Multi-stage separation and purification electronic-grade ultra-pure hydrogen preparation device

Abstract

The invention relates to the technical field of hydrogen purification, in particular to a multistage separation and purification electronic-grade ultra-pure hydrogen preparation device which comprises a storage tank, an adsorption purification mechanism, a condensation purification mechanism and a membrane separation purification mechanism. Wherein the adsorption purification mechanism is used for purifying hydrogen in the storage tank; the condensation purification mechanism is used for purifying the hydrogen purified by the adsorption purification mechanism; the membrane separation and purification mechanism is used for purifying the hydrogen purified by the condensation and purification mechanism; the device consists of multiple stages of purification mechanisms, and the multiple stages of purification mechanisms are coupled through pipelines, so that one set of device can be used for preparing high-purity hydrogen and ultra-pure hydrogen of various specifications, and the production requirements of electronic factories for simultaneously using hydrogen of different specifications and different purity levels are met.

Description

Technical Field

[0001] The present invention relates to the technical field of hydrogen purification, and specifically to an electronic-grade ultra-pure hydrogen preparation device for multi-stage separation and purification. Background Art

[0002] Nowadays, hydrogen has important uses in the fields of semiconductor material manufacturing, solar cell manufacturing, and electronic material manufacturing. In the field of electronic material manufacturing, there are extremely high requirements for the purity of hydrogen. It can be said that the purity of hydrogen directly affects the production quality of electronic materials.

[0003] In traditional technologies, equipment for hydrogen purification includes adsorption purification equipment, condensation purification equipment, membrane separation purification equipment, etc. Among them, the adsorption purification equipment adsorbs impurity gases through an adsorbent to achieve the purpose of purification; the condensation purification equipment purifies hydrogen by lowering the temperature of hydrogen, so that the impurity gases are liquefied due to low temperature, while hydrogen remains in a gaseous state to achieve hydrogen purification; the membrane separation purification mechanism separates based on the different permeation rates of different gas molecules in the membrane.

[0004] Among them, existing condensation purification equipment usually uses liquid nitrogen as a refrigerant, then hydrogen is introduced into a condenser to liquefy the impurity gases in hydrogen, and finally separation is carried out through a gas-liquid separator to discharge the liquid impurities. However, the condensed gas-liquid mixture still needs to be separated through a gas-liquid separator, which undoubtedly increases the equipment investment cost and raises the manufacturing cost of purified hydrogen. For this reason, we propose an electronic-grade ultra-pure hydrogen preparation device for multi-stage separation and purification to well solve the above drawbacks. Summary of the Invention

[0005] The purpose of the present invention is to provide an electronic-grade ultra-pure hydrogen preparation device for multi-stage separation and purification to solve the problems raised in the above background art.

[0006] The present invention is achieved through the following technical solutions: An electronic-grade ultra-pure hydrogen preparation device for multi-stage separation and purification, comprising: a storage tank;

[0007] An adsorption purification mechanism for purifying hydrogen in the storage tank;

[0008] A condensation purification mechanism for purifying the hydrogen purified by the adsorption purification mechanism;

[0009] A membrane separation purification mechanism for purifying the hydrogen purified by the condensation purification mechanism;

[0010] Among them, the condensation and purification mechanism includes a liquid nitrogen generator and a condensation coil. The condensation coil is spiral and includes an outer tube body and an inner tube body. The gap between the outer tube body and the inner tube body forms a condensation chamber. The two ends of the condensation coil are respectively provided with a liquid inlet and a liquid outlet communicated with the condensation chamber. The liquid inlet and the liquid outlet are respectively connected to the output end and the input end of the liquid nitrogen generator. The two ends of the condensation coil are respectively used to be connected to the output end of the adsorption and purification mechanism and the input end of the membrane separation and purification mechanism.

[0011] Optionally, the storage tank, the adsorption and purification mechanism, the condensation and purification mechanism, and the membrane separation and purification mechanism are sequentially connected by conveying pipelines, and electromagnetic valves are arranged on each conveying pipeline.

[0012] Optionally, the condensation and purification mechanism further includes a base and a tank body. The tank body and the liquid nitrogen generator are both arranged on the base. The spiral section of the condensation coil is arranged in the tank body, and both ends of the condensation coil extend out of the tank body.

[0013] Optionally, the outer tube body includes an outer decorative layer, an inner lining layer, and a heat insulation layer, where the heat insulation layer is located between the outer decorative layer and the inner lining layer.

[0014] Optionally, a plurality of support members are arranged between the outer tube body and the inner tube body to maintain the gap between the outer tube body and the inner tube body.

[0015] Optionally, the inner tube body is made of copper, and a plurality of heat conduction fins are further arranged on the inner surface of the inner tube body.

[0016] Optionally, a liquid leakage port is opened at the bottom position of the spiral section of the inner tube body, and a liquid leakage pipe penetrates through the bottom position of the spiral section of the outer tube body. The liquid leakage pipe is connected to the corresponding liquid leakage port.

[0017] Optionally, a horizontal pipe arranged in the horizontal direction is provided at the bottom of the tank body, and a plurality of the liquid leakage pipes are all connected to the horizontal pipe.

[0018] Optionally, a liquid discharge pipe is provided at the bottom of the horizontal pipe. A switching valve is arranged on the liquid discharge pipe, and one end of the liquid discharge pipe extends out of the tank body.

[0019] Optionally, a water level sensor is arranged inside the horizontal pipe, and a controller is further arranged outside the tank body. The signal output end of the water level sensor is connected to the controller, and the controller is connected to the switching valve.

[0020] Compared with the prior art, the present invention provides an electronic-grade ultra-pure hydrogen preparation device with multi-stage separation and purification, and has the following beneficial effects:

[0021] 1. The present invention is composed of a multi-stage purification mechanism, and the coupling between the multi-stage purification mechanisms is realized through pipelines. Therefore, a set of devices can prepare high-purity hydrogen and ultra-high-purity hydrogen of various specifications, meeting the production requirements of an electronics factory for simultaneously using hydrogen of different specifications and different purity levels;

[0022] 2. In the present invention, hydrogen condensation is carried out in a condensation coil, and the liquefied impurities can be discharged through the liquid leakage port at the bottom of the condensation coil, so that it is not necessary to separate impurities through a gas-liquid separator, which helps to reduce the manufacturing cost of hydrogen condensation and purification;

[0023] 3. In the present invention, liquid nitrogen is located in the condensation coil, while hydrogen is located in the inner tube body. This design can fully improve the utilization rate of liquid nitrogen, thus helping to save energy consumption. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 is a schematic structural diagram of the present invention;

[0025] Figure 2 is a schematic diagram of the condensation and purification mechanism of the present invention;

[0026] Figure 3 is a schematic structural diagram of the condensation coil of the present invention;

[0027] Figure 4 is Figure 2 the enlarged corresponding diagram at position A in

[0028] In the figure: 100, storage tank; 200, adsorption and purification mechanism; 300, condensation and purification mechanism; 301, liquid nitrogen generator; 302, condensation coil; 3021, outer tube body; 3022, inner tube body; 303, liquid inlet; 304, liquid outlet; 305, base; 306, tank body; 307, support member; 308, heat conduction fin; 309, liquid leakage port; 310, liquid leakage pipe; 311, horizontal pipe; 312, drain pipe; 313, water level sensor; 400, membrane separation and purification mechanism. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0029] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0030] Embodiment 1: Please refer to Figure 1 - Figure 3, this embodiment proposes an electronic-grade ultra-pure hydrogen production device with multi-stage separation and purification, including a storage tank 100, an adsorption purification mechanism 200, a condensation purification mechanism 300, and a membrane separation purification mechanism 400; among them, the adsorption purification mechanism 200 is used to purify the hydrogen in the storage tank 100, the condensation purification mechanism 300 is used to purify the hydrogen purified by the adsorption purification mechanism 200, and the membrane separation purification mechanism 400 is used to purify the hydrogen purified by the condensation purification mechanism 300; that is to say, this embodiment has three levels of purification mechanisms. Specifically, in the application process, according to the hydrogen demand, the coupling of the multi-stage purification system can be realized by switching, so as to meet various hydrogen demands.

[0031] It should be noted that the storage tank 100, the adsorption purification mechanism 200, the condensation purification mechanism 300, and the membrane separation purification mechanism 400 are sequentially connected by conveying pipelines, and electromagnetic valves are arranged on each conveying pipeline. Among them, the adsorption purification mechanism 200 adsorbs the impurity gas in the hydrogen through an adsorbent (such as activated carbon) to achieve the purification purpose. This is the prior art and will not be elaborated in this embodiment; the condensation purification mechanism 300 utilizes the difference in boiling points between hydrogen and other gases, cools the mixed gas to a low temperature through refrigeration, liquefies the impurity gas, and hydrogen remains in a gaseous state, thereby realizing separation; the membrane separation purification mechanism 400 realizes separation based on the different permeation rates of different gas molecules in the membrane. For example, only hydrogen molecules can pass through the palladium alloy membrane, and other gas molecules cannot pass through, so as to achieve the purpose of purifying hydrogen.

[0032] Furthermore, the condensation purification mechanism 300 includes a liquid nitrogen generator 301 and a condensation coil 302. The condensation coil 302 is spiral. The condensation coil 302 includes an outer tube body 3021 and an inner tube body 3022. The gap between the outer tube body 3021 and the inner tube body 3022 forms a condensation chamber. The two ends of the condensation coil 302 are respectively provided with a liquid inlet 303 and a liquid outlet 304 communicating with the condensation chamber. The liquid inlet 303 and the liquid outlet 304 are respectively connected to the output end and the input end of the liquid nitrogen generator 301. The two ends of the condensation coil 302 are respectively used to connect to the output end of the adsorption purification mechanism 200 and the input end of the membrane separation purification mechanism 400.

[0033] Among them, the liquid nitrogen generator 301 includes structures such as an air compressor, a nitrogen-oxygen separator, a refrigeration and liquefaction system, and a liquid storage tank. Among them, the prepared liquid nitrogen is stored in the liquid storage tank, and the outlet and inlet of the liquid storage tank are respectively connected to the liquid inlet 303 and the liquid outlet 304, so that the liquid nitrogen circulates in the condensation coil 302 to ensure that the inside of the condensation coil 302 is always in an ultra-low temperature state.

[0034] Further, the condensation and purification mechanism 300 further includes a base 305 and a tank body 306. The tank body 306 and the liquid nitrogen generator 301 are both arranged on the base 305. The spiral section of the condensation coil 302 is arranged inside the tank body 306, and both ends of the condensation coil 302 extend outside the tank body 306. The tank body 306 has a heat preservation function to prevent the external temperature from affecting the condensation coil 302.

[0035] In this embodiment, the multi-stage purification mechanisms are coupled to each other through pipelines. One set of devices can produce high-purity hydrogen and ultra-high-purity hydrogen of various specifications, meeting the production requirements of an electronics factory for simultaneously using hydrogen of different specifications and different purity levels.

[0036] Embodiment 2: Please refer to Figure 1 - Figure 4 This application embodiment also proposes an electronic-grade ultra-high-purity hydrogen production device for multi-stage separation and purification. The difference between this embodiment and Embodiment 1 is that the outer pipe body 3021 includes an exterior layer, a lining layer, and a heat preservation layer, where the heat preservation layer is located between the exterior layer and the lining layer. The function of the heat preservation layer is to prevent the liquid nitrogen from being affected by the external environmental temperature. A plurality of support members 307 are provided between the outer pipe body 3021 and the inner pipe body 3022 to maintain the gap between the outer pipe body 3021 and the inner pipe body 3022. The inner pipe body 3022 is made of copper, and a plurality of heat conduction fins 308 are further provided on the inner surface of the inner pipe body 3022. The inner pipe body 3022 and the heat conduction fins 308 are of an integrally formed structure.

[0037] Further, a liquid leakage port 309 is provided at the bottom position of the spiral section of the inner pipe body 3022, and a liquid leakage pipe 310 is provided through the bottom position of the spiral section of the outer pipe body 3021. The liquid leakage pipe 310 is connected to the corresponding liquid leakage port 309. A horizontal pipe 311 arranged in the horizontal direction is provided at the bottom of the tank body 306, and a plurality of liquid leakage pipes 310 are all connected to the horizontal pipe 311. Therefore, when the gas impurities inside the inner pipe body 3022 are liquefied, water droplets can gather at the bottom of the spiral section and are discharged through the liquid leakage pipe 310.

[0038] In addition, a liquid discharge pipe 312 is provided at the bottom of the horizontal pipe 311. A switch valve is provided on the liquid discharge pipe 312, and one end of the liquid discharge pipe 312 extends outside the tank body 306. A water level sensor 313 is provided inside the horizontal pipe 311, and a controller (not shown in the figure, specifically a PLC controller can be used) is further provided outside the tank body 306. The signal output end of the water level sensor 313 is connected to the controller, and the controller is connected to the switch valve. Specifically, in the normal state, the switch valve is in a closed state. When the water level inside the horizontal pipe 311 accumulates to the threshold height, the switch valve opens for drainage. When the water level inside the horizontal pipe 311 is lower than the threshold height, the switch valve automatically closes again, thereby preventing the inner pipe body 3022 from communicating with the external environment.

[0039] In summary, during the specific implementation of this embodiment, the storage tank 100 releases the hydrogen to be purified. After the hydrogen undergoes multi-stage purification by the adsorption purification mechanism 200, the condensation purification mechanism 300, and the membrane separation purification mechanism 400 in sequence, ultrapure hydrogen with a purity of 6N or above can finally be obtained. Among them, when the hydrogen flows in the condensation coil 302, the impurity gas is liquefied and remains in the inner tube body 3022. Finally, under the action of gravity, the liquid droplets pass through the drain pipe 312 and are discharged. Compared with the method of separating the two through a gas-liquid separation device, this embodiment can greatly reduce the equipment input cost. Secondly, timely discharging of the liquid to avoid accumulation also helps to improve the purification accuracy of hydrogen and reduce the consumption of liquid nitrogen.

[0040] It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variant thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements not only includes those elements, but also includes other elements not expressly listed, or further includes elements inherent to such process, method, article or device. Without further limitation, an element defined by the statement "including an..." does not exclude the existence of additional identical elements in the process, method, article or device including the element.

[0041] Although the embodiments of the present invention have been shown and described, those of ordinary skill in the art can understand that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. An electronic-grade ultra-pure hydrogen gas preparation device for multi-stage separation and purification, characterized in that, Comprising: A storage tank (100); An adsorption purification mechanism (200) for purifying hydrogen in the storage tank (100); A condensation purification mechanism (300) for purifying the hydrogen purified by the adsorption purification mechanism (200); A membrane separation purification mechanism (400) for purifying the hydrogen purified by the condensation purification mechanism (300); Among them, the condensation purification mechanism (300) includes a liquid nitrogen generator (301) and a condensation coil (302). The condensation coil (302) is spiral. The condensation coil (302) includes an outer tube body (3021) and an inner tube body (3022). The gap between the outer tube body (3021) and the inner tube body (3022) forms a condensation chamber. Both ends of the condensation coil (302) are respectively provided with a liquid inlet (303) and a liquid outlet (304) communicating with the condensation chamber. The liquid inlet (303) and the liquid outlet (304) are respectively connected to the output end and the input end of the liquid nitrogen generator (301). Both ends of the condensation coil (302) are respectively used to be connected to the output end of the adsorption purification mechanism (200) and the input end of the membrane separation purification mechanism (400).

2. The apparatus for preparing electronic-grade ultra-pure hydrogen gas with multi-stage separation and purification according to claim 1, wherein: The storage tank (100), the adsorption purification mechanism (200), the condensation purification mechanism (300), and the membrane separation purification mechanism (400) are sequentially connected by a conveying pipeline, and electromagnetic valves are arranged on each conveying pipeline.

3. The device for preparing electronic-grade ultra-pure hydrogen gas with multi-stage separation and purification according to claim 1, wherein: The condensation purification mechanism (300) further includes a base (305) and a tank body (306). The tank body (306) and the liquid nitrogen generator (301) are both arranged on the base (305). The spiral section of the condensation coil (302) is arranged inside the tank body (306), and both ends of the condensation coil (302) extend outside the tank body (306).

4. The apparatus for preparing electronic-grade ultra-pure hydrogen gas with multi-stage separation and purification according to claim 1, wherein: The outer tube body (3021) includes an outer decorative layer, an inner lining layer, and a heat insulation layer, where the heat insulation layer is located between the outer decorative layer and the inner lining layer.

5. The apparatus for preparing electronic-grade ultrapure hydrogen by multi-stage separation and purification according to claim 1, wherein: A plurality of support members (307) are arranged between the outer tube body (3021) and the inner tube body (3022) to maintain the gap between the outer tube body (3021) and the inner tube body (3022).

6. The apparatus for preparing electronic-grade ultrapure hydrogen by multi-stage separation and purification according to claim 1, wherein: The inner tube body (3022) is made of copper material, and a plurality of heat conducting fins (308) are further arranged on the inner surface of the inner tube body (3022).

7. The device for preparing electronic-grade ultra-pure hydrogen gas with multi-stage separation and purification according to claim 3, wherein: A liquid leakage port (309) is opened at the bottom position of the spiral section of the inner tube body (3022). A liquid leakage pipe (310) is penetrated through the bottom position of the spiral section of the outer tube body (3021). The liquid leakage pipe (310) is connected to the corresponding liquid leakage port (309).

8. An apparatus for preparing electronic-grade ultra-pure hydrogen gas by multi-stage separation and purification according to claim 7, characterized in that: A horizontal pipe (311) arranged in the horizontal direction is provided at the bottom of the tank body (306). A plurality of the liquid leakage pipes (310) are all connected to the horizontal pipe (311).

9. The apparatus for preparing electronic-grade ultra-pure hydrogen gas with multi-stage separation and purification according to claim 8, wherein: A drain pipe (312) is provided at the bottom of the horizontal pipe (311). A switch valve is arranged on the drain pipe (312), and one end of the drain pipe (312) extends outside the tank body (306).

10. The apparatus for preparing electronic-grade ultra-pure hydrogen gas by multi-stage separation and purification according to claim 9, wherein: A water level sensor (313) is provided inside the horizontal pipe (311), and a controller is further provided outside the tank body (306). A signal output end of the water level sensor (313) is connected to the controller, and the controller is connected to the switching valve.

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