.

[0004] Currently, commonly used purification technologies for ultrapure hydrogen include catalytic adsorption and cryogenic adsorption. However, neither catalytic adsorption nor cryogenic adsorption can guarantee 100% purity of the raw gas. In contrast, purification technology using palladium alloy membranes can achieve extremely high hydrogen purity due to their 100% selectivity for hydrogen. However, palladium alloy membranes are not only expensive, but also typically consist of a palladium alloy membrane separation layer coated on a stainless steel tubular support, resulting in low packing density and susceptibility to damage during temperature fluctuations.

[0005] Therefore, the rational configuration of the various components of a hydrogen purification device to reduce the cost of the device and improve energy efficiency is a concern for those skilled in the art. Utility Model Content

[0006] The purpose of this invention is to provide a hydrogen purification device to solve at least one of the problems in the background art.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] A hydrogen purification device includes two or more parallel hydrogen purification units, a raw material main pipeline, a purified hydrogen pipeline, and a release and separation tail gas pipeline.

[0009] The aforementioned hydrogen purification unit is connected to the main raw material pipeline via an inlet branch, and a pressure reducing valve for the main raw material pipeline is installed outside the main raw material pipeline.

[0010] The aforementioned hydrogen purification unit includes a metal hollow fiber membrane assembly, a heating element, an upper flange with an outlet for discharging purified hydrogen, an intermediate flange with a heat exchange jacket, and a housing with a lower flange. The aforementioned upper flange with an outlet, the aforementioned intermediate flange with a heat exchange jacket, and the aforementioned housing with a lower flange are airtightly connected by nuts. The aforementioned housing with a lower flange is disposed within the aforementioned heating element. The aforementioned metal hollow fiber membrane assembly is configured to pass through the intermediate flange with a heat exchange jacket and be located within the housing with a lower flange.

[0011] The aforementioned upper flange with a gas outlet is equipped with a purified hydrogen outlet at its top, and the purified hydrogen outlet is connected to a purified hydrogen pipeline.

[0012] The aforementioned housing with a lower flange has a crude hydrogen feed gas inlet on its upper side and a purge separation tail gas outlet at the bottom, which is connected to the aforementioned purge separation tail gas pipeline.

[0013] The aforementioned intermediate flange with a heat exchange jacket has a heat exchange jacket inlet on one side and a heat exchange jacket outlet on the other side. The heat exchange jacket inlet is connected to the gas inlet branch, and the heat exchange jacket outlet is connected to the crude hydrogen feed gas inlet via a pipeline.

[0014] The aforementioned heating element has an external insulation layer, and the aforementioned pipe passes through the lower part of the insulation layer of the aforementioned heating element.

[0015] In some embodiments of the hydrogen purification device, a branch pressure reducing valve is provided outside the aforementioned inlet branch, a second check valve is provided outside the aforementioned purified hydrogen pipeline, a first check valve is provided outside the aforementioned pipeline, and a backup pressure valve is provided in the aforementioned release and separation tail gas pipeline.

[0016] In some embodiments of the hydrogen purification apparatus, a pressurization unit is also included, which is located upstream of the aforementioned raw material main pipeline and is used to pressurize the crude hydrogen raw material gas introduced into the aforementioned raw material main pipeline.

[0017] In some embodiments of the hydrogen purification apparatus, the pores between the aforementioned hollow metal membrane modules and the pores between the hollow metal membrane modules and the intermediate flange with the heat exchange jacket are sealed with sealant. When the hollow metal membrane is applied to the hydrogen purification apparatus, its ultra-fine diameter and ultra-thin membrane wall make it impossible to use the mechanical seals employed by traditional tubular palladium alloy membranes. By using sealant, it can be matched with the hollow metal membrane module, enabling it to seal well.

[0018] In some embodiments of the hydrogen purification apparatus, the lower end of the aforementioned hollow metal membrane assembly is closed, the upper end of the aforementioned hollow metal membrane assembly is open, and the upper end of the opening is exposed through the sealing portion of the intermediate flange with a heat exchange jacket.

[0019] In some embodiments of the hydrogen purification apparatus, the pipe (13) is also covered with insulation material.

[0020] By adopting the above technical solution, the present invention achieves the following beneficial effects:

[0021] By adopting the hydrogen purification device of this invention, the crude hydrogen feed gas passes through a heat exchange jacket before being purified using a metal hollow fiber membrane module. The heat exchange jacket is used for heat exchange and temperature rise, which can preheat the feed gas, improve energy efficiency, help maintain system thermal balance, reduce equipment depreciation and operational risks caused by temperature fluctuations, and enhance the safety of the device.

[0022] In addition, by setting the pipe connecting the heat exchange jacket outlet and the crude hydrogen feed gas inlet to pass through the lower part of the insulation layer of the heating element, the crude hydrogen feed gas enters the heating element through the pipe and passes through the lower part of the insulation layer of the heating element. After being heated by the heating element, it enters the outer wall of the metal hollow membrane module through the crude hydrogen feed gas inlet for separation and purification. On the other hand, the purified hydrogen gas is drawn upward from the inner cavity of the metal hollow fiber module into the purified hydrogen gas outlet of the upper flange with the gas outlet. Thus, heat can be exchanged between the cold crude hydrogen feed gas and the heated purified hydrogen gas, thereby enabling waste heat recovery.

[0023] In addition, by utilizing the heat exchanger of the crude hydrogen feed gas to remove some of the heat, the temperature at the sealing end can be reduced. This reduces the temperature resistance requirements of the sealing material used to seal the metal hollow fiber membrane, allowing the use of medium-temperature seals instead of high-temperature seals and simplifying the sealing system.

[0024] In addition, by connecting the various hydrogen purification units in parallel and setting up an independent heating unit for each hydrogen purification unit, each hydrogen purification unit forms an independent operating unit that can be independently turned off or on without affecting other hydrogen purification units. This facilitates the adjustment of the total hydrogen production and makes it easier to perform maintenance and replacement at any time, avoiding downtime during maintenance.

[0025] In addition, metal hollow fiber membranes with self-supporting structures have similar hydrogen separation capabilities to palladium alloy membranes, but at a lower cost, and the packing density is significantly increased due to the hollow fiber configuration. Attached Figure Description

[0026] Figure 1This is a schematic diagram of a hydrogen purification device according to one embodiment of the present invention.

[0027] Figure 2 for Figure 1 The diagram shows a hydrogen purification unit included in the hydrogen purification device.

[0028] Figure label:

[0029] 1. Hydrogen purification device; 2. Hydrogen purification unit; 3. Main feedstock line; 4. Purified hydrogen pipeline; 5. Release separation tail gas pipeline; 6. Main feedstock line pressure reducing valve; 7. Inlet branch line; 8. Metal hollow fiber membrane module; 9. Heating component; 10-1. Upper flange with outlet; 10-2. Intermediate flange with heat exchange jacket; 10-3. Outer shell with lower flange; 10-4. Nut; 11-1. Purified hydrogen outlet; 11-2. Crude hydrogen feedstock inlet; 11-3. Release separation tail gas outlet; 12-1. Heat exchange jacket inlet; 12-2. Heat exchange jacket outlet; 13. Pipeline; 14. Insulation layer; 15-1. Branch pressure reducing valve; 15-2. First check valve; 15-3. Second check valve; 15-4. Backup pressure valve; 16. Sealant. Detailed Implementation

[0030] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present utility model.

[0031] The hydrogen purification apparatus of one embodiment of the present invention will now be described with reference to the accompanying drawings.

[0032] The hydrogen purification device includes two or more hydrogen purification units. There is no particular limitation on the number of hydrogen purification units, as long as there are two or more; for example, there can be three, four, five, etc. Figure 1 This is a schematic diagram of a hydrogen purification device according to one embodiment of the present invention. Figure 1 The hydrogen purification apparatus shown includes three hydrogen purification units. The number of hydrogen purification units can be appropriately set by those skilled in the art as needed.

[0033] Figure 2 for Figure 1 The diagram shows a hydrogen purification unit included in the hydrogen purification device.

[0034] like Figure 1 and Figure 2As shown, the hydrogen purification device 1 includes a hydrogen purification unit 2 connected in parallel, a raw material main pipeline 3, a purified hydrogen pipeline 4, and a release and separation tail gas pipeline 5.

[0035] The hydrogen purification unit 2 is connected to the raw material main pipeline 3 via the inlet branch 7. A raw material main pipeline pressure reducing valve 6 is installed outside the raw material main pipeline 3.

[0036] The hydrogen purification unit 2 includes a metal hollow fiber membrane assembly 8, a heating element 9, an upper flange 10-1 with an outlet for discharging purified hydrogen, an intermediate flange 10-2 with a heat exchange jacket, and a housing 10-3 with a lower flange. The upper flange 10-1 with an outlet, the intermediate flange 10-2 with a heat exchange jacket, and the housing 10-3 with a lower flange are airtightly connected by nuts 10-4. The housing 10-3 with the lower flange is located inside the heating element 9. The metal hollow fiber membrane assembly 8 passes through the intermediate flange 10-2 with a heat exchange jacket and is disposed inside the housing 10-3 with the lower flange.

[0037] The top of the upper flange 10-1 with the gas outlet is provided with a purified hydrogen outlet 11-1, which is connected to the purified hydrogen pipeline 4.

[0038] The outer casing 10-3 with a lower flange has a crude hydrogen feed gas inlet 11-2 on its upper side and a purge separation tail gas outlet 11-3 at its bottom, which is connected to the purge separation tail gas pipeline 5.

[0039] The intermediate flange 10-2 with a heat exchange jacket has a heat exchange jacket inlet 12-1 on one side and a heat exchange jacket outlet 12-2 on the other side. The heat exchange jacket inlet 12-1 is connected to the gas inlet branch 7, and the heat exchange jacket outlet 12-2 is connected to the crude hydrogen feed gas inlet 11-2 through a pipe 13.

[0040] The heating element 9 has an insulation layer 14 on its exterior, and the pipe 13 passes through the lower part of the insulation layer 14 of the heating element 9.

[0041] The aforementioned heating element 9 can be any commonly used heating device, such as an electric heating element or electromagnetic heating, without any particular limitation. Those skilled in the art can select the appropriate device based on their needs. Alternatively, a programmable temperature controller can be used to precisely control its heating temperature.

[0042] A branch pressure reducing valve 15-1 is installed outside the aforementioned intake branch 7; a second check valve 15-3 is installed outside the aforementioned purified hydrogen pipeline 4; a first check valve 15-2 is installed outside the aforementioned pipeline 13; and a backup pressure valve 15-4 is installed outside the aforementioned release and separation tail gas pipeline 5. The aforementioned backup pressure valve 15-4 is used to control the internal pressure of the system, i.e., the feed pressure, and can also be closed to completely seal this pipeline.

[0043] The pores between the aforementioned metal hollow fiber membrane modules 8 and the pores between the metal hollow fiber membrane modules 8 and the intermediate flange 10-2 with the heat exchange jacket are sealed with sealant 16.

[0044] The aforementioned sealant 16 is preferably a high-temperature resistant sealant. "High-temperature resistant" means that it can withstand the temperatures required for hydrogen purification processes, such as 700°C.

[0045] The lower end of the aforementioned metal hollow fiber membrane assembly 8 is closed, and the upper end of the aforementioned metal hollow fiber membrane assembly 8 is open, and the upper end of the opening is exposed through the sealing portion of the intermediate flange 10-2 with heat exchange jacket.

[0046] Before starting operation, the branch pressure reducing valve 15-1, the second check valve 15-3, and the first check valve 15-2 should all be open, as should the backup pressure valve 15-4. Purge the entire gas path with high-pressure nitrogen until all oxygen is removed from the pipeline. Then, adjust the backup pressure valve 15-4 to pressurize the hydrogen purification device 1 to 3.0 MPa. At this point, close the branch pressure reducing valve 15-1 and the first check valve 15-2, and check the system's airtightness to ensure there is no pressure drop.

[0047] After ensuring the system's airtightness, switch the high-pressure nitrogen gas to high-pressure crude hydrogen feed gas. Open branch pressure reducing valve 15-1 and first check valve 15-2, and adjust the backup pressure valve 15-4 to bring the system pressure to 1.0 MPa. Then, use heating element 9 to heat the system to 700℃. After heating, adjust the backup pressure valve 15-4 to maintain the system pressure at 1.5 MPa, and keep the separation and purge tail gas velocity at 0.5 m / s. 3 h -1 ;

[0048] The crude hydrogen feed gas first enters the inlet branch 7 through the main feed gas line 3, and is introduced into the heat exchange jacket for preheating via the heat exchange jacket inlet 12-1, raising its temperature to 200°C. The preheated crude hydrogen feed gas then enters the pipeline 13 from the heat exchange jacket outlet 12-2, passes through the insulation layer 14 of the heating component 9, and enters the outer wall of the hollow fiber membrane in the metal hollow fiber membrane assembly 8 via the crude hydrogen feed gas inlet 11-2. During this process, the crude hydrogen feed gas is heated to 700°C. Subsequently, the crude hydrogen feed gas is separated and purified by the metal hollow fiber membrane assembly 8. During this process, the pure hydrogen component in the crude hydrogen feed gas enters the inner cavity of the hollow fiber membrane in the metal hollow fiber membrane assembly 8, passes through the intermediate flange 10-2 with the sealing end (16) of the metal hollow fiber membrane assembly, and then flows upward into the upper flange 10-1 with the outlet, and then flows into the purified hydrogen pipeline 4 via the purified hydrogen outlet 11-1.

[0049] In the above process, the crude hydrogen feed gas passes through a heat exchange jacket before entering the metal hollow fiber membrane module. Heat exchange and temperature rise are carried out here to preheat the feed gas and reduce the operating temperature of the sealing end. This allows the sealing end to be sealed with sealant, avoiding the use of high-temperature molten metal as a sealant. The operation is simpler and less damaging to the membrane.

[0050] As the purified hydrogen flows through the sealed end, heat exchange occurs between the heated purified hydrogen and the cold crude hydrogen feed gas, thereby enabling the recovery of the waste heat from the purified hydrogen.

[0051] The aforementioned metal hollow fiber membrane module 8 can be, for example, a nickel alloy hollow fiber membrane module. Compared to hydrogen purification devices using metal alloy membranes such as palladium alloy membranes, devices using metal hollow fiber membranes for hydrogen purification have a significantly increased membrane area within the same space due to the elongated fiber shape of the metal hollow fiber membrane, thus greatly increasing the packing density. This means that a larger contact area can be provided within the same volume of the device, thereby improving gas separation efficiency and production capacity.

[0052] The hydrogen purification device 1 can also be equipped with a pressurization unit upstream of the raw material main pipeline 3 for pressurizing the crude hydrogen raw material gas introduced into the raw material main pipeline 3. Figure 1 (Not shown in the image). The so-called upstream of the main feedstock pipeline refers to the upstream of the air inlet. Figure 1 In the hydrogen purification apparatus shown, a pressurization unit can be installed, for example, before the pressure reducing valve 6 on the main feed line. The crude hydrogen feed gas introduced into the main line is pressurized using the pressurization unit.

[0053] By incorporating a pressurization unit, the crude nitrogen feed gas in the metal hollow fiber membrane module is pressurized during operation, achieving a high pressure of 0.4–3.0 MPa on the feed side of the membrane, while maintaining atmospheric pressure on the separation side, thus achieving a transmembrane pressure difference across the membrane. Compared to existing devices that evacuate the membrane, this significantly improves the purity of hydrogen, reaching electronic-grade levels (≥99.9999%).

[0054] The aforementioned pipe (13) may also be covered with insulation material. This can prevent the loss of heat from the gas flowing through the pipe (13).

[0055] The above description is only a preferred embodiment of the present utility model, but the protection scope of the present utility model is not limited thereto. Any equivalent substitutions or changes made by those skilled in the art within the technical scope disclosed in the present utility model, based on the technical solution and the inventive concept of the present utility model, should be included within the protection scope of the present utility model.

Claims

1. A hydrogen purification device, characterized in that, It includes two or more parallel hydrogen purification units (2), a raw material main pipeline (3), a purified hydrogen pipeline (4), and a release and separation tail gas pipeline (5). The hydrogen purification unit (2) is connected to the raw material main pipeline (3) through the inlet branch (7), and the raw material main pipeline (3) is equipped with a raw material main pipeline pressure reducing valve (6). The hydrogen purification unit (2) includes a metal hollow fiber membrane assembly (8), a heating element (9), an upper flange (10-1) with an outlet for discharging purified hydrogen, an intermediate flange (10-2) with a heat exchange jacket, and a housing (10-3) with a lower flange. The upper flange (10-1) with an outlet, the intermediate flange (10-2) with a heat exchange jacket, and the housing (10-3) with a lower flange are airtightly connected by nuts (10-4). The housing (10-3) with a lower flange is located inside the heating element (9). The metal hollow fiber membrane assembly (8) is configured to pass through the intermediate flange (10-2) with a heat exchange jacket and be located inside the housing (10-3) with a lower flange. The top of the upper flange (10-1) with the gas outlet is provided with a purified hydrogen outlet (11-1), which is connected to the purified hydrogen pipeline (4). The upper side of the outer shell (10-3) with the lower flange is provided with a crude hydrogen feed gas inlet (11-2), and the bottom is provided with a release separation tail gas outlet (11-3), which is connected to the release separation tail gas pipeline (5). The intermediate flange (10-2) with heat exchange jacket has a heat exchange jacket inlet (12-1) on one side and a heat exchange jacket outlet (12-2) on the other side. The heat exchange jacket inlet (12-1) is connected to the gas inlet branch (7), and the heat exchange jacket outlet (12-2) is connected to the crude hydrogen raw material gas inlet (11-2) through a pipeline (13). The heating element (9) has an insulation layer (14) on its exterior, and the pipe (13) passes through the lower part of the insulation layer (14) of the heating element (9).

2. The hydrogen purification apparatus according to claim 1, characterized in that, The intake branch (7) is equipped with a branch pressure reducing valve (15-1). The purified hydrogen pipeline (4) is equipped with a second check valve (15-3). A first check valve (15-2) is provided outside the pipe (13). The exhaust gas separation pipeline (5) is equipped with a backup pressure valve (15-4).

3. The hydrogen purification apparatus according to claim 1, characterized in that, It also includes a pressurization unit, The pressurization unit is located upstream of the main raw material pipeline (3) and is used to pressurize the crude hydrogen raw material gas introduced into the main raw material pipeline (3).

4. The hydrogen purification apparatus according to claim 1, characterized in that, The pores between the metal hollow fiber membrane modules (8) and the pores between the metal hollow fiber membrane modules (8) and the intermediate flange (10-2) with the heat exchange jacket are sealed with sealant (16).

5. The hydrogen purification apparatus according to claim 1, characterized in that, The lower end of the metal hollow fiber membrane assembly (8) is closed, and the upper end of the metal hollow fiber membrane assembly (8) is open, and the upper end of the opening is exposed through the sealing portion of the intermediate flange (10-2) with heat exchange jacket.

6. The hydrogen purification apparatus according to claim 1, characterized in that, The pipe (13) is also covered with insulation material.

Images