CN114031038B - Self-heating palladium membrane purification device and purification method - Google Patents

Self-heating palladium membrane purification device and purification method Download PDF

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Publication number
CN114031038B
CN114031038B CN202111511282.8A CN202111511282A CN114031038B CN 114031038 B CN114031038 B CN 114031038B CN 202111511282 A CN202111511282 A CN 202111511282A CN 114031038 B CN114031038 B CN 114031038B
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cavity
sleeve
valve
purification
gas
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CN114031038A (en
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张�浩
朱玉厚
黄润伍
马骏驰
袁智
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Wuhan Institute of Marine Electric Propulsion China Shipbuilding Industry Corp No 712 Institute CSIC
Wuhan Hydrogen Energy and Fuel Cell Industry Technology Research Institute Co Ltd
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Wuhan Institute of Marine Electric Propulsion China Shipbuilding Industry Corp No 712 Institute CSIC
Wuhan Hydrogen Energy and Fuel Cell Industry Technology Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/501Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
    • C01B3/503Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion characterised by the membrane
    • C01B3/505Membranes containing palladium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0405Purification by membrane separation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0001Separation or purification processing
    • C01B2210/0009Physical processing
    • C01B2210/001Physical processing by making use of membranes
    • C01B2210/0012Physical processing by making use of membranes characterised by the membrane

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Abstract

The invention discloses an autothermal palladium membrane purification device and a purification method, comprising the following steps: the thimble assembly, purification subassembly and heating element, the thimble assembly includes first sleeve pipe, second sleeve pipe and third sleeve pipe, arrange first sleeve pipe in the second sleeve pipe, and arrange the second sleeve pipe in the third sleeve pipe, and become the first cavity of mutual intercommunication with first sheathed tube internal partitioning, second cavity and third cavity, first cavity, second cavity and third cavity set gradually along first sheathed tube is radial, purification subassembly includes at least one purification piece, place the second cavity in the purification piece, a crude hydrogen gas body for the second cavity is flowed through in the purification flow, heating element includes the heating element, place first cavity in the heating element is even, a space for providing crude hydrogen gas burning, and with produced heat transfer to purification subassembly of crude hydrogen gas burning, so that purification subassembly thermally equivalent. The invention can solve the problem that the hydrogen can not be purified under the condition of lacking external electric energy or other heating modes.

Description

Self-heating palladium membrane purification device and purification method
Technical Field
The invention relates to the technical field of hydrogen purification, in particular to an autothermal palladium membrane purification device and a purification method.
Background
In recent years, with the rapid development of industries such as hydrogen energy and the like, the demand of high-purity hydrogen is rapidly increased, the research on the production and separation technology of high-purity hydrogen is promoted, a palladium membrane diffusion method is one of methods for obtaining the high-purity hydrogen, the dissolution of hydrogen in a palladium membrane is a spontaneous heat release process, and the solubility is reduced along with the rise of temperature. The palladium membrane is in the alpha phase in the temperature range higher than 300 ℃, and when the temperature is gradually reduced from 300 ℃, the solubility of hydrogen is gradually increased, and the beta phase begins to be formed. Because the alpha phase and the beta phase have different unit cell parameters, when the palladium membrane is subjected to hydrogen adsorption/desorption or temperature rise/reduction circulation for a plurality of times, the crystal structure is repeatedly changed between the alpha phase and the beta phase, so that the palladium membrane is distorted and even broken to become hydrogen embrittlement. To avoid this phenomenon, the palladium membrane is operated at a temperature higher than 300 ℃ for hydrogen separation and purification. Therefore, when designing a palladium membrane purifier, a corresponding preheating device is required to heat the purifier.
For example, application numbers are: chinese patent invention CN202010365262.3, entitled: a hydrogen purification device and a method for independently heating a feed gas and a palladium membrane purifier comprise a feed gas pipeline and a palladium membrane purifier; the feed gas pipeline is communicated with the palladium membrane purifier through a feed gas outlet pipe and a purifier inlet pipe in sequence; and the feed gas pipeline is arranged outside the palladium membrane purifier; the first heater is arranged on the inner side of the raw material gas pipeline close to the palladium membrane purifier and used for heating the raw material gas pipeline; and a second heater is arranged between the palladium membrane purifier and the first heater and used for heating the palladium membrane purifier. And provides a hydrogen purification method in which the raw material gas and the palladium membrane purifier are independently heated. The hydrogen purification device has a simple structure, can be uniformly heated and can control the temperature, and can improve the hydrogen purification efficiency; correspondingly, the hydrogen purification method provided by the invention is simple and convenient to operate, uniform in heating and accurate in temperature control, and can improve the hydrogen purification efficiency, and when the similar purifiers are heated by adopting a heating device, and the purifiers do not have the condition of heating by external electric energy or other external heating devices under the actual use environment, the purifiers cannot increase the temperature in time, so that the hydrogen purification effect is influenced.
Therefore, there is a need for an autothermal palladium membrane purification device and method for purifying hydrogen gas, which can solve the problem in the prior art that the device cannot purify hydrogen gas because it does not have external electric energy or other heating means.
Disclosure of Invention
In view of the above, it is necessary to provide an autothermal palladium membrane purification device and a purification method, which solve the technical problem in the prior art that the device cannot purify hydrogen gas because it does not have external electric energy or other heating methods.
In order to achieve the above technical object, a technical solution of the present invention provides an autothermal palladium membrane purification device, comprising:
the sleeve assembly comprises a first sleeve, a second sleeve and a third sleeve, wherein the second sleeve is arranged in the first sleeve, the third sleeve is arranged in the second sleeve and divides the interior of the first sleeve into a first cavity, a second cavity and a third cavity which are communicated with each other, and the first cavity, the second cavity and the third cavity are sequentially arranged along the radial direction of the first sleeve;
the purification assembly comprises at least one purification piece, the purification piece is arranged in the second cavity and is used for purifying the crude hydrogen gas flowing through the second cavity;
and the heating component comprises a heating element, the heating element is uniformly arranged in the first cavity and used for providing a space for burning the crude hydrogen gas and transferring the heat generated by burning the crude hydrogen gas to the purification component so as to ensure that the purification component is uniformly heated.
Furthermore, the purifying part comprises a fourth sleeve and at least one palladium membrane purifying tube, the fourth sleeve is arranged in the second cavity and uniformly arranged along the circumferential direction of the second sleeve, and the palladium membrane purifying tubes are arranged along the axial direction of the first sleeve and uniformly arranged in the fourth sleeve.
Furthermore, the heating element comprises at least two first fins, at least two second fins and a combustion catalyst, the first fins are arranged on the circumferential inner wall of the first sleeve along the radial direction of the first sleeve and are connected with the inner wall of the first sleeve and the outer wall of the second sleeve, the second fins are arranged between the two adjacent first fins, the second fins are connected with the inner wall of the first sleeve and the outer wall of the second sleeve, and the combustion catalyst is uniformly coated on the second fins.
Furthermore, the heating assembly further comprises a screen, and the screen is uniformly arranged in the first cavity and is connected with the inner wall of the first sleeve and the outer wall of the other end of the second sleeve.
Furthermore, the sleeve assembly further comprises a first sealing plate and a second sealing plate, the first sealing plate and the second sealing plate are respectively connected to two ends of the first sleeve and used for sealing two ends of the first sleeve, and one end of the second sleeve and one end of the third sleeve are connected with the first sealing plate.
Furthermore, the sleeve assembly further comprises a first sealing plate and a second sealing plate, the first sealing plate and the second sealing plate are respectively connected to two ends of the first sleeve and used for sealing two ends of the first sleeve, and one end of the second sleeve and one end of the third sleeve are connected with the first sealing plate.
The gas inlet assembly comprises at least one first gas inlet pipe, at least one first valve, at least one second gas inlet pipe, at least one second valve, a crude hydrogen gas inlet and at least one air inlet, the first gas inlet pipe is communicated with the first cavity and connected to the first sealing plate and used for introducing crude hydrogen gas into the first cavity, the first valves are arranged in one-to-one correspondence with the first gas inlet pipe and arranged on the first gas inlet pipe, the second gas inlet pipe is communicated with the second cavity and connected to the first sealing plate and used for introducing crude hydrogen gas into the second cavity, the second valves are arranged in one-to-one correspondence with the second gas inlet pipe and arranged on the second gas inlet pipe, the crude hydrogen gas inlet is communicated with the first gas inlet pipe and the second gas inlet pipe, and the air inlet is communicated with the first gas inlet pipe.
The gas outlet assembly comprises at least one first gas outlet pipe, at least one third valve, at least one second gas outlet pipe, at least one fourth valve, a third gas outlet pipe and a tail gas outlet, the first gas outlet pipe is communicated with the second cavity and connected to the second sealing plate and used for discharging hydrogen purified by the purifying part, the third valves are arranged in one-to-one correspondence with the first gas outlet pipe and arranged on the first gas outlet pipe, the second gas outlet pipe is communicated with the second cavity and connected to the first sealing plate and used for discharging tail gas purified by the purifying part, the fourth valves are arranged in one-to-one correspondence with the second gas outlet pipe and arranged on the second gas outlet pipe, the third gas outlet pipe is communicated with the third cavity and connected to the second sealing plate and used for discharging tail gas combusted by the heating part, and the tail gas outlet is communicated with the first gas outlet pipe, the second gas outlet pipe and the third gas outlet pipe.
Furthermore, the temperature measuring device also comprises a temperature measuring part, wherein the temperature measuring part is connected to the outer wall of the first sleeve, and the measuring end of the temperature measuring part is arranged in the second cavity.
Further, the heat exchanger also comprises at least one third fin, wherein the third fin is arranged along the radial direction of the third sleeve and connected to the circumferential inner wall of the third sleeve.
The technical scheme of the invention also provides a self-heating palladium membrane purification method, which comprises the following steps:
s1, closing the first valve, the third valve and the fourth valve, opening the second valve, connecting the second valve with the crude hydrogen gas inlet by using vacuumizing equipment, vacuumizing the interiors of the first cavity, the second cavity and the third cavity to 0.01-0.05 MPa, and then closing the second valve;
s2, opening the first valve, introducing crude hydrogen gas along a crude hydrogen gas inlet, introducing air from the air inlet, igniting the mixed gas in a heating element to heat the purification assembly, and discharging the combusted tail gas through the tail gas outlet;
s3, controlling the flow rate of the first valve, and monitoring the temperature of the palladium membrane purification tube through the temperature measuring part to maintain the temperature of the palladium membrane purification tube at 350-400 ℃;
s4, opening the second valve, the third valve and the fourth valve to enable crude hydrogen gas to enter the palladium membrane purification pipe, purifying the crude hydrogen gas, discharging the hydrogen gas through the first gas outlet pipe, and discharging purified tail gas and combusted tail gas through the tail gas outlet;
s5, closing the third valve and the fourth valve, vacuumizing the interiors of the first cavity, the second cavity and the third cavity to 0.01-0.05 MPa according to the step in the S1, and closing the first valve and the second valve to naturally cool the purification piece.
Compared with the prior art, the invention has the beneficial effects that: the second sleeve is internally arranged in the first sleeve, the third sleeve is internally arranged in the second sleeve, the interior of the first sleeve is divided into a first cavity, a second cavity and a third cavity which are communicated with each other, at least one purifying piece is arranged in the second cavity and used for purifying crude hydrogen gas flowing through the second cavity, the heating piece is uniformly arranged in the first cavity and used for providing a space for burning the crude hydrogen gas, heat generated by burning the crude hydrogen gas is transferred to the purifying component, so that the purifying component is uniformly heated, and purification of the crude hydrogen gas introduced into the purifying piece is facilitated.
Drawings
Fig. 1 is a schematic cross-sectional view of an autothermal palladium membrane purification device according to an embodiment of the present invention;
FIG. 2 isbase:Sub>A cross-sectional view taken along line A-A of FIG. 1;
fig. 3 is a schematic cross-sectional view of a second fin and combustion catalyst junction provided by an embodiment of the present invention.
Detailed Description
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate preferred embodiments of the invention and together with the description, serve to explain the principles of the invention and not to limit the scope of the invention.
Referring to fig. 1, the present invention provides an autothermal palladium membrane purification device, comprising: sleeve assembly 1, purification subassembly 2 and heating element 3, sleeve assembly 1 includes first sleeve pipe 11, second sleeve pipe 12 and third sleeve pipe 13, place first sleeve pipe 11 in second sleeve pipe 12, and place second sleeve pipe 12 in third sleeve pipe 13, and separate into the first cavity of mutual intercommunication with the inside of first sleeve pipe 11, second cavity and third cavity, first cavity, second cavity and third cavity set gradually along first sleeve pipe 11's radial, purification subassembly 2 includes at least one purification subassembly 21, place the second cavity in the purification subassembly 21, be used for the crude hydrogen gas of purification flow through the second cavity, heating element 3 includes heating member 31, place first cavity in the heating member 31 is even, be used for providing the space that crude hydrogen gas burns, and transmit the produced heat of crude hydrogen gas burning to purification subassembly 2, so that purification subassembly 2 is heated evenly.
It can be understood that the second sleeve 12 is arranged in the first sleeve 11, the third sleeve 13 is arranged in the second sleeve 12, the interior of the first sleeve 11 is divided into a first cavity, a second cavity and a third cavity which are communicated with each other, at least one purifying piece 21 is arranged in the second cavity and used for purifying crude hydrogen gas flowing through the second cavity, the heating piece 31 is uniformly arranged in the first cavity and used for providing a space for burning the crude hydrogen gas, and heat generated by burning the crude hydrogen gas is transferred to the purifying component 2, so that the purifying component 2 is uniformly heated, and the purifying piece 21 is favorable for purifying the crude hydrogen gas introduced into the purifying piece.
Furthermore, the purification device of the invention further comprises an air inlet component 4 for controlling air to enter the purification device, an air outlet component 5 for controlling air to be discharged from the purification device, a temperature measuring component 6 for monitoring the temperature of the purification component 2, and at least one third fin 7 for promoting the heat dissipation of the tail gas.
Furthermore, the first sleeve 11, the second sleeve 12 and the third sleeve 13 in the device are all made of 316 or 316L stainless steel and are electropolished.
As shown in fig. 1, the sleeve assembly 1 further includes a first closing plate 14 and a second closing plate 15, the first closing plate 14 and the second closing plate 15 are respectively connected to two ends of the first sleeve 11 for closing off two ends of the first sleeve 11, and one end of the second sleeve 12 and one end of the third sleeve 13 are both connected to the first closing plate 14.
It will be appreciated that the first and second closure plates 14 and 15 seal off the ends of the first sleeve 11 to form a closed and sealed space for the purification of the crude hydrogen gas.
As shown in fig. 1 and fig. 2, the purifying member 21 includes a fourth sleeve 211 and at least one palladium membrane purifying tube 212, the fourth sleeve 211 is disposed in the second cavity and uniformly arranged along the circumferential direction of the second sleeve 12, and the palladium membrane purifying tubes 212 are disposed along the axial direction of the first sleeve 11 and uniformly disposed in the fourth sleeve 211.
It can be understood that the purification apparatus of the present invention comprises a plurality of purification units 21, and each purification unit 21 is composed of a fourth sleeve 211 and at least one palladium membrane purification tube 212, and the fourth sleeve 211 is sleeved outside the plurality of palladium membrane purification tubes 212, so that the crude hydrogen is in sufficient contact with the palladium membrane purification tubes 212, which is beneficial to the purification of the crude hydrogen.
Specifically, the number of the palladium membrane purification tubes 212 is 18-60, and the palladium membrane purification tubes are manufactured by a drawing method, one end of each palladium membrane purification tube is welded on the first closing plate 14, the other end of each palladium membrane purification tube is sealed by a brazing plug, the outer diameter of each palladium membrane purification tube is 5-10 mm, the length of each palladium membrane purification tube is 300-600 mm, the wall thickness of each palladium membrane purification tube is 50-120 microns, and the palladium membrane tubes are preferably made of palladium yttrium, palladium copper or palladium silver alloy.
Further, the palladium membrane purification tube 212 of the present invention purifies hydrogen gas using noble metals such as palladium, and the palladium membrane purification tube 212 is a conventional arrangement known to those skilled in the art and will not be described in detail.
As shown in fig. 1 to 3, the heating member 31 includes at least two first fins 311, at least two second fins 312, and a combustion catalyst 313, the first fins 311 are disposed on the circumferential inner wall of the first sleeve 11 along the radial direction of the first sleeve 11 and are connected to both the inner wall of the first sleeve 11 and the outer wall of the second sleeve 12, the second fins 312 are disposed between two adjacent first fins 311, the second fins 312 are connected to both the inner wall of the first sleeve 11 and the outer wall of the second sleeve 12, and the combustion catalyst 313 is uniformly coated on the second fins 312.
It can be understood that the first fins 311 and the second fins 312 are uniformly distributed along the circumferential inner wall of the first sleeve 11, so as to uniformly heat the whole sleeve assembly 1 and the purification assembly 2 arranged in the second chamber, which is more beneficial to the purification of hydrogen.
Further, in the present invention, the cross section of the second fin 312 is spiral, and the cross section of the second fin is continuously increased along the axial direction away from the first sleeve 11, and the combustion catalyst 313 is uniformly coated on the second fin 312 for increasing the heat exchange area of the catalytic combustion.
Furthermore, the combustion catalyst 313 in the invention is a supported Pt granular catalyst using gamma-Al 2O 3-Carbon Nano Tube (CNT) as a carrier, the diameter of the granular catalyst is 2-3 mm, or a wall-supported catalyst using Al2O3 as a transition layer and then a Pt active layer is chemically deposited, and the wall-supported catalyst is uniformly coated on the surface of the secondary fin.
In one embodiment, the heating assembly 3 further includes a screen 32, and the screen 32 is uniformly disposed in the first cavity and connected to the inner wall of the first sleeve 11 and the outer wall of the other end of the second sleeve 12 for supporting and filtering the combustion member.
Further, the screen 32 is a composite screen 32 with two layers of different mesh numbers, specifically, the mesh numbers of the screen 32 in the present invention are 5 mesh and 40 mesh, wherein the 5 mesh screen 32 plays a supporting role, and the 40 mesh screen 32 plays a role of filtering the catalytic combustion catalyst 313.
As shown in fig. 1, the air intake assembly 4 includes at least one first air intake pipe 41, at least one first valve 42, at least one second air intake pipe 43, at least one second valve 44, a crude hydrogen gas inlet 45, and at least one air inlet 46, the first air intake pipe 41 is communicated with the first cavity and connected to the first sealing plate 14 for introducing crude hydrogen gas into the first cavity, the first valve 42 is disposed in one-to-one correspondence with the first air intake pipe 41 and disposed on the first air intake pipe 41, the second air intake pipe 43 is communicated with the second cavity and connected to the first sealing plate 14 for introducing crude hydrogen gas into the second cavity, the second valve 44 is disposed in one-to-one correspondence with the second air intake pipe 43 and disposed on the second air intake pipe 43, the crude hydrogen gas inlet 45 is communicated with both the first air intake pipe 41 and the second air intake pipe 43, and the air inlet 46 is communicated with the first air intake pipe 41.
It can be understood that, the cooperation of the first air inlet pipe 41 and the first valve 42 is used for controlling the rate of crude hydrogen gas entering the combustion assembly, the cooperation of the second air inlet pipe 43 and the second valve 44 is used for controlling crude hydrogen gas entering the purifying part 21, the crude hydrogen gas inlet 45 is communicated with the first air inlet pipe 41 and the second air inlet pipe 43, meanwhile, the air inlet 46 is communicated with the first air inlet pipe 41 and is used for introducing air into the combustion assembly, and the combusted tail gas passes through the purifying part 21 in the second chamber and is discharged from the third chamber.
As shown in fig. 1, the gas outlet assembly 5 includes at least one first gas outlet pipe 51, at least one third valve 52, at least one second gas outlet pipe 53, at least one fourth valve 54, a third gas outlet pipe 55 and a tail gas outlet 56, the first gas outlet pipe 51 is communicated with the second cavity and connected to the second sealing plate 15 for discharging the hydrogen gas purified by the purifying member 21, the third valve 52 is disposed in one-to-one correspondence with the first gas outlet pipe 51 and disposed on the first gas outlet pipe 51, the second gas outlet pipe 53 is communicated with the second cavity and connected to the first sealing plate 14 for discharging the tail gas purified by the purifying member 21, the fourth valve 54 is disposed in one-to-one correspondence with the second gas outlet pipe 53 and disposed on the second gas outlet pipe 53, the third gas outlet pipe 55 is communicated with the third cavity and connected to the second sealing plate 15 for discharging the tail gas combusted by the heating member 31, and the tail gas outlet 56 is communicated with the first gas outlet pipe 51, the second gas outlet pipe 53 and the third gas outlet pipe 55.
It can be understood that the first outlet pipe 51 is matched with the third valve 52 for controlling the discharge of the hydrogen purified by the purifying member 21, the second outlet pipe 53 is matched with the fourth valve 54 for controlling the discharge of the tail gas purified by the purifying member 21, and the third outlet pipe 55 is communicated with the third chamber and finally communicated with the tail gas outlet 56 for the tail gas discharge of the whole device.
As shown in FIG. 1, the temperature measuring member 6 is connected to the outer wall of the first sleeve 11, and the measuring end thereof is disposed in the second cavity.
It can be understood that the probe of the temperature measuring unit 6 is located in the palladium membrane purifying tube 212 for monitoring the temperature of the palladium membrane purifying tube 212, and then the user can adjust and control the flow of the crude hydrogen gas in the combustion assembly according to the monitored temperature, and maintain the temperature of the palladium membrane purifying tube 212 at 350-400 ℃.
As shown in fig. 2, the third fin 7 is disposed in a radial direction of the third sleeve 13 and connected to a circumferential inner wall of the third sleeve 13.
It can be understood that the third fin 7 is used for increasing the heat transfer area of burning tail gas, make full use of tail gas heat, improve the whole thermal efficiency of device. Specifically, as shown in fig. 2, the number of the third fins 7 is 6, and a material is preferably a copper-based alloy to increase the thermal conductivity.
The invention also provides an autothermal palladium membrane purification method, which comprises the following steps:
s1, closing a first valve 42, a third valve 52 and a fourth valve 54, opening a second valve 44, connecting a crude hydrogen gas inlet 45 by using vacuumizing equipment, vacuumizing the interiors of a first cavity, a second cavity and a third cavity to 0.01-0.05 MPa, and then closing the second valve 44;
s2, opening the first valve 42, introducing crude hydrogen gas along the crude hydrogen gas inlet 45, introducing air from the air inlet 46, igniting the mixed gas in the heating element 31 to heat the purification assembly 2, and discharging the combusted tail gas through the tail gas outlet 56;
s3, controlling the flow rate of the first valve 42, and monitoring the temperature of the palladium membrane purification tube 212 through the temperature measuring part 6, so that the temperature of the palladium membrane purification tube 212 is maintained at 350-400 ℃;
s4, opening the second valve 44, the third valve 52 and the fourth valve 54 to enable the crude hydrogen to enter the palladium membrane purification pipe 212, discharging the hydrogen from the first gas outlet pipe 51 after purification, and discharging purified tail gas and combusted tail gas from a tail gas outlet 56;
s5, closing the third valve 52 and the fourth valve 54, vacuumizing the interiors of the first cavity, the second cavity and the third cavity to 0.01-0.05 MPa according to the step in the S1, and closing the first valve 42 and the second valve 44 to naturally cool the purifying part 21.
According to the specific working process, the second sleeve 12 is arranged in the first sleeve 11, the third sleeve 13 is arranged in the second sleeve 12, the interior of the first sleeve 11 is divided into a first cavity, a second cavity and a third cavity which are communicated with each other, at least one purifying piece 21 is arranged in the second cavity and used for purifying crude hydrogen gas flowing through the second cavity, the heating piece 31 is uniformly arranged in the first cavity and used for providing a combustion space for the crude hydrogen gas and transferring heat generated by the combustion of the crude hydrogen gas to the purifying assembly 2, so that the purifying assembly 2 is uniformly heated, the purifying piece 21 is favorable for purifying the crude hydrogen gas introduced into the purifying assembly, and the structure combines a palladium membrane purifier with a hydrogen catalytic combustion technology and heats the palladium membrane purifier by using the crude hydrogen catalytic combustion and tail gas thereof.
When the user uses the device, the first valve 42, the third valve 52 and the fourth valve 54 are firstly closed, the second valve 44 is opened, the vacuumizing equipment is utilized to be connected with the crude hydrogen gas inlet 45, the interiors of the first cavity, the second cavity and the third cavity are vacuumized to 0.01-0.05 MPa, and then the second valve 44 is closed; then opening the first valve 42, introducing crude hydrogen gas along the crude hydrogen gas inlet 45, introducing air from the air inlet 46, igniting the mixed gas in the heating element 31 to heat the purification component 2, discharging the combusted tail gas through the tail gas outlet 56, controlling the flow rate of the first valve 42, and monitoring the temperature of the palladium membrane purification tube 212 through the temperature measuring element 6 to maintain the temperature of the palladium membrane purification tube 212 at 350-400 ℃; then the second valve 44, the third valve 52 and the fourth valve 54 are opened, so that the crude hydrogen enters the palladium membrane purification pipe 212, the hydrogen is discharged from the first gas outlet pipe 51 after purification, and the purified tail gas and the combusted tail gas are both discharged from the tail gas outlet 56; and finally, closing the third valve 52 and the fourth valve 54, vacuumizing the interiors of the first cavity, the second cavity and the third cavity to 0.01-0.05 MPa according to the step in the step S1, and closing the first valve 42 and the second valve 44 to naturally cool the purifying part 21.
Such structure combines together palladium membrane purifier and hydrogen catalytic combustion technique, uses crude hydrogen catalytic combustion and tail gas to heat palladium membrane purifier, solves among the prior art because of the condition that does not possess outside electric energy or other heating methods to lead to the device can't carry out the technical problem purified to hydrogen.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (7)

1. An autothermal palladium membrane purification device comprising:
the sleeve assembly comprises a first sleeve, a second sleeve, a third sleeve, a first sealing plate and a second sealing plate, wherein the first sleeve is arranged in the second sleeve, the second sleeve is arranged in the third sleeve, the interior of the first sleeve is divided into a first cavity, a second cavity and a third cavity which are communicated with each other, the first cavity, the second cavity and the third cavity are sequentially arranged along the radial direction of the first sleeve, the first sealing plate and the second sealing plate are respectively connected to two ends of the first sleeve and used for sealing two ends of the first sleeve, and one end of the second sleeve and one end of the third sleeve are connected with the first sealing plate;
the gas inlet assembly comprises at least one first gas inlet pipe, at least one first valve, at least one second gas inlet pipe, at least one second valve, a crude hydrogen gas inlet and at least one air inlet, the first gas inlet pipe is communicated with the first cavity, connected to the first sealing plate and used for introducing crude hydrogen gas into the first cavity, the first valves are arranged in one-to-one correspondence with the first gas inlet pipes and arranged on the first gas inlet pipes, the second gas inlet pipe is communicated with the second cavity, connected to the first sealing plate and used for introducing crude hydrogen gas into the second cavity, the second valves are arranged in one-to-one correspondence with the second gas inlet pipes and arranged on the second gas inlet pipes, the crude hydrogen gas inlet is communicated with the first gas inlet pipe and the second gas inlet pipe, and the air inlet is communicated with the first gas inlet pipe;
the gas outlet assembly comprises at least one first gas outlet pipe, at least one third valve, at least one second gas outlet pipe, at least one fourth valve, a third gas outlet pipe and a tail gas outlet, the first gas outlet pipe is communicated with the second cavity and connected to the second sealing plate and used for discharging hydrogen purified by the purifying part, the third valves are arranged in one-to-one correspondence with the first gas outlet pipe and arranged on the first gas outlet pipe, the second gas outlet pipe is communicated with the second cavity and connected to the first sealing plate and used for discharging tail gas purified by the purifying part, the fourth valves are arranged in one-to-one correspondence with the second gas outlet pipe and arranged on the second gas outlet pipe, the third gas outlet pipe is communicated with the third cavity and connected to the second sealing plate and used for discharging tail gas combusted by the heating element, and the tail gas outlet is communicated with the first gas outlet pipe, the second gas outlet pipe and the third gas outlet pipe;
the purification assembly comprises at least one purification piece, the purification piece is arranged in the second cavity and is used for purifying the crude hydrogen gas flowing through the second cavity;
and the heating component comprises a heating element, the heating element is uniformly arranged in the first cavity and used for providing a space for burning the crude hydrogen gas and transferring the heat generated by burning the crude hydrogen gas to the purification component so as to ensure that the purification component is uniformly heated.
2. The self-heating palladium membrane purification device according to claim 1, wherein the purification member comprises a fourth sleeve and at least one palladium membrane purification tube, the fourth sleeve is disposed in the second cavity and uniformly arranged along the circumferential direction of the second sleeve, and the palladium membrane purification tubes are disposed along the axial direction of the first sleeve and uniformly disposed in the fourth sleeve.
3. The autothermal palladium membrane purification device of claim 1, wherein the heating element includes at least two first fins, at least two second fins and a combustion catalyst, the first fins are arranged on the circumferential inner wall of the first sleeve along the radial direction of the first sleeve and are connected with the inner wall of the first sleeve and the outer wall of the second sleeve, the second fins are arranged between two adjacent first fins, the second fins are connected with the inner wall of the first sleeve and the outer wall of the second sleeve, and the combustion catalyst is uniformly coated on the second fins.
4. The autothermal palladium membrane purification device of claim 1, wherein the heating element further comprises a screen uniformly disposed within the first cavity and connected to both the inner wall of the first sleeve and the outer wall of the second sleeve at the opposite end.
5. The autothermal palladium membrane purification device of claim 1, further comprising a temperature measurement member, wherein the temperature measurement member is connected to the outer wall of the first sleeve and the measurement end of the temperature measurement member is disposed in the second cavity.
6. The self-heating palladium membrane purification device according to claim 5, further comprising at least one third fin disposed radially of the third sleeve and connected to the inner circumferential wall of the third sleeve.
7. An autothermal palladium membrane purification method, according to any one of claims 1 to 6, characterized by comprising the steps of:
s1, closing the first valve, the third valve and the fourth valve, opening the second valve, connecting the second valve with the crude hydrogen gas inlet by using vacuumizing equipment, vacuumizing the interiors of the first cavity, the second cavity and the third cavity to 0.01MPa to 0.05MPa, and then closing the second valve;
s2, opening the first valve, introducing crude hydrogen gas along a crude hydrogen gas inlet, introducing air from the air inlet, igniting the mixed gas in a heating element to heat the purification assembly, and discharging the combusted tail gas through the tail gas outlet;
s3, controlling the flow rate of the first valve, and monitoring the temperature of the palladium membrane purification tube through the temperature measurement piece to enable the temperature of the palladium membrane purification tube to be maintained at 350-400 ℃;
s4, opening the second valve, the third valve and the fourth valve to enable crude hydrogen gas to enter the palladium membrane purification pipe, purifying the crude hydrogen gas, discharging the hydrogen gas through the first gas outlet pipe, and discharging purified tail gas and combusted tail gas through the tail gas outlet;
s5, closing the third valve and the fourth valve, vacuumizing the first cavity, the second cavity and the third cavity to 0.01MPa to 0.05MPa according to the step S1, and closing the first valve and the second valve to naturally cool the purification piece.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110171805A (en) * 2019-06-26 2019-08-27 中国计量大学 A kind of detection method of hydrogen purification apparatus and its purifying hydrogen efficiency

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JPH10203803A (en) * 1997-01-20 1998-08-04 Ngk Insulators Ltd Apparatus for recovery, purification and storage of hydrogen gas
CN111483979A (en) * 2020-04-30 2020-08-04 上海齐耀动力技术有限公司 Hydrogen purification device and method with independently heated feed gas and palladium membrane purifier

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110171805A (en) * 2019-06-26 2019-08-27 中国计量大学 A kind of detection method of hydrogen purification apparatus and its purifying hydrogen efficiency

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