CN212396398U - Composite membrane for hydrogen separation - Google Patents
Composite membrane for hydrogen separation Download PDFInfo
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- CN212396398U CN212396398U CN202021466536.XU CN202021466536U CN212396398U CN 212396398 U CN212396398 U CN 212396398U CN 202021466536 U CN202021466536 U CN 202021466536U CN 212396398 U CN212396398 U CN 212396398U
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Abstract
The utility model provides a complex film for hydrogen separation. The utility model discloses a complex film includes the supporter the both sides of supporter are equipped with vanadium carbide film respectively. The utility model discloses a complex film has excellent hydrogen catalysis dissociation performance, shows good stability in high temperature environment, has advantages such as hydrogen permeability is good, the hydrogen production is efficient, operating temperature range is wide, with low costs, has wide application prospect in high-purity hydrogen production field.
Description
Technical Field
The utility model belongs to the technical field of the hydrogen separation technique and specifically relates to a complex film for hydrogen separation is related to.
Background
In recent years, environmental issues worldwide have necessitated the search for new clean energy sources to replace traditional fossil fuels. Hydrogen has attracted extensive attention as a zero-emission fuel, a carrier of clean energy. The membrane method for producing high-purity hydrogen is a feasible and efficient method in the industries of chemical engineering, petrifaction and the like.
Among the hydrogen separation membranes, palladium membranes and palladium alloy membranes, although exhibiting good hydrogen permeation performance (high hydrogen permeation performance and unique hydrogen selectivity), have the following drawbacks: 1) pure Pd membrane exposed to H2Alpha-beta phase transformation can occur at the temperature of lower than 300 ℃, so that hydrogen embrittlement is caused; 2) the high-temperature heat treatment may cause cracks/pinholes on the Pd-based alloy film; 3) the impurity gases in the purification environment compete with the palladium alloy surface for adsorption and formation of palladium compounds, resulting in Pd poisoning. Therefore, the thermal and chemical stability of palladium/palladium alloy membranes is one of the major obstacles to their commercial application. In addition, palladium metal reserves are low and expensive, further limiting the commercial application of the alloy membrane. Therefore, a non-noble metal material capable of replacing Pd alloys is sought.
Body-centered cubic (bcc) metals of niobium, tantalum, vanadium, etc. have theoretical hydrogen permeabilities higher than that of face-centered cubic (fcc) palladium metal and costs 2-3 orders of magnitude less than palladium, limiting their development by a negligible catalytic activity on hydrogen dissociation relative to palladium metal. Currently, the typical solution to this problem is to plate a thin platinum group metal hydrogen dissociation catalyst layer on both sides of the bulk membrane metal. Palladium and palladium alloys are the most commonly used catalyst layers, however, they increase the cost of the membrane and reduce the hydrogen transport rate due to the lower permeability of hydrogen leaving the catalyst layer. More importantly, the use of these metal catalysts limits the operable temperature range of the membrane due to the gradual decrease in hydrogen permeability resulting from intermetallic diffusion between the Pd and BCC metals due to high temperatures.
In view of this, the utility model is especially provided.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a complex film for hydrogen separation, this complex film have excellent hydrogen catalysis dissociation performance, show good stability in high temperature environment, have that hydrogen permeability is good, produce hydrogen efficient, operating temperature range is wide, advantage such as with low costs.
The utility model provides a complex film for hydrogen separation, including the supporter the both sides of supporter are equipped with vanadium carbide film respectively.
Further, the support is a compact metal layer, a compact metal alloy layer, a porous metal layer or a porous ceramic layer.
Further, the dense metal layer is a vanadium metal layer, a niobium metal layer, a tantalum metal layer, a molybdenum metal layer, a nickel metal layer, a titanium metal layer, a palladium metal layer or a platinum metal layer.
Further, the dense metal alloy layer is a vanadium-nickel alloy layer, a vanadium-copper alloy layer, a vanadium-iron alloy layer, a vanadium-aluminum alloy layer, a vanadium-cobalt alloy layer, a vanadium-molybdenum alloy layer, a vanadium-tungsten alloy layer, a vanadium-titanium-nickel alloy layer, a vanadium-iron-aluminum alloy layer, a vanadium-molybdenum-tungsten alloy layer, a niobium-titanium-nickel alloy layer, a niobium-titanium-cobalt alloy layer or a niobium-molybdenum-tungsten alloy layer.
Further, the porous metal layer is a porous stainless steel layer or a porous titanium-aluminum alloy layer.
Further, the porous ceramic layer is a porous alumina layer, a porous zirconia layer or a zeolite layer.
Further, the thickness of the support is 20-2000 μm.
Further, the support body is sheet-shaped or tubular.
Further, the thickness of the vanadium carbide film is 5-500 nm.
Further, the thickness of the vanadium carbide film is 10-60 nm.
The hydrogen separation composite membrane of the utility model is provided with the vanadium carbide films on the two sides of the support body respectively, which avoids using noble metal Pd and alloy thereof and reduces the cost of the composite membrane; the composite membrane has high hydrogen catalytic dissociation performance, still shows good stability in a high-temperature environment, improves the hydrogen permeability of the composite membrane, solves the problems of narrow operation temperature range and the like of the composite membrane, and has wide application prospect in the field of high-purity hydrogen production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the technical solutions in the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural view of the composite membrane of the present invention;
FIG. 2 is a schematic diagram of the hydrogen permeation process of the composite membrane of the present invention;
fig. 3 is a single side cross-sectional SEM image of the composite membrane of the present invention;
FIG. 4 is a surface XRD pattern of the composite film of the present invention;
FIG. 5 is a graph showing hydrogen permeation flow rates of composite membranes of examples 1 to 3 and comparative examples 1 to 2;
FIG. 6 is a graph showing the hydrogen permeation durability of the composite membrane of the test example.
Description of reference numerals:
1: a support body; 2: a vanadium carbide film.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms also include the plural forms unless the context clearly dictates otherwise, and further, it is understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, devices, components, and/or combinations thereof.
The technical solution of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Example 1
As shown in fig. 1, the composite membrane for hydrogen separation of the present embodiment includes a support 1, and vanadium carbide thin films 2 are respectively disposed on both sides of the support 1; wherein the support body 1 is a commercially available pure vanadium foil wafer with the thickness of 100 mu m and the diameter of 20mm, and is subjected to surface polishing treatment; the molar ratio of vanadium to carbon in the vanadium carbide film 2 is 1: 1.
the composite membrane for hydrogen separation of the present example may be prepared by:
1. support pretreatment
Ultrasonic cleaning vanadium foil with analytically pure acetone and anhydrous ethanol for 10min, repeating for 2-3 times, washing with deionized water for 1 min, and drying in a drying oven at 120 deg.C.
2. Cleaning of support
Respectively arranging the pretreated vanadium foil and a vanadium carbide (atomic ratio is 1:1) target material on a sample table and a target head of a magnetron sputtering coating chamber, pumping the vacuum degree of the chamber to be below 10-4Pa by using a molecular pump, setting an electron beam current of 50mA, an argon gas flow rate of 5sccm and a chamber pressure of 0.5Pa, and cleaning the surface of the vanadium foil for 30min by using an argon ion beam.
3. Vanadium carbide plated film
Heating the vanadium foil to 400 ℃, setting the bias voltage to be 0, sputtering power to be 50W, chamber pressure to be 1.0Pa, pre-sputtering the vanadium carbide target for 5min, after cleaning the pollutants on the surface of the target, increasing the sputtering power to 200W for 20min, and plating a layer of vanadium carbide film on the surface of the vanadium foil.
And then, turning over the vanadium foil, repeating the steps, plating a layer of vanadium carbide film on the other side of the vanadium foil, and taking out to obtain the composite film.
The hydrogen permeation process of the composite membrane is shown in figure 2, the SEM image of the object cross section is shown in figure 3, and the surface characterization XRD is shown in figure 4. The results in FIG. 3 show that: the compactness of the magnetron sputtering vanadium carbide film is good; the results in FIG. 4 show that: the vanadium carbide film with the vanadium-carbon ratio of 1:1 is prepared by magnetron sputtering, and the crystallinity of the vanadium carbide film is highest under the condition that the temperature of a matrix is 400 ℃.
The relationship between the hydrogen permeation performance and the temperature obtained by the hydrogen permeation experiment performed by the hydrogen permeation device is shown in fig. 5. The results in FIG. 5 show that: the hydrogen permeability of the composite membrane of the embodiment is better than that of Pd at various temperatures, the hydrogen permeability is increased along with the increase of the temperature, and particularly the hydrogen permeability at 873K
Is 9.5 multiplied by 10-8mol H2 m-1s-1Pa-0.5Basically approaches to a theoretical value, and has excellent high-temperature hydrogen permeability and high-temperature stability.
Example 2
The composite membrane for hydrogen separation of the embodiment comprises a support body, wherein vanadium carbide films are respectively arranged on two sides of the support body; wherein the support body is a commercially available pure vanadium foil wafer, the thickness of the support body is 100 mu m, the diameter of the support body is 20mm, and the surface of the support body is polished; the molar ratio of vanadium to carbon in the vanadium carbide film is 1: 1.
the composite film of this example can be prepared in the same manner as in example 1, except that the vanadium foil is heated to 200 ℃ in step 3 during the coating process, and the other steps and parameters are the same as those in example 1.
Surface characterization XRD of the composite film of this example is shown in fig. 4; from fig. 4, it can be seen that the vanadium carbide film with the vanadium-carbon ratio of 1:1 is prepared by magnetron sputtering, and the crystallinity of the prepared vanadium carbide film is the lowest under the condition that the temperature of the matrix is 200 ℃.
The relationship between the hydrogen permeability and the temperature of the composite membrane of the present example is shown in fig. 5; the results in FIG. 5 show that: the composite membrane of this example is hydrogen permeable at 873K
Is 4.5 multiplied by 10-8mol H2 m-1s-1Pa-0.5Is far higher than Pa, and has excellent high-temperature hydrogen permeability.
Example 3
The composite membrane for hydrogen separation of the embodiment comprises a support body, wherein vanadium carbide films are respectively arranged on two sides of the support body; wherein the support body is a commercially available pure vanadium foil wafer, the thickness of the support body is 100 mu m, the diameter of the support body is 20mm, and the surface of the support body is polished; the molar ratio of vanadium to carbon in the vanadium carbide film is 1: 1.
the composite film of this example can be prepared in the same manner as in example 1, except that the temperature of the vanadium foil is controlled to room temperature in step 3 during the coating process, in the same manner as in example 1.
Surface characterization XRD of the composite film of this example is shown in fig. 4; the results in FIG. 4 show that: the vanadium carbide film with the vanadium-carbon ratio of 1:1 is prepared by magnetron sputtering, and under the condition that the matrix temperature is room temperature, the vanadium carbide film has relatively high crystallinity and higher grain boundary density, and is beneficial to the transmission of hydrogen atoms in the film.
The relationship between the hydrogen permeability and the temperature of the composite membrane of the present example is shown in fig. 5; the results of FIG. 5 show that the hydrogen permeability of the composite membrane of this example is better than Pd at various temperatures, and the hydrogen permeability increases with the temperatureHydrogen permeability, especially at 873K
Is 8.9 multiplied by 10-8mol H2 m-1s-1Pa-0.5Basically approaches to a theoretical value, and has excellent high-temperature hydrogen permeability and high-temperature stability.
Comparative example 1
The composite membrane for hydrogen separation of the comparative example includes a support, and Pd thin films are respectively provided on both sides of the support; wherein the support is a commercially available pure vanadium foil wafer with the thickness of 100 mu m and the diameter of 20mm, and is subjected to surface polishing treatment.
The preparation method of the composite membrane for hydrogen separation of this comparative example was as follows:
1. support pretreatment
Ultrasonic cleaning vanadium foil with analytically pure acetone and anhydrous ethanol for 10min, repeating for 2-3 times, washing with deionized water for 1 min, and drying in a drying oven at 120 deg.C.
2. Cleaning of support
Respectively arranging the pretreated vanadium foil and the pure Pd target material on a sample table and a target head of a magnetron sputtering coating chamber, and pumping the vacuum degree of the chamber to 10 by using a molecular pump-4And (4) below Pa, setting an electron beam current of 50mA, an argon gas flow rate of 5sccm and a chamber pressure of 0.5Pa, and cleaning the surface of the vanadium foil for 20min by using an argon ion beam.
3. Pd-plated thin film
Heating the vanadium foil to 400 ℃, setting the bias voltage to be 0, sputtering power to be 50W, chamber pressure to be 1.0Pa, pre-sputtering the Pd target for 5min, after cleaning the pollutants on the surface of the target, increasing the sputtering power to 200W for 20min, and plating a Pd film on the surface of the vanadium foil.
And then, turning over the vanadium foil, repeating the steps, plating a Pd film on the other side of the vanadium foil, and taking out to obtain the composite film.
The relationship between the hydrogen permeation performance and the temperature obtained by the hydrogen permeation experiment performed by the hydrogen permeation device is shown in fig. 5. The results in FIG. 5 show that: the hydrogen permeability of the composite membrane of the embodiment at high temperature is better than that of the Pd-based composite membrane of the comparative example, and although the Pd-based composite membrane has certain permeability, the Pd-based composite membrane has poor high-temperature stability, is easy to be poisoned and failed and is expensive.
Comparative example 2
The composite membrane for hydrogen separation of this comparative example includes a support body, and Mo is provided on both sides of the support body2C, a film; wherein the support is a commercially available pure vanadium foil wafer with the thickness of 100 mu m and the diameter of 20mm, and is subjected to surface polishing treatment.
The preparation method of the composite membrane for hydrogen separation of this comparative example was as follows:
1. support pretreatment
Ultrasonic cleaning vanadium foil with analytically pure acetone and anhydrous ethanol for 10min, repeating for 2-3 times, washing with deionized water for 1 min, and drying in a drying oven at 120 deg.C.
2. Cleaning of support
Mixing the pretreated vanadium foil and molybdenum carbide target material (Mo)2C) Respectively arranged on a sample stage and a target head of a magnetron sputtering coating chamber, and pumping the vacuum degree of the chamber to 10 by using a molecular pump-4And (4) below Pa, setting an electron beam current of 50mA, an argon gas flow rate of 5sccm and a chamber pressure of 0.5Pa, and cleaning the surface of the vanadium foil for 20min by using an argon ion beam.
3. Mo plating2C film
Heating vanadium foil to 400 ℃, setting bias voltage to be 0, sputtering power to be 50W, chamber pressure to be 1.0Pa, pre-sputtering the molybdenum carbide target for 5min, after cleaning treatment of pollutants on the surface of the target, increasing the sputtering power to 200W for 20min, and plating a layer of Mo on the surface of the vanadium foil2And C, film forming.
Then, turning over the vanadium foil, repeating the steps, and plating a layer of Mo on the other side of the vanadium foil2And C, taking out the film to obtain the composite film.
The relationship between the hydrogen permeation performance and the temperature obtained by the hydrogen permeation experiment performed by the hydrogen permeation device is shown in fig. 5. The results in FIG. 5 show that: mo of this comparative example2The hydrogen permeability of the C-based composite membrane at high temperature is not as good as that of the VC base of the embodimentA composite membrane.
Test examples
The composite membrane of example 1 was used for a hydrogen purification test as follows:
a hydrogen permeation device and a composite membrane material are utilized to form a set of hydrogen purification device, a hydrogen permeation mold is divided into an upstream portion and a downstream portion, and a composite membrane is placed between the two portions of the mold. In order to make the mold airtight and prevent the diaphragm from being subjected to a large stress concentration during the fastening, a porous nickel support was placed on the downstream side of the diaphragm, both sides were sealed with nickel alloy gaskets having an outer diameter of 20mm and an inner diameter of 12mm, and the airtightness was checked. The composite membrane sample is secured by bolts in the upstream and downstream dies, which are then attached to the equipment at the upstream and downstream ports. After the pipeline is connected, the pipeline and the interior of the mould are pumped into a vacuum state, the pipeline and the interior of the mould are heated to 873K at the speed of 5 ℃/min and are kept warm for 30min, so that the temperature of the interior of the mould and all parts of the composite membrane is uniform, then the vacuum valve is closed, and hydrogen-containing mixed gas with the pressure of 0.15MPa is filled. When the hydrogen absorption of the composite membrane reaches saturation, the pressure reading is stable, and the hydrogen permeability test is started: the upstream pressure was increased from 0.15MPa at intervals of 0.05MPa until the pressure was increased to 0.8MPa, and a stable hydrogen permeation flow rate value was recorded for each pressure, and the downstream pressure was maintained at 0.1MPa at all times.
In addition, the stability of the hydrogen permeation flow of the composite membrane is tested by the following method: another composite membrane which is not subjected to hydrogen permeation is taken, the previous preparation steps are the same as the previous steps, when a hydrogen permeation test is carried out, the temperature is kept at 873K, the upstream pressure is kept at 0.8MPa, the downstream pressure is kept at 0.1MPa, the hydrogen permeation test is carried out for 6 hours, and the change of the hydrogen permeation flow along with the time is recorded, and the result is shown in fig. 6.
After gas phase mass spectrum testing, the purity of the finally obtained hydrogen is more than 99.999 percent.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention.
Claims (10)
1. The composite membrane for hydrogen separation is characterized by comprising a support body, wherein vanadium carbide films are respectively arranged on two sides of the support body.
2. The composite membrane of claim 1, wherein the support is a dense metal layer, a dense metal alloy layer, a porous metal layer, or a porous ceramic layer.
3. The composite film of claim 2, wherein the densified metal layer is a vanadium metal layer, a niobium metal layer, a tantalum metal layer, a molybdenum metal layer, a nickel metal layer, a titanium metal layer, a palladium metal layer, or a platinum metal layer.
4. The composite film of claim 2, wherein the dense metal alloy layer is a vanadium-nickel alloy layer, a vanadium-copper alloy layer, a vanadium-iron alloy layer, a vanadium-aluminum alloy layer, a vanadium-cobalt alloy layer, a vanadium-molybdenum alloy layer, a vanadium-tungsten alloy layer, a vanadium-titanium-nickel alloy layer, a vanadium-iron-aluminum alloy layer, a vanadium-molybdenum-tungsten alloy layer, a niobium-titanium-nickel alloy layer, a niobium-titanium-cobalt alloy layer, or a niobium-molybdenum-tungsten alloy layer.
5. The composite membrane according to claim 2, wherein the porous metal layer is a porous stainless steel layer or a porous titanium aluminum alloy layer.
6. A composite membrane according to claim 2, wherein the porous ceramic layer is a porous alumina, zirconia or zeolite layer.
7. The composite membrane of claim 1, wherein the support has a thickness of 20 to 2000 μm.
8. The composite membrane of claim 1 wherein the support is sheet-like or tubular.
9. The composite film of claim 1, wherein the vanadium carbide thin film has a thickness of 5 to 500 nm.
10. The composite film of claim 9, wherein the vanadium carbide thin film has a thickness of 10 to 60 nm.
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| CN111841339A (en) * | 2020-07-23 | 2020-10-30 | 李新中 | Composite membrane for hydrogen separation and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111841339A (en) * | 2020-07-23 | 2020-10-30 | 李新中 | Composite membrane for hydrogen separation and preparation method and application thereof |
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Effective date of registration: 20220215 Address after: 241000 No. 4, Jinye Road, Sanshan Economic Development Zone, Wuhu City, Anhui Province Patentee after: Wuhu China hydrogen New Energy Technology Co.,Ltd. Address before: 130 Flourishing Street, Nangang District, Harbin City, Heilongjiang Province Patentee before: Li Xinzhong |
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