CN113941328B - Platinum/molybdenum dehydrogenation catalytic material, preparation method and application thereof - Google Patents

Platinum/molybdenum dehydrogenation catalytic material, preparation method and application thereof Download PDF

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CN113941328B
CN113941328B CN202111334685.XA CN202111334685A CN113941328B CN 113941328 B CN113941328 B CN 113941328B CN 202111334685 A CN202111334685 A CN 202111334685A CN 113941328 B CN113941328 B CN 113941328B
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platinum
molybdenum
dehydrogenation
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catalytic material
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CN113941328A (en
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陈琪
尹中南
刘冬妮
周子兵
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Jinhong Gas Co ltd
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    • 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
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/652—Chromium, molybdenum or tungsten
    • B01J23/6525—Molybdenum
    • 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
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/656—Manganese, technetium or rhenium
    • B01J23/6562—Manganese
    • 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
    • B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
    • B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/8993—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with chromium, molybdenum or tungsten
    • 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
    • C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage

Abstract

The invention discloses a platinum/molybdenum dehydrogenation catalytic material, a preparation method and application thereof, wherein the catalytic material comprises a carrier and a catalytic composition formed on the carrier, the catalytic composition accounts for 0.75-1.5% of the total mass of the catalytic material, and the catalytic composition comprises platinum elements and molybdenum elements. The dehydrogenation catalytic material disclosed by the invention effectively improves the dehydrogenation efficiency by optimally combining the active forming.

Description

Platinum/molybdenum dehydrogenation catalytic material, preparation method and application thereof
Technical Field
The invention relates to the technical field of liquid hydrogen storage catalytic dehydrogenation, in particular to a platinum/molybdenum dehydrogenation catalytic material, a preparation method and application thereof.
Background
The hydrogen energy is expected in recent decades due to a series of advantages such as cleanness, no pollution, high calorific value and the like, and is considered as an indispensable part for solving the energy problem and developing low-carbon economy by many people. Although hydrogen energy is being developed vigorously, the key issues of hydrogen production, hydrogen storage, and fuel cells are not well addressed. Particularly, as hydrogen storage which plays a bridge role between hydrogen preparation and application, no particularly mature hydrogen storage mode which can be widely applied exists. The existing vehicle-mounted hydrogen storage mode is a mode of storing hydrogen by utilizing a physical high-pressure hydrogen storage tank, and has many defects in the aspects of energy efficiency, volume hydrogen storage capacity, safety and the like. Therefore, the lack of efficient hydrogen storage materials can be said to be a bottleneck problem to be solved in the development of hydrogen energy.
The organic hydrogen storage liquid is one of the most possible solutions to the hydrogen storage problem, but the kinetics of hydrogen absorption and desorption is poor, at present, a noble metal catalyst is basically used for catalyzing the hydrogen absorption and desorption process, and different noble metals are often used in the hydrogenation process and the dehydrogenation process, so that the use cost is too high, and the practical application is difficult. Under the existing technical conditions, dehydrogenation is a strong endothermic and highly reversible reaction, although on one aspect, high temperature is favorable for dehydrogenation reaction, but hydrogen storage materials under high temperature poison catalysts due to side reactions such as cracking and carbon deposition, and meanwhile, most of the existing catalysts have complex compositions and can effectively play a certain catalytic role under the general conditions of needing multiple catalysts to be matched with specific carrier materials, particularly specific porous carrier materials, which greatly influences the application cost and the large-scale production of catalytic materials. For example, CN201410539305, a preparation method thereof, a hydrogenation catalyst and a dehydrogenation catalyst have the problems of low efficiency, complex catalyst composition and production, strict requirements on component matching of the catalyst, and the like.
Based on the application requirements of new energy carriers, the cycle efficiency and speed of hydrogen-carrying dehydrogenation of the hydrogen storage device greatly limit the application of the organic hydrogen storage liquid to hydrogen fuel cell vehicles.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a platinum/molybdenum dehydrogenation catalytic material, a preparation method and application thereof, which effectively improve dehydrogenation efficiency and greatly improve catalytic dehydrogenation capacity of a liquid hydrogen storage material by optimizing and combining active forming.
In order to achieve the above objects, embodiments of the present invention provide a platinum/molybdenum dehydrogenation catalytic material comprising a support and a catalytic composition formed on the support, the catalytic composition comprising 0.75 to 1.5% by mass of the total mass of the catalytic material, the catalytic composition comprising platinum element and molybdenum element.
In one or more embodiments of the invention, the mass ratio of platinum element to molybdenum element in the catalytic composition is 1: (0.5-2).
In one or more embodiments of the invention, the platinum element is derived from at least any one of: pt (NO) 3 ) 4 、H 2 PtCl 6 。
In one or more embodiments of the invention, the molybdenum element is derived from at least any one of: molybdic acid and molybdate.
In one or more embodiments of the invention, the vector is selected from any one of: alumina, tiO 2 、Cr 2 O 3 、MnO 2 、Fe 2 O 3 CoO, niO, cuO and ZrO 2 。
In one or more embodiments of the present invention, a method for preparing a platinum/molybdenum dehydrogenation catalytic material is characterized by comprising the steps of: preparing a mixed solution containing a platinum source and a molybdenum source; and mixing and soaking the carrier into the mixed solution, drying after full soaking, and sintering under the condition of oxygen deficiency.
In one or more embodiments of the present invention, the drying is drying at 80-100 degrees for 2-4 hours.
In one or more embodiments of the invention, the oxygen-deficient conditions are hydrogen conditions.
In one or more embodiments of the invention, the sintering is carried out under oxygen-deficient conditions at a temperature of 250 to 350 ℃ for 2 to 6 hours.
In one or more embodiments of the invention, the use of a platinum/molybdenum dehydrogenation catalytic material as described previously in liquid hydrogen storage technology.
Compared with the prior art, the platinum/molybdenum dehydrogenation catalytic material provided by the embodiment of the invention has the advantages of simple preparation, stable composition, simple composition of the matrix and the active ingredients, higher activity and toxicity resistance, and capability of effectively improving the catalytic dehydrogenation efficiency.
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FIG. 1 is a graph comparing the dehydrogenation performance of catalytic materials of varying compositions in accordance with one embodiment of the present invention.
Fig. 2 is a graph comparing the dehydrogenation efficiencies of catalytic materials for different supports according to one embodiment of the present invention.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
For effective comparison, the following examples show that the physical properties of the carriers are all in the same form: the particle size of the spherical porous particles is 3mm, and the specific surface area is 5 square meters per gram.
Example 1
Preparing a catalyst:
1. preparing a platinum nitrate/molybdic acid mixed solution with a certain concentration according to the following table, wherein the solvent is water; to obtain solution A
2. Soaking the solution A into an alumina carrier by using an equal-volume soaking method; obtaining a precursor B
3. Putting the precursor B into an oven to be dried for 2 hours at 100 ℃; obtaining a precursor C
4. Putting the precursor C into a tubular muffle furnace, introducing hydrogen, heating to 300 ℃, and keeping for 2 hours; obtaining the catalyst.
The dehydrogenation effect test method comprises the following steps:
1. weighing 40g of 18 hydrogen-dibenzyltoluene and 2g of catalyst, and adding into a high-temperature reaction kettle;
2. repeatedly replacing the high-temperature reaction kettle by using hydrogen; keeping normal pressure;
3. starting stirring (300-1500 pm), and starting heating up to 350 ℃ for keeping.
Figure GDA0003360153070000041
Figure GDA0003360153070000051
Wherein "-" indicates that the catalytic performance of the catalyst is non-catalytic.
As shown in fig. 1, the platinum/molybdenum dehydrogenation catalytic material according to the preferred embodiment of the present invention greatly increases the application cost of the catalytic material, aiming at the problems of complicated production process, high energy consumption, high cost of the dehydrogenation catalyst, complicated active component and carrier of the catalyst, and the need of using a large amount of expensive materials in the prior art.
Example 2
Preparing a catalyst:
1. preparing a platinum nitrate/molybdic acid mixed solution with a certain concentration according to the following table, wherein the solvent is absolute ethyl alcohol; to obtain solution A
2. Soaking the solution A into TiO by using an isovolumetric soaking method 2 A carrier; obtaining a precursor B
3. Putting the precursor B into an oven, and drying for 4 hours at 80 ℃; obtaining a precursor C
4. Putting the precursor C into a tubular muffle furnace, introducing hydrogen, heating to 325 ℃, and keeping for 5 hours; obtaining the catalyst.
The dehydrogenation effect test method comprises the following steps:
1. weighing 40g of 18 hydrogen-dibenzyltoluene and 2g of catalyst, and adding into a high-temperature reaction kettle;
2. repeatedly replacing the high-temperature reaction kettle by using hydrogen; keeping normal pressure;
3. starting stirring (300-1500 pm), and starting heating up to 350 ℃ for keeping.
Figure GDA0003360153070000052
Figure GDA0003360153070000061
Wherein "-" indicates that the catalytic activity is no catalytic effect.
Example 3
Preparing a catalyst:
1. preparing a platinum nitrate/molybdic acid mixed solution with a certain concentration according to the following table, wherein the solvent is water; to obtain solution A
2. Impregnating solution A into Cr by an isovolumetric impregnation method 2 O 3 A carrier; obtaining a precursor B
3. Putting the precursor B into an oven, and drying for 3 hours at 80 ℃; obtaining a precursor C
4. Putting the precursor C into a tubular muffle furnace, introducing hydrogen, heating to 275 ℃, and keeping for 4 hours; obtaining the catalyst.
The dehydrogenation effect test method comprises the following steps:
1. weighing 40g of 18 hydrogen-dibenzyltoluene and 2g of catalyst, and adding into a high-temperature reaction kettle;
2. repeatedly replacing the high-temperature reaction kettle by using hydrogen; keeping normal pressure;
3. starting stirring (300-1500 pm), and starting heating up to 350 ℃ for keeping.
Figure GDA0003360153070000071
Wherein "-" indicates that the catalytic performance of the catalyst is non-catalytic.
Example 4
Preparing a catalyst:
1. preparing a platinum nitrate/molybdic acid mixed solution with a certain concentration according to the following table, wherein the solvent is water; to obtain solution A
2. Impregnating solution A into Fe by using an isovolumetric impregnation method 2 O 3 A carrier; obtaining a precursor B
3. Putting the precursor B into an oven to be dried for 3 hours at 90 ℃; obtaining a precursor C
4. Putting the precursor C into a tubular muffle furnace, introducing hydrogen, heating to 250 ℃, and keeping for 2 hours; obtaining the catalyst.
The dehydrogenation effect test method comprises the following steps:
1. weighing 40g of decalin and 2g of catalyst, and adding into a high-temperature reaction kettle;
2. repeatedly replacing the high-temperature reaction kettle by using hydrogen; keeping normal pressure;
3. starting stirring (300-1500 pm), and starting heating up to 350 ℃ for keeping.
Figure GDA0003360153070000081
Figure GDA0003360153070000091
Wherein "-" indicates that the catalytic activity is no catalytic effect.
Example 5
Preparing a catalyst:
1. preparing a platinum nitrate/molybdic acid mixed solution with a certain concentration according to the following table, wherein the solvent is absolute alcohol; to obtain solution A
2. Impregnating solution A into ZrO by an isovolumetric impregnation method 2 A carrier; obtaining a precursor B
3. Putting the precursor B into an oven to be dried for 4 hours at 100 ℃; obtaining a precursor C
4. Putting the precursor C into a tubular muffle furnace, introducing hydrogen, heating to 350 ℃, and keeping for 6 hours; obtaining the catalyst.
The dehydrogenation effect test method comprises the following steps:
1. weighing 40g of perhydrocarbazole and 2g of catalyst, and adding into a high-temperature reaction kettle;
2. repeatedly replacing the high-temperature reaction kettle by using hydrogen; keeping normal pressure;
3. starting stirring (300-1500 pm), and starting heating up to 350 ℃ for keeping.
Figure GDA0003360153070000092
Figure GDA0003360153070000101
Wherein "-" indicates that the catalytic performance of the catalyst is non-catalytic.
As shown in fig. 2, the platinum/molybdenum dehydrogenation catalytic materials according to the preferred embodiments of the present invention have certain flexibility to a variety of supports, and of course, as shown in the figure, exhibit certain performance selectivity, which may be correlated with the atomic number of the metal element.
The listing and comparison of the above embodiments show that the combination of the catalytic materials selected by the invention has simple composition, stronger stability and stronger adaptability to various types of carriers.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (5)

1. The application of the platinum/molybdenum dehydrogenation catalytic material in dehydrogenation of liquid hydrogen storage compounds is characterized in that the platinum/molybdenum dehydrogenation catalytic material comprises a carrier and a catalytic composition formed on the carrier, the catalytic composition accounts for 0.75-1.5% of the total mass of the catalytic material, the catalytic composition comprises platinum elements and molybdenum elements, and the mass ratio of the platinum elements to the molybdenum elements in the catalytic composition is 1: (0.5-2);
the preparation method of the platinum/molybdenum dehydrogenation catalytic material comprises the following steps: preparing a mixed solution containing a platinum source and a molybdenum source; infiltrating the mixed solution into the carrier by using an isometric infiltration method, fully infiltrating, drying and sintering; the sintering is carried out by heating to 250-350 ℃ under the condition of hydrogen and keeping for 2-6 h.
2. Use according to claim 1, wherein the platinum element is derived from at least any of the followingThe method comprises the following steps: pt (NO) 3 ) 4 、 H 2 PtCl 6 。
3. Use according to claim 1, characterized in that the molybdenum element originates from at least any one of the following: molybdic acid and molybdate.
4. The use of claim 1, wherein the carrier is selected from any one of: alumina, tiO 2 、 Cr 2 O 3 、 MnO 2 、 Fe 2 O 3 CoO, niO, cuO and ZrO 2 。
5. The use according to claim 1, wherein the drying is at 80-100 ℃ for 2-4 h.
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