CN108649243A - A kind of fuel-cell catalyst graphitized carbon carrier, preparation method and the fuel-cell catalyst using the graphitized carbon carrier - Google Patents
A kind of fuel-cell catalyst graphitized carbon carrier, preparation method and the fuel-cell catalyst using the graphitized carbon carrier Download PDFInfo
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- CN108649243A CN108649243A CN201810411790.0A CN201810411790A CN108649243A CN 108649243 A CN108649243 A CN 108649243A CN 201810411790 A CN201810411790 A CN 201810411790A CN 108649243 A CN108649243 A CN 108649243A
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- carbon carrier
- fuel
- graphitized carbon
- catalyst
- cell catalyst
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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
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- 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
- H01M4/8825—Methods for deposition of the catalytic active composition
-
- 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
- Y02E60/50—Fuel cells
Abstract
The invention discloses a kind of fuel-cell catalyst graphitized carbon carrier, preparation method and using the fuel-cell catalyst of the graphitized carbon carrier, belong to fuel-cell catalyst and carbon carrier technical field.Technical scheme of the present invention main points are：First, carbon material is uniformly mixed with metal salt by certain mass ratio, then uniformly mixed material is agitated, dry be placed in high temperature furnace carries out high-temperature heat treatment.Secondly, material washing, filtering, the drying after high-temperature heat treatment are obtained into graphitized carbon carrier, handles to obtain platinum carbon catalyst finally by it is carried out reduction of ethylene glycol chloroplatinic acid method.Preparation method of the present invention is simple, easily operated, relatively low to equipment requirement；The addition of metal salt reduces carbon material graphitization temperature；Metal platinum particles are uniformly dispersed on the carbon carrier in the catalyst of synthesis, and the two is tightly combined, and show good high voltage corrosion resistance and high catalytic activity.
Description
Technical field
The invention belongs to fuel-cell catalyst and carbon carrier technical fields, and in particular to a kind of fuel-cell catalyst stone
Inkization carbon carrier, preparation method and the fuel-cell catalyst using the graphitized carbon carrier.
Background technology
In numerous renewable new energy fields, fuel cell is shown one's talent.First, difference is filled with numerous energy storages
Such as lithium ion battery and ultracapacitor are set, fuel cell is a kind of outstanding energy conversion device, as long as having continually
Fuel supply, can produce electricl energy always.For internal combustion engine, fuel cell is not limited by Carnot cycle, and energy turns
Change efficiency to greatly improve, and the cathode reactant of fuel cell is the oxygen in air, is derived from a wealth of sources, whole process only generates
Electric energy, heat and water do not generate greenhouse gases and any pollution.Advantage in summary, fuel cell is as renewable new energy
Important component in field by various circles of society extensive concern.
Although fuel cell imagination is thermodynamically feasible, corresponding slow Cathodic oxygen reduction is dynamic
Mechanics seriously constrains the development of itself.Therefore, it is necessary to develop cathod catalyst that is a kind of efficient and stablizing.Platinum based noble metal is negative
Carry the catalyst that C catalyst is optimal at present.Although the bullion contents such as platinum are rare, expensive, what is used at present is super
The dosage of platinum can be reduced to 0.4mg/cm by sound spraying technology2, the content of platinum used in each car is no more than 10g.Therefore, platinum
The dosage of C catalyst is reduced to commercially viable range, and current maximum obstacle is to develop the fuel with good stability
Cell catalyst.
The stability of platinum carbon catalyst includes mainly two large divisions, and first, the stability of platinum grain；The second, carbon carrier
Stability.The wherein reunion of platinum grain and to fall off be the main reason for causing its stability to reduce, and generating this phenomenon is then
Caused by due to carbon carrier is in strong acid corrosion and elevated pressure life oxidation etc..Therefore, developing one kind can effectively stablize
Platinum grain, and it is the task of top priority itself to keep the carbon carrier of the characteristics such as good resistance to strong acid corrosion and high pressure resistant oxidation.Currently,
Carrier carbon graphitization can be improved into the resistance to strong acid corrosivity of carbon carrier and high pressure resistant oxidisability.Willinger et al.（ACS
Catalysis, 7 (2017) 4395-4407.）Three kinds of different types of carbon carriers, respectively height graphite are tested respectively
Change carbon, height defect carbon and height defect and functionalized carbon.It is found by test comparison, the phase of high-graphitized carbon and platinum grain
Interaction is can to reduce carbon base body by a kind of Pt-H-C connection functions and the reunion of platinum grain and fall off in corrosion process,
Show optimal stability.However, for the carbon of height defect, there can be PtOx that a part does not restore completely
Grain forms the connection function of Pt-O-C, and this effect can enhance the corrosion of carbon base body, reduce stability.Simultaneously for height defect
For functionalized carbon, a kind of Pt-C covalent linkages effect has been primarily formed, however this platinum that can not stablize its load
Grain.Although above-mentioned document indicates that high-graphitized carbon has optimal stability, the problem of selecting which kind of graphitized carbon
There is no solutions.Therefore, how a kind of graphitized carbon carrier of high stability is searched out by simple effective method to compel in eyebrow
Eyelash.
Invention content
The technical problem to be solved by the present invention is to provide a kind of fuel-cell catalyst graphitized carbon carrier and its preparation sides
Various carbon materials are graphitized by method, this method by high-temperature sintering process, then in situ by platinum nanometer by liquid-phase reflux method
Particulate load is on graphitized carbon carrier, by testing the cyclical stability under its high pressure, preferably goes out most stable of graphitized carbon
Carrier, and the platinum carbon catalyst based on graphitized carbon carrier is finally made.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, and a kind of fuel-cell catalyst graphitized carbon carries
The preparation method of body, it is characterised in that the specific steps are：First by carbon material and metal salt in mass ratio 1:1~5:1 ratio
It is uniformly mixed；Uniformly mixed material is stirred into drying in a water bath again, then the material after drying is placed in high temperature furnace with 5
The heating rate of~30 DEG C/min is warming up to 1200~2800 DEG C and carries out 1~6h of high-temperature heat treatment；It finally will be after high-temperature heat treatment
Material directly as graphitized carbon carrier using or by after high-temperature heat treatment material washing, filtering, drying obtain graphite
Change carbon carrier.
Further preferably, the carbon material is polyaniline, polypyrrole, Ketjen black, acetylene black, Vlutx-72 or PANi-10
In one or several kinds, preferably Ketjen black, Vlutx-72 or PANi-10.
Further preferably, the metal salt is nickel nitrate, nickel sulfate, nickel acetate, nickel chloride, ferric nitrate, ferric sulfate, acetic acid
One or several kinds in iron, ferricyanide, iron chloride, cobalt nitrate, cobaltous sulfate or cobalt chloride.
Further preferably, the high-temperature heat treatment temperature is preferably 1600 DEG C, and the high-temperature heat treatment time is preferably 3h.
Fuel-cell catalyst graphitized carbon carrier of the present invention, it is characterised in that be prepared by the above method
's.
The preparation method of fuel-cell catalyst of the present invention, it is characterised in that the specific steps are：
（1）The graphitized carbon carrier ultrasonic disperse that above-mentioned washed, filtering, drying are obtained is stirred for 1 in ethylene glycol solution
Platinum acid chloride solution is added after~5h, is passed through nitrogen protection, continues 1~5h of stirring and obtains solution A；
（2）The ethylene glycol solution that sodium hydroxide is added after solution A is uniformly mixed adjusts pH=8~14 of mixed system, adds
Heat then cools to room temperature to obtain solution B to 100~150 DEG C of 1~5h of reflux；
（3）PH=1~7 that dilute hydrochloric acid adjusts mixed system are added into solution B, then graphitized carbon material wash
To catalyst precursor, then vacuum filtration method filtering solution is used, and is washed with deionized and repeatedly obtains fuel cell platinum carbon
Catalyst.
Compared with the prior art, the present invention has the following advantages：1, preparation method is simple, easily operated, to equipment requirement compared with
It is low；2, the addition of metal salt reduces carbon material graphitization temperature；3, graphitized carbon carrier passes through simple reduction of ethylene glycol chlorine
Platinic acid method is made, and uniformly can effectively be supported on platinum grain on graphitized carbon carrier；4, platinum carbon catalysis produced by the present invention
Agent can effectively reduce graphitized carbon carrier and the reunion of platinum grain and fall off in corrosion process, and then show preferable stabilization
Property.
Description of the drawings
Fig. 1 is the XRD diagram that preferable electrocatalysis characteristic platinum carbon catalyst is obtained in embodiment 1；
Fig. 2 is the performance comparison curve that three kinds of different graphitization degree carbon carriers carry the platinum carbon catalyst obtained after platinum in embodiment 1；
Fig. 3 is the TEM figures that preferable electrocatalysis characteristic platinum carbon catalyst is obtained in embodiment 1.
Specific implementation mode
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on the above of the present invention belong to this hair
Bright range.
Embodiment 1
PANi-10 building-up processes：The 1M hydrochloric acid solutions of aniline and each 50mL of the 1M hydrochloric acid solutions of ammonium persulfate are mixed equal
It is even, after filtering and washing, obtained solid is dissolved in the 1M hydrochloric acid solutions of tridecyl methyl ammonium bromide, is added under condition of ice bath
The saturated solution of 3.2g toluene and the ammonium cyanate containing 13.2g dries to obtain presoma after agitation and filtration washing.Then presoma is existed
900℃N2Then middle calcining is washed with dilute hydrochloric acid to neutrality, final product is dried to obtain.
The Ketjen black, Vlutx-72 and PANi-10 for weighing 1.0g respectively are put into beaker, each nitric acid that 0.3716g is added
Nickel, the pure water for adding 75mL are uniformly mixed in ultrasound, drying are stirred, by the material after drying in 1800 DEG C in high temperature furnace
3h is calcined, graphitized carbon carrier is obtained through deionized water washing, filtering, drying.
The graphitized carbon carrier for weighing 0.20g respectively is placed in ultrasound 10min, magnetic agitation 0.5h in 50mL ethylene glycol and adds
Enter 20mL（7.5mg/mL）Platinum acid chloride solution, and stir 2h under nitrogen protection, mixture adjusted with the solution of sodium hydroxide
PH=10 of system, flow back 4h in 110 DEG C, room temperature natural cooling, then pH=4 of mixed system are adjusted with dilute hydrochloric acid, and miillpore filter is taken out
It is washed with deionized after filter, drying to load capacity is the platinum carbon catalyst of 24wt%.
The technical process of the present embodiment is simple, obtains the carbon carrier after being graphitized with PANi-10 and carries the platinum carbon formed after platinum
Catalyst has good electrocatalysis characteristic.
Embodiment 2
It weighs the PANi-10 that five parts of quality are 1.0g respectively to be put into beaker, each nickel nitrate that 0.3716g is added adds
The pure water of 75mL in ultrasound be uniformly mixed, stir drying, by the material after drying respectively in high temperature furnace in 1500 DEG C, 1600
DEG C, 1700 DEG C, 1800 DEG C and 2000 DEG C calcining 3h, then through deionized water washing, filtering, drying obtain graphitized carbon carrier.
The graphitized carbon carrier for weighing 0.20g respectively is placed in ultrasound 10min, magnetic agitation 0.5h in 50mL ethylene glycol and adds
Enter 20mL（7.5mg/mL）Platinum acid chloride solution, and stir 2h under nitrogen protection, mixture adjusted with the solution of sodium hydroxide
PH=10 of system, flow back 4h in 110 DEG C, room temperature natural cooling, then pH=4 of mixed system are adjusted with dilute hydrochloric acid, and miillpore filter is taken out
It is washed with deionized after filter, drying to load capacity is the platinum carbon catalyst of 24wt%.
The platinum carbon catalyst being graphitized at 1600 DEG C is obtained in the present embodiment has the electro-catalysis of comparative superiority
Performance.
Embodiment 3
It weighs the PANi-10 that two parts of quality are 1g respectively to be put into beaker, each nickel nitrate that 0.3716g is added adds 75mL
Pure water in ultrasound be uniformly mixed, stir drying, by the material after drying in high temperature furnace in 1600 DEG C calcine 2h, 3h, 4h
And 5h.Again graphitized carbon carrier is obtained through deionized water washing, filtering, drying.
The graphitized carbon carrier for weighing 0.20g respectively is placed in ultrasound 10min, magnetic agitation 0.5h in 50mL ethylene glycol and adds
Enter 20mL（7.5mg/mL）Platinum acid chloride solution, and stir 2h under nitrogen protection, mixture adjusted with the solution of sodium hydroxide
PH=10 of system, flow back 4h in 110 DEG C, room temperature natural cooling, then pH=4 of mixed system are adjusted with dilute hydrochloric acid, and miillpore filter is taken out
It is washed with deionized after filter, drying to load capacity is the platinum carbon catalyst of 24wt%.
Catalyst prepared by carbon carrier when being 3h between being obtained in the present embodiment upon calcination after graphitization has preferable
Electrocatalysis characteristic.
Embodiment above describes the basic principles and main features and advantage of the present invention, and the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the originals of the present invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (6)
1. a kind of preparation method of fuel-cell catalyst graphitized carbon carrier, it is characterised in that the specific steps are：First by carbon
Material and metal salt in mass ratio 1:1~5:1 ratio is uniformly mixed；Uniformly mixed material is stirred in a water bath again dry
It is dry, then by the material after drying be placed in high temperature furnace with the heating rate of 5~25 DEG C/min be warming up to 1500~2800 DEG C into
1~5h of row high-temperature heat treatment；Finally by the material after high-temperature heat treatment directly as graphitized carbon carrier using or by high temperature
Material washing, filtering, drying after heat treatment obtain graphitized carbon carrier.
2. the preparation method of fuel-cell catalyst graphitized carbon carrier according to claim 1, it is characterised in that：It is described
Carbon material is the one or several kinds in polyaniline, polypyrrole, Ketjen black, acetylene black, Vlutx-72 or PANi-10.
3. the preparation method of fuel-cell catalyst graphitized carbon carrier according to claim 1, it is characterised in that：It is described
Metal salt is nickel nitrate, nickel sulfate, nickel acetate, nickel chloride, ferric nitrate, ferric sulfate, ferric acetate, ferricyanide, iron chloride, nitric acid
One or several kinds in cobalt, cobaltous sulfate or cobalt chloride.
4. the preparation method of fuel-cell catalyst graphitized carbon carrier according to claim 1, it is characterised in that：It is described
High-temperature heat treatment temperature is preferably 1600 DEG C, and the high-temperature heat treatment time is preferably 3h.
5. a kind of fuel-cell catalyst graphitized carbon carrier, it is characterised in that be described in any one of Claims 1 to 4
Method be prepared.
6. a kind of preparation method of fuel-cell catalyst, it is characterised in that the specific steps are：
（1）By washed in claim 1, filtering, obtained graphitized carbon carrier ultrasonic disperse is dried in ethylene glycol solution,
Platinum acid chloride solution is added after being stirred for 1~5h, is passed through nitrogen protection, continues 1~5h of stirring and obtains solution A；
（2）The ethylene glycol solution that sodium hydroxide is added after solution A is uniformly mixed adjusts pH=8~14 of mixed system, adds
Heat then cools to room temperature to obtain solution B to 100~150 DEG C of 1~5h of reflux；
（3）PH=1~7 that dilute hydrochloric acid adjusts mixed system are added into solution B, then graphitized carbon material wash
To catalyst precursor, then vacuum filtration method filtering solution is used, and is washed with deionized and repeatedly obtains fuel cell platinum carbon
Catalyst.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111129518A (en) * | 2019-12-30 | 2020-05-08 | 一汽解放汽车有限公司 | Modified carbon carrier, preparation method thereof and application thereof in fuel cell |
| CN111129525A (en) * | 2019-12-30 | 2020-05-08 | 一汽解放汽车有限公司 | Carbon carrier for fuel cell, preparation method thereof and application thereof in fuel cell |
| CN112174130A (en) * | 2020-09-30 | 2021-01-05 | 福建海峡石墨烯产业技术研究院有限公司 | Preparation method of crosslinked thin-layer graphite serving as negative electrode of potassium ion battery |
| CN112850787A (en) * | 2021-01-27 | 2021-05-28 | 浙江高成绿能科技有限公司 | Catalyst carrier for fuel cell, catalyst and preparation method thereof |
| CN113506885A (en) * | 2021-06-25 | 2021-10-15 | 中自环保科技股份有限公司 | Graphitized carbon carrier for hydrogen fuel cell, preparation method and cell catalyst thereof |
| CN114122427A (en) * | 2020-08-27 | 2022-03-01 | 中国石油化工股份有限公司 | Platinum-carbon catalyst and preparation method and application thereof |
| CN114373944A (en) * | 2021-12-15 | 2022-04-19 | 青岛创启新能催化科技有限公司 | Preparation method of anti-reversal alloy catalyst for fuel cell |
| CN114497593A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Phosphorus-boron doped carbon material, platinum-carbon catalyst, and preparation methods and applications thereof |
| CN114824332A (en) * | 2022-03-29 | 2022-07-29 | 江苏龙蟠氢能源科技有限公司 | Preparation method of fuel cell platinum-carbon catalyst |
| CN115784294A (en) * | 2022-11-22 | 2023-03-14 | 国家电投集团氢能科技发展有限公司 | Metal oxide carrier and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111129518A (en) * | 2019-12-30 | 2020-05-08 | 一汽解放汽车有限公司 | Modified carbon carrier, preparation method thereof and application thereof in fuel cell |
| CN111129525A (en) * | 2019-12-30 | 2020-05-08 | 一汽解放汽车有限公司 | Carbon carrier for fuel cell, preparation method thereof and application thereof in fuel cell |
| CN114122427A (en) * | 2020-08-27 | 2022-03-01 | 中国石油化工股份有限公司 | Platinum-carbon catalyst and preparation method and application thereof |
| CN112174130A (en) * | 2020-09-30 | 2021-01-05 | 福建海峡石墨烯产业技术研究院有限公司 | Preparation method of crosslinked thin-layer graphite serving as negative electrode of potassium ion battery |
| CN114497593A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Phosphorus-boron doped carbon material, platinum-carbon catalyst, and preparation methods and applications thereof |
| CN114497593B (en) * | 2020-10-23 | 2024-04-02 | 中国石油化工股份有限公司 | Phosphorus-boron doped carbon material, platinum-carbon catalyst, and preparation methods and applications thereof |
| CN112850787A (en) * | 2021-01-27 | 2021-05-28 | 浙江高成绿能科技有限公司 | Catalyst carrier for fuel cell, catalyst and preparation method thereof |
| CN113506885A (en) * | 2021-06-25 | 2021-10-15 | 中自环保科技股份有限公司 | Graphitized carbon carrier for hydrogen fuel cell, preparation method and cell catalyst thereof |
| CN114373944A (en) * | 2021-12-15 | 2022-04-19 | 青岛创启新能催化科技有限公司 | Preparation method of anti-reversal alloy catalyst for fuel cell |
| CN114824332A (en) * | 2022-03-29 | 2022-07-29 | 江苏龙蟠氢能源科技有限公司 | Preparation method of fuel cell platinum-carbon catalyst |
| CN114824332B (en) * | 2022-03-29 | 2023-08-29 | 江苏龙蟠氢能源科技有限公司 | Preparation method of fuel cell platinum-carbon catalyst |
| CN115784294A (en) * | 2022-11-22 | 2023-03-14 | 国家电投集团氢能科技发展有限公司 | Metal oxide carrier and preparation method and application thereof |
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