CN112875647B - Method for producing hydrogen by catalysis at room temperature - Google Patents

Method for producing hydrogen by catalysis at room temperature Download PDF

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CN112875647B
CN112875647B CN202110179506.3A CN202110179506A CN112875647B CN 112875647 B CN112875647 B CN 112875647B CN 202110179506 A CN202110179506 A CN 202110179506A CN 112875647 B CN112875647 B CN 112875647B
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physical vapor
vapor deposition
metal
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room temperature
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习卫
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Tianjin University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
    • C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
    • C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
    • C01B3/40—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts characterised by the catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/52—Gold
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/755—Nickel
    • B01J35/40—
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
    • C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/10—Catalysts for performing the hydrogen forming reactions
    • C01B2203/1041—Composition of the catalyst
    • C01B2203/1047—Group VIII metal catalysts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/10—Catalysts for performing the hydrogen forming reactions
    • C01B2203/1041—Composition of the catalyst
    • C01B2203/1047—Group VIII metal catalysts
    • C01B2203/1052—Nickel or cobalt catalysts
    • C01B2203/1058—Nickel catalysts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/10—Catalysts for performing the hydrogen forming reactions
    • C01B2203/1041—Composition of the catalyst
    • C01B2203/1082—Composition of support materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Abstract

The invention provides a method for producing hydrogen by catalysis at room temperature, which comprises the following steps: s1, providing a carrier; s2, growing metal nano particles by using a physical vapor deposition method, wherein the interplanar spacing expansion rate of the metal nano particles is more than 8%; s3, catalytic hydrogen production; and packaging the carrier carrying the metal nano particles into a plastic pipe, firstly introducing pure argon to flush a pipeline for 10-100 minutes, and then introducing pure methane gas with one atmospheric pressure at room temperature to perform catalytic reaction to obtain hydrogen. The invention utilizes the nano material with expanded crystal lattice prepared by the physical vapor deposition method to catalyze the lower hydrocarbon (such as methane) to prepare hydrogen at room temperature. The realization of the room-temperature catalytic hydrogen production method is expected to really promote the industrialization of methane hydrogen production and provide clean and efficient energy for the development of national economy.

Description

Method for producing hydrogen by catalysis at room temperature
Technical Field
The invention relates to the technical field of energy, in particular to a method for producing hydrogen by catalysis at room temperature.
Background
One of the major challenges with the continued growth of the global population and economy is the increased energy demand and the limitation of greenhouse gas emissions. With the large consumption of fossil fuels, the search for new energy sources is imperative. Methane is a main component of natural gas, biogas, combustible ice, oil and gas fields and coal mine pit gas, wherein the methane contained in the natural gas is over 167.9 billion cubic meters, and with the development of hydraulic fracturing technology and the development of shale gas, the future recoverable reserves and supply of the natural gas will be further increased. However, at present the main use of methane is as a primary energy source, i.e. it is directly combusted to provide energy. Methane itself has a strong greenhouse effect and, when it is used as a primary energy source, contributes to 1/5 of the global carbon dioxide emission. Therefore, how to prepare clean energy by taking methane as a raw material is very important.
At present, the main way for efficiently and cleanly utilizing methane is to prepare hydrogen from methane. Hydrogen has been considered one of the greenest fuels with a high heating value and non-polluting properties. And global statistics indicate that 48% of the hydrogen is currently produced from methane (natural gas) conversion. Although there are many methods for producing hydrogen from methane, only thermocatalytic CH is considered for greenhouse gas emission and economic problems thereof 4 Direct decomposition for preparing H 2 The method is a hydrogen production method with zero carbon emission, and is the most promising hydrogen production method with industrial prospect.
Due to the extremely high symmetry of the methane molecule, this stable non-polar structure results in low polarizability and extremely high dissociation energy of carbon-hydrogen bonds (439.3 kJ/mol). Various current catalytic attempts have also failed to effectively lower the temperature for methane cracking, requiring high temperatures above 650 ℃ to effectively activate the methane molecules. And the high energy consumption and the economic cost of factory maintenance and the like brought by high-temperature catalysis enable the product to have no economic advantages at all. Therefore, the research on the hydrogen production from methane at low temperature and even room temperature reduces the international political pressure brought by carbon dioxide emission, and the realization of the green sustainable development has important significance to China.
Disclosure of Invention
In view of this, the embodiment of the present invention provides a method for producing hydrogen by catalysis at room temperature, so as to solve the problems in the prior art.
According to a first aspect, embodiments of the present invention provide a method for producing hydrogen by room-temperature catalysis, the method comprising the following steps:
s1, providing a carrier;
wherein the support comprises a common carbon paper or an ultra-thin carbon film;
s2, growing metal nano particles by using a physical vapor deposition method;
preparing metal target materials into metal nano particles by a physical vapor deposition method, and uniformly dispersing the metal nano particles on the carrier, wherein the method specifically comprises the following steps:
adjusting the power in the physical vapor deposition process to be 1-10W, the argon flow to be 50-100 standard milliliters/minute and the deposition time to be 1-10 s to obtain metal nano particles with the interplanar spacing expansion rate of more than 8 percent, wherein the average particle size of the metal nano particles is 2-7nm; wherein, the calculation formula of the interplanar spacing expansion rate is as follows:
Figure BDA0002941031120000021
s3, catalytic hydrogen production;
packaging the carrier loaded with the metal nano particles into a plastic pipe, firstly introducing pure argon to flush a pipeline for 10-100 minutes, and then introducing pure methane gas with one atmospheric pressure at room temperature to perform catalytic reaction to obtain hydrogen, wherein the chemical reaction equation of the catalytic reaction is as follows:
2CH 4 →H 2 +C 2 H 6 ，C 2 H 6 →H 2 +C 2 H 4 ，C 2 H 4 →H 2 +C 2 H 2 ，C 2 H 2 →H 2 +2C。
preferably, the metal target comprises a gold, iron, or nickel target.
Preferably, the physical vapor deposition method includes: one or more of vacuum evaporation, sputtering coating, arc plasma coating, ion coating and molecular beam epitaxy.
Preferably, the purity of the metal target material is more than 99.99%.
Preferably, the power in the physical vapor deposition process in step S2 is 10W, the deposition time is 10S, the metal target material includes gold, and the interplanar spacings of the metal nanoparticles {111} and {200} are respectively 10W
Figure BDA0002941031120000022
And
Figure BDA0002941031120000023
the {111} and {200} interplanar spacing expansion ratios were 12% and 12%, respectively.
Preferably, in the step S2, the power in the physical vapor deposition process is 1W, the deposition time is 5S, the metal target material includes gold, and the spacing between {111} crystallographic planes of the metal nanoparticles is
Figure BDA0002941031120000024
(111) the interplanar spacing expansion ratio was 8%, and the average particle diameter of the metal nanoparticles was 2nm.
Preferably, in the step S2, the power in the physical vapor deposition process is 10W, the deposition time is 1S, the metal target material includes nickel, and the spacing between {111} crystallographic planes of the metal nanoparticles is
Figure BDA0002941031120000031
The {111} interplanar spacing expansion rate was 10%.
The invention utilizes the gold, iron, nickel and other nano materials with expanded lattices prepared by a physical vapor deposition method to catalyze lower hydrocarbons (such as methane) to prepare hydrogen at room temperature. The realization of the room-temperature catalytic hydrogen production method is expected to really promote the industrialization of methane hydrogen production and provide clean and efficient energy for the development of national economy.
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The features and advantages of the present invention will be more clearly understood by reference to the accompanying drawings, which are illustrative and not to be construed as limiting the invention in any way, and in which:
FIG. 1 shows the result of mass spectrometry of hydrogen production from methane catalyzed by lattice-expanded gold particles at room temperature.
FIG. 2 shows the morphology characterization of lattice-expanded gold particles before and after hydrogen production from methane catalyzed at room temperature.
FIG. 3 shows the transmission electron image of the condenser before the gold particles produced by physical vapor deposition under 1W and 5s conditions are not reacted.
FIG. 4 is a transmission electron image of a condenser before the nickel particles produced by physical vapor deposition under 10W for 1s are not reacted.
FIG. 5 shows the morphology characterization of the lattice-expanded nickel particles before and after catalyzing hydrogen production from methane at room temperature.
FIG. 6 shows the comparison of mass spectrum results of different kinds of lattice-expanding particles in the present invention catalyzing methane to produce hydrogen.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
The catalyst generally has a size effect, the smaller the size, the higher the catalytic efficiency. On the other hand, a catalyst having stress strain would also have an unexpectedly superior catalytic effect. The invention utilizes the nano materials with expanded lattices, such as gold, iron, nickel and the like, prepared by a physical vapor deposition method to catalyze the lower hydrocarbons (such as methane) to prepare hydrogen at room temperature. The realization of the room-temperature catalytic hydrogen production method is expected to really promote the industrialization of methane hydrogen production and provide clean and efficient energy for the development of national economy.
The invention provides a method for producing hydrogen by catalysis at room temperature, which comprises the following steps:
s1, providing a carrier;
in this step, the support comprises a carbon paper support. In a specific embodiment, the carbon paper support comprises a common carbon paper or an ultra-thin carbon film.
S2, growing metal nanoparticles by using a physical vapor deposition method;
in the step, the metal target material is prepared into small nano-metal particles by a physical vapor deposition method, and the small nano-metal particles are uniformly dispersed on the carrier. The metal target comprises gold, iron, nickel and other targets, and the purity of the metal target is more than 99.99%. In a particular embodiment, the physical vapor deposition method includes: one or more of vacuum evaporation, sputtering coating, arc plasma coating, ion coating and molecular beam epitaxy.
In the step, parameters such as power, argon flow, deposition time and the like in the deposition process are regulated and controlled, so that the prepared metal nanoparticles have expanded lattice lattices.
In one embodiment, the power of the PVD process is 1-10W, the argon flow is 50-100 standard milliliters per minute (sccm), and the deposition time is 1-10 s to control the particle size.
FIG. 2 (a) shows a transmission electron mirror image, an electron diffraction pattern and a high-resolution image of the gold particles prepared by physical vapor deposition under 10W and 10s before reaction, and analysis results of diffraction and high-resolution images show that the crystal face spacing expansion of the gold particles {111} and {200} exceeds 10%. Specifically, the theoretical value of the interplanar spacing of the gold particles is {111} and {200}, namely
Figure BDA0002941031120000041
And
Figure BDA0002941031120000042
and the spacing between the crystal planes of the gold particles {111} and {200} is measured by an electron diffraction experiment to be
Figure BDA0002941031120000043
And
Figure BDA0002941031120000044
the expansion ratios of {111} and {200} interplanar spacings were 12% and 12%. Wherein, the calculation formula of the interplanar spacing expansion rate is as follows:
Figure BDA0002941031120000045
FIG. 3 shows a transmission electron mirror image of a condenser before the gold particles prepared by physical vapor deposition under 1W and 5s conditions are not reacted. The analysis result showed that the gold particles had a {111} interplanar spacing of
Figure BDA0002941031120000046
Compared with the theoretical spacing
Figure BDA0002941031120000047
Figure BDA0002941031120000048
It expands by 8%.
FIG. 4 shows a transmission electron mirror image of a condenser before the nickel particles produced by physical vapor deposition under 10W for 1s are not reacted. The analysis result showed that the nickel particles had a {111} interplanar spacing of
Figure BDA0002941031120000049
Compared with the theoretical spacing
Figure BDA0002941031120000051
It expands by 10%.
S3, catalytic hydrogen production;
in the step, the carbon paper loaded with the expanded lattice metal nano material is packaged into a reaction bin, pure argon is firstly introduced to flush a pipeline for 10-100 minutes, and then pure methane gas with one atmospheric pressure is introduced at room temperature to carry out a catalytic experiment. The reaction bin comprises a plastic pipe.
In a specific embodiment, the tail gas end of the reaction chamber is connected with a mass spectrometer for detecting tail gas components. FIG. 1 shows the mass spectrometry results of hydrogen production by catalyzing methane at room temperature with lattice-expanded gold particles, and the stability test thereof. Wherein the circular line is the methane mass spectrum signal, the square line is the hydrogen mass spectrum signal, and the triangular line is the ethane mass spectrum signal. The mass spectrum result shows that the lattice expanded gold particles realize the hydrogen production by catalyzing methane at room temperature. After more than forty hours of testing, the signal of methane hydrogen production has no obvious change. Among the chemical reactions that apparently occur in the present invention are:
2CH 4 →H 2 +C 2 H 6
the complete chemical reaction equation is as follows:
2CH 4 →H 2 +C 2 H 6 ，C 2 H 6 →H 2 +C 2 H 4 ，C 2 H 4 →H 2 +C 2 H 2 ，C 2 H 2 →H 2 +2C。
FIG. 2 shows the morphology characterization of the lattice-expanded gold particles before and after catalyzing methane to produce hydrogen at room temperature. Wherein, fig. 2 (a) is a transmission electron mirror image, an electron diffraction diagram and a high-resolution image before the gold particles are not reacted, and fig. 2 (b) is a morphology image of the gold particles after hydrogen production by catalyzing methane with the gold particles at room temperature. Obviously, the morphology of the gold particles is greatly changed in the process of catalyzing methane to produce hydrogen at room temperature.
FIG. 5 shows the morphology characterization of the lattice-expanded nickel particles before and after catalyzing hydrogen production from methane at room temperature. Obviously, the morphology of the nickel particles is greatly changed in the process of catalyzing methane to produce hydrogen at room temperature.
FIG. 6 shows the comparison of mass spectrum results of different kinds of lattice-expanding particles in the present invention catalyzing methane to produce hydrogen. Au (gold), fe (iron) and Ni (nickel) are mass spectrum signals of catalyzing methane to produce hydrogen at room temperature, wherein Fe 5nm refers to 5nm of average particle size, au 2nm refers to 2nm of average particle size, and Ni 7nm refers to 2nm of average particle size. NPG is a mass spectrum signal of the nanoporous gold catalyzing methane to produce hydrogen at 346 ℃, and is used as a control result. The result clearly shows that the hydrogen production effect of the Au 2nm room temperature catalysis methane obtained under the conditions that the sputtering power is 1W and the sputtering time is 5s, wherein the {111} interplanar spacing is expanded by 8%, is very good, because the small particles have the advantage that the structure that the surface atomic arrangement deviates from the lattice point position possibly contributes to catalyzing methane besides the lattice expansion.
The above-described embodiments are merely illustrative of the principles of the present invention and its efficacy, rather than limiting the invention, and it will be apparent to those skilled in the art that various modifications and variations can be made without departing from the spirit and scope of the invention, such modifications and variations being within the scope of the appended claims.

Claims (7)

1. A method for producing hydrogen by catalysis at room temperature is characterized by comprising the following steps:
s1, providing a carrier;
wherein the support comprises a common carbon paper or an ultra-thin carbon film;
s2, growing metal nano particles by using a physical vapor deposition method;
preparing metal target materials into metal nano particles by a physical vapor deposition method, and uniformly dispersing the metal nano particles on the carrier, wherein the method specifically comprises the following steps:
adjusting the power in the physical vapor deposition process to be 1-10W, the argon flow to be 50-100 standard milliliters/minute and the deposition time to be 1-10 s to obtain metal nano particles with the interplanar spacing expansion rate of 8-12 percent, wherein the average particle size of the metal nano particles is 2-7nm; wherein, the calculation formula of the interplanar spacing expansion rate is as follows:
Figure DEST_PATH_IMAGE002
；
s3, catalytic hydrogen production;
packaging the carrier loaded with the metal nano particles into a plastic pipe, firstly introducing pure argon to flush a pipeline for 10-100 minutes, and then introducing pure methane gas with one atmospheric pressure at room temperature to perform catalytic reaction to obtain hydrogen, wherein the chemical reaction equation of the catalytic reaction is as follows:
Figure DEST_PATH_IMAGE004
，C 2 H 6 →H 2 +C 2 H 4 ，C 2 H 4 →H 2 +C 2 H 2 ，C 2 H 2 →H 2 +2C。
2. the method of claim 1, wherein the metal target comprises a gold, iron, or nickel target.
3. The method of claim 1 or 2, wherein the physical vapor deposition method comprises: one or more of vacuum evaporation, sputtering coating, arc plasma coating, ion coating and molecular beam epitaxy.
4. The method according to claim 1 or 2, wherein the purity of the metal target is greater than 99.99%.
5. The method according to claim 1 or 2, wherein the power during physical vapor deposition in step S2 is 10W, the deposition time is 10S, the metal target comprises gold, the metal nanoparticles have a {111} and {200} interplanar spacing of 2.65 a and 2.28 a, respectively, and a {111} and {200} interplanar spacing expansion of 12%, respectively.
6. The method according to claim 1 or 2, characterized in that the power during physical vapor deposition in step S2 is 1W, the deposition time is 5S, the metal target comprises gold, the metal nanoparticles have a {111} interplanar spacing of 2.55 a, a {111} interplanar spacing expansion ratio of 8%, and the metal nanoparticles have an average particle diameter of 2nm.
7. The method according to claim 1 or 2, wherein the power during physical vapor deposition in step S2 is 10W and the deposition time is 1S, the metal target comprises nickel, the metal nanoparticles have a {111} interplanar spacing of 2.25 a and a {111} interplanar spacing expansion ratio of 10%.
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