CN110652993A - Research on hydrogen production performance of ammonia borane catalyzed by cobalt-nitrogen-doped graphene-based catalyst - Google Patents

Research on hydrogen production performance of ammonia borane catalyzed by cobalt-nitrogen-doped graphene-based catalyst Download PDF

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Publication number
CN110652993A
CN110652993A CN201910940601.3A CN201910940601A CN110652993A CN 110652993 A CN110652993 A CN 110652993A CN 201910940601 A CN201910940601 A CN 201910940601A CN 110652993 A CN110652993 A CN 110652993A
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cobalt
ammonia borane
based catalyst
graphene
catalyst
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CN201910940601.3A
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马晓艳
高庆玲
张洋
胡莉
郝杰
张旭梅
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Chengdu Univeristy of Technology
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Chengdu Univeristy of Technology
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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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • 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
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • 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
    • C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
    • C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition 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
    • C01B2203/1052—Nickel or cobalt catalysts
    • 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
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a research on the performance of catalyzing ammonia borane to produce hydrogen by using a cobalt aza graphene-based catalyst. Besides being used as a high-energy hydrogen storage material, ammonia borane and derivatives thereof can also be used as a reducing agent in the field of organic synthetic chemistry for reduction reaction of aldehyde ketone and carbonyl compounds in recent years, and compared with the traditional reducing agent, the ammonia borane has the advantages of mild reaction conditions, strong selectivity, high product yield and the like. Ammonia borane compound (NH)3BH3) The material is a novel chemical hydride hydrogen storage material which is recently and closely focused, and has the advantages of ultrahigh hydrogen density (19.6 wt%), good thermal stability and chemical stability and the like, thereby having wide application prospect. Wherein the ammonia borane has the fastest hydrogen production rate under the conditions of T298K and 15 percent NaOH, and the TOF value is 54moLH2.min‑1.moLCa ‑1The apparent activation energy is 27.1kJ/mol, the loading of metallic cobalt is 1-2 wt%, and the catalyst is successfully preparedHas great significance for producing hydrogen from ammonia borane.

Description

Research on hydrogen production performance of ammonia borane catalyzed by cobalt-nitrogen-doped graphene-based catalyst
Technical Field
The invention belongs to the field of catalysts, and particularly relates to a preparation method of a non-noble metal catalyst and research on hydrogen production performance of ammonia borane.
Background
In recent years, with the rapid development of global economy, the demand of human beings on energy sources accelerates the consumption of non-renewable energy sources such as coal, petroleum, natural gas and the like, and also causes serious pollution to the global environment, and the hydrogen energy has the advantages of rich content, high fuel value, reproducibility, no pollution and the like and is paid attention to by people. Ammonia borane (NH)3BH3AB for short, has a high hydrogen storage density (19.6%) and a low molecular weight (30.9 gmol)-1) It is one of the chemical hydride hydrogen storage materials with the highest hydrogen storage capacity. Meanwhile, the development and utilization of hydrogen energy have received high attention from researchers, but the storage and utilization of hydrogen gas have been faced with great challenges. The most critical problems are the difficulty in quickly and efficiently producing hydrogen and the safe storage of hydrogen. Hydrogen is one of the best expected energy carriers to meet the growing demand for clean and efficient energy supplies. The hydrogen production of ammonia borane can be realized by two modes of pyrolysis and hydrolysis, however, the pyrolysis method needs to be carried out at higher temperature, and the aqueous solution of ammonia borane is stable and can be quickly and easily hydrolyzed at room temperature to generate hydrogen in the presence of a proper catalyst.
In view of the above, the present invention is proposed to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a research on the hydrogen production performance of ammonia borane catalyzed by a cobalt aza graphene-based catalyst, which adopts the cobalt aza graphene-based catalyst, has mild reaction conditions and high catalysis efficiency, and is suitable for the catalysis field.
A cobalt aza graphene based catalyst ammonia borane hydrogen production performance research comprises the following specific steps:
s1, preparing a cobalt nitrogen graphene-based catalyst;
and S2, catalyzing ammonia borane to produce hydrogen by using the cobalt aza graphene-based catalyst.
Further, the preparation method of the cobalt aza graphene-based catalyst in S1 comprises the specific steps of: putting urea, phthalic anhydride, ammonium molybdate and cobalt chloride hexahydrate in a 500mL beaker, heating and stirring in an oil bath kettle at a certain temperature, cooling to room temperature after a sample reaches a molten state, heating in a microwave oven for a period of time, taking out, cooling to room temperature, grinding, adding a sodium hydroxide solution with a certain volume and concentration, boiling for 30min, carrying out suction filtration, washing to be neutral, drying and grinding; dissolving the dried product with concentrated sulfuric acid, diluting with deionized water, filtering, washing to neutrality, drying, and grinding to obtain cobalt phthalocyanine; calcining cobalt phthalocyanine at high temperature to obtain a cobalt aza graphene-based catalyst;
further, in the preparation method of the cobalt aza graphene-based catalyst in S1, the mass of the urea, phthalic anhydride, ammonium molybdate and cobalt chloride hexahydrate in the step are 27g, 16.8g, 1.5g and 5.7g respectively;
further, in the preparation method of the cobalt-nitrogen-doped graphene-based catalyst in S1, the oil bath temperature in the step is 100-120 ℃, and the reaction time in microwave is 6-8 min;
further, in the preparation method of the cobalt aza graphene-based catalyst in S1, the volume of sodium hydroxide in the step is 340mL, and the concentration is 20%;
further, in the preparation method of the cobalt aza graphene-based catalyst in S1, the loading amount of cobalt in the step is 1-2%;
further, the cobalt aza graphene-based catalyst in S2 is used for catalyzing ammonia borane to produce hydrogen, and the specific steps are as follows: adding a certain amount of catalyst, reaction substrate and solvent into a two-mouth flask, designing experiments under different conditions by using a controlled variable method, and inspecting the influence of the catalyst on the ammonia borane hydrolysis rate under different conditions;
further, in the step S2, the cobalt aza graphene-based catalyst catalyzes ammonia borane to produce hydrogen, and the conditions designed in the step are sodium hydroxide concentration, catalyst concentration, concentration of aqueous solution, ammonia borane concentration, temperature, and catalyst cycling stability experiment.
The invention has the beneficial effects that:
1. in the research on the performance of catalyzing ammonia borane to generate hydrogen by using the cobalt aza graphene-based catalyst provided by the invention, the catalyst has high activity and high selectivity;
2. in the research on the performance of catalyzing ammonia borane to generate hydrogen by using the cobalt aza graphene-based catalyst provided by the invention, the preparation method of the catalyst is simple and easy to implement and has low cost;
3. the catalyst of the invention has less by-products in catalyzing ammonia borane to produce hydrogen, mild reaction conditions, simple and convenient operation and good reproducibility;
4. the raw material of the invention has high hydrogen storage density (19.6%) and low molecular weight (30.9g mol)-1) No toxicity, high stability, environment friendship, etc.
Drawings
FIG. 1 is a graph of the effect of NaOH concentration on ammonia borane hydrolysis to produce hydrogen;
FIG. 2 is a graph of the effect of catalyst concentration on ammonia borane hydrolysis to produce hydrogen;
FIG. 3 is a graph of the effect of water concentration on ammonia borane hydrolysis to produce hydrogen;
FIG. 4 is a graph of the effect of ammonia borane concentration on ammonia borane hydrolysis to produce hydrogen;
FIG. 5 is a graph of the effect of temperature on ammonia borane hydrolysis to produce hydrogen;
FIG. 6 is a graph of the effect of catalyst recycle on ammonia borane hydrolysis to produce hydrogen;
fig. 7 is a Scanning Electron Microscope (SEM) image of a cobalt aza graphene-based catalyst.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Detailed description of the preferred embodiment 1
Preparing a cobalt-nitrogen-doped graphene-based catalyst: putting urea, phthalic anhydride, ammonium molybdate and cobalt chloride hexahydrate in a 500mL beaker, heating and stirring in an oil bath kettle at a certain temperature, cooling to room temperature after a sample reaches a molten state, heating in a microwave oven for a period of time, taking out, cooling to room temperature, grinding, adding a sodium hydroxide solution with a certain volume and concentration, boiling for 30min, carrying out suction filtration, washing to be neutral, drying and grinding; dissolving the dried product with concentrated sulfuric acid, diluting with deionized water, filtering, washing to neutrality, drying, and grinding to obtain cobalt phthalocyanine; and calcining the cobalt phthalocyanine at high temperature to obtain the cobalt aza-graphene-based catalyst.
Detailed description of the preferred embodiment 2
The cobalt aza graphene-based catalyst prepared by the invention has the advantages that T298K, P is 1.01kPa, mca＝10mg、mAB40mg at 450 d/min-1The effect of different sodium hydroxide concentrations on the hydrolysis of ammonia borane to produce hydrogen is shown in figure 1 of the accompanying drawings.
Detailed description of preferred embodiments 3
The cobalt aza graphene-based catalyst prepared by the invention has the characteristics of T298K, P being 1.01kPa and CNaOH＝15％、mAB40mg at 450 d/min-1The effect of different catalyst concentrations on the hydrolysis of ammonia borane to produce hydrogen is shown in figure 2 of the accompanying drawings.
Detailed description of preferred embodiments 4
The cobalt aza graphene-based catalyst prepared by the invention has the characteristics of T298K, P being 1.01kPa and CNaOH＝15％、mAB＝40mg、mca50mg at 450 d/min-1The effect of different water concentrations on the hydrolysis of ammonia borane to produce hydrogen is shown in figure 3 of the accompanying drawings.
Best mode for carrying out the invention
The cobalt aza graphene-based catalyst prepared by the invention has the characteristics of T298K, P being 1.01kPa and CNaOH＝15％、mca50mg at 450 d/min-1The effect of different ammonia borane concentrations on the hydrolysis of ammonia borane to produce hydrogen is shown in figure 4 of the accompanying drawings.
Detailed description of preferred embodiments 6
The cobalt aza graphene-based catalyst prepared by the invention has the advantages of high catalytic activity and low catalytic activity when P is 1.01kPa and C isNaOH＝15％、mAB＝40mg、mca50mg at 450 d/min-1The effect of different temperatures on the hydrolysis of ammonia borane to produce hydrogen is shown in figure 5 of the accompanying drawings.
Best mode for carrying out the invention
The cobalt aza graphene-based catalyst prepared by the invention has the characteristics of T298K, P being 1.01kPa and CNaOH＝15％、mAB＝40mg、mca50mg at 450 d/min-1The effect of the catalyst recycle experiments on the hydrolysis of ammonia borane to produce hydrogen is shown in figure 6 of the accompanying drawings.
Best mode for carrying out the invention
Preparing a cobalt-nitrogen-doped graphene-based catalyst: putting urea, phthalic anhydride, ammonium molybdate and cobalt chloride hexahydrate in a 500mL beaker, heating and stirring in an oil bath kettle at a certain temperature, cooling to room temperature after a sample reaches a molten state, heating in a microwave oven for a period of time, taking out, cooling to room temperature, grinding, adding a sodium hydroxide solution with a certain volume and concentration, boiling for 30min, carrying out suction filtration, washing to be neutral, drying and grinding; dissolving the dried product with concentrated sulfuric acid, diluting with deionized water, filtering, washing to neutrality, drying, and grinding to obtain cobalt phthalocyanine; and calcining the cobalt phthalocyanine at high temperature to obtain the cobalt aza-graphene-based catalyst. Scanning electron microscopy characterization of the cobalt-based catalyst was performed as shown in figure 7 of the accompanying drawings.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.

Claims (6)

1. A research on the hydrogen production performance of ammonia borane catalyzed by a cobalt-nitrogen-doped graphene-based catalyst is characterized by comprising the following specific steps:
s1, preparing the cobalt-nitrogen-doped graphene-based catalyst, which comprises the following steps:
weighing urea, phthalic anhydride, ammonium molybdate and cobalt chloride hexahydrate in a 500mL beaker, placing the beaker in an oil bath kettle at a certain temperature for heating and stirring, cooling to room temperature after a sample reaches a molten state, placing the sample in a microwave oven for heating for a period of time, taking out the sample, cooling to room temperature, grinding, adding a sodium hydroxide solution with a certain volume and concentration, boiling for 30min, carrying out suction filtration, washing to be neutral, drying and grinding; dissolving the dried product with concentrated sulfuric acid, diluting with deionized water, filtering, washing to neutrality, drying, and grinding to obtain cobalt phthalocyanine; calcining cobalt phthalocyanine at high temperature to obtain a cobalt aza graphene-based catalyst;
s2, catalyzing ammonia borane to produce hydrogen by using the cobalt aza graphene-based catalyst, the method comprises the following steps:
adding a certain amount of catalyst, reaction substrate and solvent into a two-neck flask, designing experiments under different conditions by using a controlled variable method, and inspecting the influence of the catalyst on the ammonia borane hydrolysis rate under different conditions.
2. The method of claim 1, wherein the cobalt aza-graphene-based catalyst is prepared according to S1, wherein the mass of urea, phthalic anhydride, ammonium molybdate, and cobalt chloride hexahydrate is 27g, 16.8g, 1.5g, and 5.7 g.
3. The method for preparing the cobalt-aza-graphene-based catalyst in S1 according to claim 1, wherein the oil bath temperature is 100 ℃ and 120 ℃, and the reaction time in microwave is 6-8 min.
4. The method of claim 1, S1, wherein the cobalt aza graphene-based catalyst is prepared with a sodium hydroxide volume of 340mL and a concentration of 20%.
5. The method of preparing a cobalt aza graphene-based catalyst as claimed in S1, wherein the loading of cobalt is 1-2%.
6. In the experiment of producing hydrogen by catalyzing ammonia borane with the cobalt aza graphene-based catalyst according to the claim 1 in S2, the designed conditions are sodium hydroxide concentration, catalyst concentration, concentration of aqueous solution, ammonia borane concentration, temperature and catalyst cycling stability experiment.
CN201910940601.3A 2019-09-30 2019-09-30 Research on hydrogen production performance of ammonia borane catalyzed by cobalt-nitrogen-doped graphene-based catalyst Pending CN110652993A (en)

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Application publication date: 20200107