CN108390073A - A kind of special base metal hydrolytic hydrogen production catalyst of fuel cell and preparation method - Google Patents
A kind of special base metal hydrolytic hydrogen production catalyst of fuel cell and preparation method Download PDFInfo
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- CN108390073A CN108390073A CN201810390911.8A CN201810390911A CN108390073A CN 108390073 A CN108390073 A CN 108390073A CN 201810390911 A CN201810390911 A CN 201810390911A CN 108390073 A CN108390073 A CN 108390073A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- 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
- Y02E60/50—Fuel cells
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Abstract
The present invention provides a kind of special base metal hydrolytic hydrogen production catalyst of fuel cell and preparation methods.After evenly mixing by L cysteines, melamine and ammonium molybdate, carry out vacuum pre-sintering, then it is calcined using hot isostatic pressure stove, under high temperature and each collective effect to balanced high pressure gas, make molybdenum oxide granulated carbon metaplasia at molybdenum carbide, carbonitride is converted into porous carbon materials, to which hydrolytic hydrogen production catalyst be made.This method passes through vacuum pre-sintering+heat and other static pressuring processes, the crystallite dimension of catalyst obtained is larger, pore-size reduces, relative density and hardness are higher, catalyst obtained be nitrogen, element sulphur doping carbon material be porous structure, the molybdenum carbide particles of ultra high density, which are embedded in porous carbon structure, forms composite material, hydrolytic hydrogen production catalytic performance mechanics, and stability is good.Preparation suitable for the special hydrogen of fuel cell.
Description
Technical field
The present invention relates to hydrolytic hydrogen production fields, and in particular to the preparation of catalyst, it is special more particularly to a kind of fuel cell
With base metal hydrolytic hydrogen production catalyst and preparation method.
Background technology
Hydrogen is a kind of reproducible secondary energy sources, and calorific value is high, and reaction speed is fast, can be made by a variety of reaction paths.
By-product of the hydrogen after releasing energy is water, environmentally friendly.Although current Hydrogen Energy is used widely not yet, hydrogen is known as
The one promising energy reduces the row of greenhouse gases and other toxic gases for reducing our dependences to fossil fuel
It puts, benefits environment, be but of great significance to the research and development of Hydrogen Energy.There are many approach of hydrogen manufacturing, compound can both be reformed,
The methods of decomposition, photodissociation or hydrolysis are produced, and can be also made by electrolysis water, or carry out fermentation or photosynthetic work using production hydrogen microorganism
For obtaining hydrogen.
With the development of fuel cell, the demand to parent continues to increase, development of high-purity, the efficient hydrogen manufacturing to fuel cell
It is particularly important.In recent years, it more and more focuses on and hydrogen is produced by sustainable electrochemical process, in order to realize
The water decomposition of high-energy reduces evolving hydrogen reaction with catalyst（HER）Driving energy be very important.P/C is current city
H2-producing capacity is best on field, a kind of most stable of catalyst.But since its resource is less, cost is higher, it cannot be large-scale
Using.More and more researchs concentrate on pursuing the inexpensive substitute for having similar activity and stability with Pt.In mistake
It goes in 10 years, transient metal sulfide, nitride, phosphide, carbide have been used as promising elctro-catalyst to be reported.Its
Middle molybdenum carbide has significant catalytic activity, is attributed to its unique electricity and catalytic performance similar to noble metal, is hydrolyzing
The application of hydrogen preparation field is increasingly taken seriously.
Chinese invention patent application number 201510971074.4 discloses a kind of reduced graphene load molybdenum carbide or tungsten is urged
Agent and its preparation method and application.Include the following steps：（1）Using heteropoly acid, polymer conductor, graphene containing molybdenum or tungsten
For raw material, pass through one pot process heteropoly acid-polymer conductor/reduced graphene composite material；（2）In the protection of inert gas
Under, 2 ~ 5h is heat-treated at 700 ~ 1100 DEG C, cooling, pickling obtains reduced graphene load molybdenum carbide or tungsten catalyst.
Chinese invention patent application number 201710474099.2 discloses a kind of surface for carbon dioxide hydrogenation reaction
The preparation method of functionalization molybdenum carbide-C catalyst, mainly includes the following steps that：（1）Using deionized water as solvent, by alginic acid
Sodium is put into freeze drying box with ammonium molybdate solution and is freeze-dried after mixing；（2）High-temperature roasting under an inert atmosphere obtains
Porous graphitic carbon inlays polymolecularity molybdenum carbide；（3）Porous graphitic carbon obtained is inlayed polymolecularity molybdenum carbide to pass through with urea
It is put into Muffle furnace after crossing mechanical lapping, surface-functionalized molybdenum carbide-C catalyst is obtained after annealing.
Chinese invention patent application number 201710785956.0 discloses a kind of graphene winding molybdenum carbide/carbosphere electricity and urges
It applies, includes the following steps in agent and preparation method thereof and in acid condition water electrolysis hydrogen production：（1）By molybdate and oxygen
Graphite alkene is soluble in water, and chitosan is dissolved in the in the mixed solvent of acetic acid and water, then mixes two kinds of solution, certain speed
Lower stirring；（2）：By step（1）Then mixed solution collects solid powder by spray drying, high under atmosphere of inert gases
Temperature annealing obtains graphene winding molybdenum carbide/carbosphere elctro-catalyst.
Chinese invention patent application number 201310589889.7 discloses a kind of fast reaction membrane formation process and prepares eggshell type carbon
Change molybdenum catalyst, this method is that have the carrier of oxidation molybdenum base group to be added in melamine solution adsorption, passes through trimerization
The fast reaction of cyanamide and molybdenum oxide group is quickly generated the film being made of molybdenum carbide presoma in carrier surface, after pyrolysis shape
At eggshell type molybdenum carbide catalyst.
According to above-mentioned, for carbide such as the molybdenum carbides of hydrolytic hydrogen production in the carbide after high-temperature process in existing scheme
It will appear polymerism so that become large-sized, specific surface area reduces, and so as to cause hydrolytic hydrogen production poor performance, stability is bad.Mirror
In this, the present invention proposes a kind of special base metal hydrolytic hydrogen production catalyst of fuel cell and preparation method, can effectively solve
Above-mentioned technical problem.
Invention content
For the current molybdenum carbide catalyst using wider hydrolytic hydrogen production, there are occur polymerism, ruler after high-temperature process
It is very little big and specific surface area is small, there are the effects of hydrolytic hydrogen production it is undesirable, stability is poor the problems such as, the present invention proposes a kind of fuel electricity
The special base metal hydrolytic hydrogen production catalyst in pond and preparation method, to effectively control the size of molybdenum carbide, gained molybdenum carbide
The large specific surface area of catalyst, hydrolytic hydrogen production effect is good, and performance is stablized.
Specific technical solution of the present invention is as follows：
A kind of preparation method of the special base metal hydrolytic hydrogen production catalyst of fuel cell, includes the following steps：
（1）L-cysteine, melamine and ammonium molybdate are uniformly mixed, mixture is obtained；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering, so that ammonium molybdate is decomposed and generates molybdenum oxide particle, while three
Poly cyanamid polymerization generates stratiform carbon nitride material, and carbonitride inhibits the aggregation of molybdenum oxide particle as soft template；
（3）Further, it is calcined using hot isostatic pressure stove, in high temperature and each collective effect to balanced high pressure gas
Under, make molybdenum oxide granulated carbon metaplasia at molybdenum carbide, carbonitride is converted into porous carbon materials, to which hydrolytic hydrogen production catalyst be made.
Under the conditions of vacuum-sintering, furnace pressure only has tens pas（Pa）, even lower, O2、N2、H2And H2O molecules pole
Few, many reactions are negligible, the influence very little of medium, and the impurity of hard phase adsorption is few；And hot isostatic pressing be by
Product is placed into closed container, applies to product each to same pressure, while high temperature is imposed, in the effect of high temperature and pressure
Under, product is able to be sintered and be densified；Vacuum-sintering+heat and other static pressuring processes that the present invention uses, comprehensive two kinds of process advantages, the
Ammonium molybdate, which decomposes, during one-step calcination generates molybdenum oxide particle, while melamine polymerization generates stratiform carbon nitride material, nitrogen
Change the aggregation that carbon inhibits molybdenum oxide particle as soft template.Under high-temperature calcination, molybdenum oxide carbonization generates molybdenum carbide, and carbonitride turns
Porous carbon materials are turned to, catalyst material is made, obtained crystallite dimension is larger, and pore-size reduces and porosity declines, phase
Density and hardness is significantly improved.
Preferably, step（1）In the mixture, 20 ~ 25 parts by weight of L-cysteine, 30 ~ 50 parts by weight of melamine,
30 ~ 45 parts by weight of ammonium molybdate.
Preferably, step（2）The vacuum degree that the vacuum is pre-sintered is 40 ~ 70Pa.
Preferably, step（2）The temperature that the vacuum is pre-sintered is 600 ~ 900 DEG C, and the time is 2 ~ 4h.
Preferably, step（3）The pressure medium of the HIP sintering is argon gas.
Preferably, step（3）The static pressure pressure of the HIP sintering is 20 ~ 30MPa.
Preferably, step（3）The temperature of the HIP sintering is 1300 ~ 1500 DEG C, and sintering time is 5 ~ 7h.
The present invention also provides a kind of special base metal hydrolysis systems of kind fuel cell that above-mentioned preparation method is prepared
Hydrogen catalyst.By nitrogen, element sulphur adulterate carbon material be porous structure, and the molybdenum carbide particles of ultra high density be embedded in it is porous
Composite material is formed in carbon structure, obtained composite material has very excellent hydrolytic hydrogen production catalytic in acidic electrolyte bath
Energy and good stability.
The present invention provides a kind of special base metal hydrolytic hydrogen production catalyst of fuel cell and preparation methods, with existing skill
Art is compared, and the feature and excellent effect protruded is：
1, it proposes that calcining prepares the special base metal hydrolytic hydrogen production of fuel cell by the way of vacuum pre-sintering+hot isostatic pressing to urge
The method of agent.
2, by vacuum pre-sintering+heat and other static pressuring processes, the crystallite dimension of catalyst obtained is larger, and pore-size subtracts
Small, relative density and hardness are higher.
3, catalyst produced by the present invention be nitrogen, element sulphur doping carbon material be porous structure, the carbonization of ultra high density
Molybdenum is particle studded to form composite material in porous carbon structure, and hydrolytic hydrogen production catalytic performance is good, and good stability.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
Preparation process is：
（1）L-cysteine, melamine and ammonium molybdate are uniformly mixed, mixture is obtained；In mixture, L-cysteine 23
Parts by weight, 40 parts by weight of melamine, 37 parts by weight of ammonium molybdate；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering；The vacuum degree that vacuum is pre-sintered is 50Pa；Vacuum pre-burning
The temperature of knot is 700 DEG C, time 3h；
（3）Further, it is calcined using hot isostatic pressure stove, to which hydrolytic hydrogen production catalyst be made；HIP sintering
Pressure medium be argon gas；The static pressure pressure of HIP sintering is 26MPa；The temperature of HIP sintering is 1450 DEG C, is burnt
The knot time is 6h.
Test method：
Catalyst made from 1g embodiments 1 is taken, whether has polymerism using SEM perspective Electronic Speculum observation particles；
Catalyst made from 1g embodiments 1 is taken, average particle size is measured using Ou Qiao Occhio grain size testers；
Take catalyst made from 1g embodiments 1,2020 Plus serial physicals of ASAP absorption-quick specific surface area and mercury injection method
Analysis-e/or determining specific surface area.
Polymerism, average grain diameter and specific surface area such as 1 institute of table of the catalyst of the embodiment 1 measured by the above method
Show.
Embodiment 2
Preparation process is：
（1）L-cysteine, melamine and ammonium molybdate are uniformly mixed, mixture is obtained；In mixture, L-cysteine 22
Parts by weight, 46 parts by weight of melamine, 32 parts by weight of ammonium molybdate；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering；The vacuum degree that vacuum is pre-sintered is 50Pa；Vacuum pre-burning
The temperature of knot is 650 DEG C, time 3.5h；
（3）Further, it is calcined using hot isostatic pressure stove, to which hydrolytic hydrogen production catalyst be made；HIP sintering
Pressure medium be argon gas；The static pressure pressure of HIP sintering is 22MPa；The temperature of HIP sintering is 1350 DEG C, is burnt
The knot time is 6.5h.
Test method：
Catalyst made from 1g embodiments 2 is taken, whether has polymerism using SEM perspective Electronic Speculum observation particles；
Catalyst made from 1g embodiments 2 is taken, average particle size is measured using Ou Qiao Occhio grain size testers；
Take catalyst made from 1g embodiments 2,2020 Plus serial physicals of ASAP absorption-quick specific surface area and mercury injection method
Analysis-e/or determining specific surface area.
Polymerism, average grain diameter and specific surface area such as 1 institute of table of the catalyst of the embodiment 2 measured by the above method
Show.
Embodiment 3
Preparation process is：
（1）L-cysteine, melamine and ammonium molybdate are uniformly mixed, mixture is obtained；In mixture, L-cysteine 24
Parts by weight, 34 parts by weight of melamine, 42 parts by weight of ammonium molybdate；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering；The vacuum degree that vacuum is pre-sintered is 60Pa；Vacuum pre-burning
The temperature of knot is 840 DEG C, time 2.5h；
（3）Further, it is calcined using hot isostatic pressure stove, to which hydrolytic hydrogen production catalyst be made；HIP sintering
Pressure medium be argon gas；The static pressure pressure of HIP sintering is 28MPa；The temperature of HIP sintering is 148 DEG C, sintering
Time is 5.5h.
Test method：
Catalyst made from 1g embodiments 3 is taken, whether has polymerism using SEM perspective Electronic Speculum observation particles；
Catalyst made from 1g embodiments 3 is taken, average particle size is measured using Ou Qiao Occhio grain size testers；
Take catalyst made from 1g embodiments 3,2020 Plus serial physicals of ASAP absorption-quick specific surface area and mercury injection method
Analysis-e/or determining specific surface area.
Polymerism, average grain diameter and specific surface area such as 1 institute of table of the catalyst of the embodiment 3 measured by the above method
Show.
Embodiment 4
Preparation process is：
（1）L-cysteine, melamine and ammonium molybdate are uniformly mixed, mixture is obtained；In mixture, L-cysteine 20
Parts by weight, 50 parts by weight of melamine, 30 parts by weight of ammonium molybdate；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering；The vacuum degree that vacuum is pre-sintered is 40Pa；Vacuum pre-burning
The temperature of knot is 600 DEG C, time 4h；
（3）Further, it is calcined using hot isostatic pressure stove, to which hydrolytic hydrogen production catalyst be made；HIP sintering
Pressure medium be argon gas；The static pressure pressure of HIP sintering is 20MPa；The temperature of HIP sintering is 1300 DEG C, is burnt
The knot time is 7h.
Test method：
Catalyst made from 1g embodiments 4 is taken, whether has polymerism using SEM perspective Electronic Speculum observation particles；
Catalyst made from 1g embodiments 4 is taken, average particle size is measured using Ou Qiao Occhio grain size testers；
Take catalyst made from 1g embodiments 4,2020 Plus serial physicals of ASAP absorption-quick specific surface area and mercury injection method
Analysis-e/or determining specific surface area.
Polymerism, average grain diameter and specific surface area such as 1 institute of table of the catalyst of the embodiment 4 measured by the above method
Show.
Embodiment 5
Preparation process is：
（1）L-cysteine, melamine and ammonium molybdate are uniformly mixed, mixture is obtained；In mixture, L-cysteine 25
Parts by weight, 30 parts by weight of melamine, 45 parts by weight of ammonium molybdate；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering；The vacuum degree that vacuum is pre-sintered is 70Pa；Vacuum pre-burning
The temperature of knot is 900 DEG C, time 2h；
（3）Further, it is calcined using hot isostatic pressure stove, to which hydrolytic hydrogen production catalyst be made；HIP sintering
Pressure medium be argon gas；The static pressure pressure of HIP sintering is 30MPa；The temperature of HIP sintering is 1500 DEG C, is burnt
The knot time is 5h.
Test method：
Catalyst made from 1g embodiments 5 is taken, whether has polymerism using SEM perspective Electronic Speculum observation particles；
Catalyst made from 1g embodiments 5 is taken, average particle size is measured using Ou Qiao Occhio grain size testers；
Take catalyst made from 1g embodiments 5,2020 Plus serial physicals of ASAP absorption-quick specific surface area and mercury injection method
Analysis-e/or determining specific surface area.
Polymerism, average grain diameter and specific surface area such as 1 institute of table of the catalyst of the embodiment 5 measured by the above method
Show.
Embodiment 6
Preparation process is：
（1）L-cysteine, melamine and ammonium molybdate are uniformly mixed, mixture is obtained；In mixture, L-cysteine 22
Parts by weight, 40 parts by weight of melamine, 38 parts by weight of ammonium molybdate；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering；The vacuum degree that vacuum is pre-sintered is 60Pa；Vacuum pre-burning
The temperature of knot is 800 DEG C, time 3h；
（3）Further, it is calcined using hot isostatic pressure stove, to which hydrolytic hydrogen production catalyst be made；HIP sintering
Pressure medium be argon gas；The static pressure pressure of HIP sintering is 25MPa；The temperature of HIP sintering is 1400 DEG C, is burnt
The knot time is 6h.
Test method：
Catalyst made from 1g embodiments 6 is taken, whether has polymerism using SEM perspective Electronic Speculum observation particles；
Catalyst made from 1g embodiments 6 is taken, average particle size is measured using Ou Qiao Occhio grain size testers；
Take catalyst made from 1g embodiments 6,2020 Plus serial physicals of ASAP absorption-quick specific surface area and mercury injection method
Analysis-e/or determining specific surface area.
Polymerism, average grain diameter and specific surface area such as 1 institute of table of the catalyst of the embodiment 6 measured by the above method
Show.
Comparative example 1
Preparation process is：
（1）L-cysteine and ammonium molybdate are uniformly mixed, mixture is obtained；In mixture, 42 parts by weight of L-cysteine, molybdenum
58 parts by weight of sour ammonium；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering；The vacuum degree that vacuum is pre-sintered is 60Pa；Vacuum pre-burning
The temperature of knot is 800 DEG C, time 3h；
（3）Further, it is calcined using hot isostatic pressure stove, to which hydrolytic hydrogen production catalyst be made；HIP sintering
Pressure medium be argon gas；The static pressure pressure of HIP sintering is 25MPa；The temperature of HIP sintering is 1400 DEG C, is burnt
The knot time is 6h.
Test method：
Catalyst made from 1g comparative examples 1 is taken, whether has polymerism using SEM perspective Electronic Speculum observation particles；
Catalyst made from 1g comparative examples 1 is taken, average particle size is measured using Ou Qiao Occhio grain size testers；
Take catalyst made from 1g comparative examples 1,2020 Plus serial physicals of ASAP absorption-quick specific surface area and mercury injection method
Analysis-e/or determining specific surface area.
Polymerism, average grain diameter and specific surface area such as 1 institute of table of the catalyst of the comparative example 1 measured by the above method
Show.
Table 1：
| Performance indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example 1 |
| With the presence or absence of polymerism | Nothing | Nothing | Nothing | Nothing | Nothing | Nothing | There are a small amount of polymerisms |
| Average particle size（μm） | 0.74 | 0.75 | 0.79 | 0.72 | 0.73 | 0.68 | 1.12 |
| Specific surface area（m2/g） | 143.2 | 145.3 | 144.2 | 140.5 | 143.2 | 146.2 | 50.5 |
Claims (8)
1. a kind of preparation method of the special base metal hydrolytic hydrogen production catalyst of fuel cell, which is characterized in that including following step
Suddenly：
（1）L-cysteine, melamine and ammonium molybdate are uniformly mixed, mixture is obtained；
（2）To step（1）Obtained mixture carries out vacuum pre-sintering, so that ammonium molybdate is decomposed and generates molybdenum oxide particle, while three
Poly cyanamid polymerization generates stratiform carbon nitride material, and carbonitride inhibits the aggregation of molybdenum oxide particle as soft template；
（3）Further, it is calcined using hot isostatic pressure stove, in high temperature and each collective effect to balanced high pressure gas
Under, make molybdenum oxide granulated carbon metaplasia at molybdenum carbide, carbonitride is converted into porous carbon materials, to which hydrolytic hydrogen production catalyst be made.
2. the preparation method of the special base metal hydrolytic hydrogen production catalyst of a kind of fuel cell according to claim 1, special
Sign is：Step（1）In the mixture, 20 ~ 25 parts by weight of L-cysteine, 30 ~ 50 parts by weight of melamine, ammonium molybdate 30
~ 45 parts by weight.
3. the preparation method of the special base metal hydrolytic hydrogen production catalyst of a kind of fuel cell according to claim 1, special
Sign is：Step（2）The vacuum degree that the vacuum is pre-sintered is 40 ~ 70Pa.
4. the preparation method of the special base metal hydrolytic hydrogen production catalyst of a kind of fuel cell according to claim 1, special
Sign is：Step（2）The temperature that the vacuum is pre-sintered is 600 ~ 900 DEG C, and the time is 2 ~ 4h.
5. the preparation method of the special base metal hydrolytic hydrogen production catalyst of a kind of fuel cell according to claim 1, special
Sign is：Step（3）The pressure medium of the HIP sintering is argon gas.
6. the preparation method of the special base metal hydrolytic hydrogen production catalyst of a kind of fuel cell according to claim 1, special
Sign is：Step（3）The static pressure pressure of the HIP sintering is 20 ~ 30MPa.
7. the preparation method of the special base metal hydrolytic hydrogen production catalyst of a kind of fuel cell according to claim 1, special
Sign is：Step（3）The temperature of the HIP sintering is 1300 ~ 1500 DEG C, and sintering time is 5 ~ 7h.
8. the special base metal hydrolytic hydrogen production of a kind of fuel cell that any one of claim 1 ~ 7 preparation method is prepared
Catalyst.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115548265A (en) * | 2022-09-01 | 2022-12-30 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon embedded nanocrystalline active material composite foam |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115548265A (en) * | 2022-09-01 | 2022-12-30 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon embedded nanocrystalline active material composite foam |
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