CN108360010B - A kind of preparation method of solid oxide electrolysis cell electrode catalyst coating - Google Patents
A kind of preparation method of solid oxide electrolysis cell electrode catalyst coating Download PDFInfo
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- CN108360010B CN108360010B CN201810078244.XA CN201810078244A CN108360010B CN 108360010 B CN108360010 B CN 108360010B CN 201810078244 A CN201810078244 A CN 201810078244A CN 108360010 B CN108360010 B CN 108360010B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 33
- 239000007787 solid Substances 0.000 title claims abstract description 24
- 238000000576 coating method Methods 0.000 title claims abstract description 16
- 239000011248 coating agent Substances 0.000 title claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000011943 nanocatalyst Substances 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 4
- 238000011068 loading method Methods 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 7
- 230000001976 improved effect Effects 0.000 claims description 6
- 230000005611 electricity Effects 0.000 claims description 2
- 210000000988 bone and bone Anatomy 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 229910052751 metal Inorganic materials 0.000 abstract description 11
- 239000002184 metal Substances 0.000 abstract description 11
- 150000003839 salts Chemical class 0.000 abstract description 8
- 230000006641 stabilisation Effects 0.000 abstract description 3
- 238000011105 stabilization Methods 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000007598 dipping method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002803 maceration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
-
- 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
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B01J35/33—
-
- B01J35/40—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0221—Coating of particles
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
Abstract
The invention discloses a kind of preparation methods of solid oxide electrolysis cell electrode catalyst coating, comprising the following steps: (1) prepares nano-catalyst particles suspension;(2) suspension of step (1) is added in porous electrode surface, by uniform suspension is loaded in porous electrode using capillary force;(3) solvent is evaporated, catalyst nano-particles can be uniformly coated on electrode skeleton surface.The exemplary preparation method of the embodiment of the present invention replaces conventional metal salt predecessor to prepare electrode catalyst coating using the catalyst nano-particles of dispersion, to improve the dispersibility of electrode catalyst layer preparation efficiency and catalyst, the battery electrode of method preparation of the invention, carries out CO2Electrolysis, electrolytic cell has been run 220 hours, and in addition to the battery normal attenuation in 10 hours, battery electrolysis performance tends towards stability, and is that report battery performance has reached stabilization within 10 hours for the first time.
Description
Technical field
The present invention relates to the technical field of solid oxide electrolysis cell electrode catalyst preparation more particularly to a kind of solids
The preparation method of oxide electrolysis cells electrode catalyst coating.
Background technique
Using renewable energy, pass through solid oxide electrolysis cell electrolysis water, CO at high temperature2Or NOx etc., realization can
The storage of the renewable sources of energy, using or reduce environmental pollution.Relative to low-temperature electrolytic process, high-temperature electrolysis needs less electric energy,
It can use industrial exhaust heat, thus energy efficiency with higher.Catalyst is in these gas reactions of cathode surface electroreduction
In play an important role: reduce electrolysis energy consumption, improve electrolysis stability.Now using impregnation catalyst agent metal ion predecessor
Then metal ion is transformed into metal or metal oxide catalyst through Overheating Treatment by method.Catalyst is being made in order to prevent
Reunite during standby, using a small amount of multiple method, increases catalyst preparation process and cost.
The predecessor that nanocatalyst uses metal salt as catalyst is prepared on porous electrode surface now, at overheat
The predecessor is converted catalyst granules by reason.During heat treatment, newly-generated catalyst granules is be easy to cause to reunite.
Reunite frequently with each dipping loading capacity and multiple dipping the preparation method (on a small quantity repeatedly) is reduced to reduce.Catalyst is extended in this way
Preparation time increases preparation section and cost.Therefore, metal salt is used as the predecessor of catalyst and utilizes production in place
Nano particle the reunion of catalyst and the complexity and Gao Chengben of preparation section are caused as catalyst.
Solid oxide electrolysis cell can use renewable energy to produce fuel or decompose environmental contaminants.In Europe
Beauty, which has been used to production hydrogen or synthesis gas, to get rid of the dependence to fossil energy.The electrode performance of electrolytic cell and
Its stability has been largely fixed the technological industrialization.It is conventional to use predecessor and Re Chu of the metal salt as catalyst
The method that reason forms catalyst limits the improvement to electrode performance and its stability, needs a kind of new method for preparing catalyst
To reach the electrode of preparation high-performance and high stability.
Summary of the invention
Based on the above-mentioned prior art, the purpose of the present invention is to provide a kind of paintings of solid oxide electrolysis cell electrode catalyst
The preparation method of layer, the electrode catalyst preparation method for solving solid oxide electrolysis cell in the prior art be easy to cause catalysis
Agent particle agglomeration needs to reunite using a small amount of multiple repeated impregnations method to reduce, when increasing preparation cost, extending preparation
Between.
In a first aspect, the embodiment of the present application provides a kind of preparation side of solid oxide electrolysis cell electrode catalyst coating
Method, comprising the following steps: (1) prepare nano-catalyst particles suspension;(2) suspension of step (1) is added in porous electrode
Surface by uniform suspension is loaded in porous electrode using capillary force;(3) solvent is evaporated, catalyst nano-particles are
Electrode skeleton surface can be uniformly coated on.
It is preferred: by the hanging drop on porous electrode surface in the step (2).
Preferred: the partial size of nano-catalyst particles is 5-100nm in the step (1).
Preferred: the nano-catalyst particles suspension in the step (1) can be selected from commercial catalysts nano particle
Suspension or by nano-catalyst particles dispersion in a liquid, the liquid can be with for the those skilled in the art such as water, alcohol
The liquid for the dispersed catalyst nano particle expected.
Preferred: the step (2) is carried out by means of vacuum.
It is preferred: loading capacity and loading efficiency are controlled by control nano-catalyst particles content in the step (2),
In catalyst content 0-50%, catalyst granules loading capacity and loading efficiency are improved with the increase of its content.
Second aspect, the embodiment of the present application provide a kind of solid oxide electrolysis cell electrode, including any of the above-described institute
The catalyst coatings that the preparation method for the solid oxide electrolysis cell electrode catalyst coating stated is prepared.
Compared with prior art, the invention has the following advantages:
1, the preparation of solid oxide electrolysis cell catalyst is all the method for using dipping in the prior art, and is existed
The problem of reuniting in solid oxide electrolysis cell catalyst preparation process is all by dipping time and maceration extract at present
It is improved in concentration, improved effect is unobvious, and the present invention fundamentally solves the problems, such as this from method, overcomes technology inclined
See, the change on raw material is improved to nano-catalyst particles suspension by the metal salt solution of the prior art, avoids metal salt
Agglomeration traits during solution heated oxide, and by original impregnation preparation method be improved to coating mode, utilize hair
Tubule power and nano-catalyst particles are uniformly loaded in porous electrode by means of vacuum, the surface of electrode is made to adhere to one layer
Uniform catalyst layer, the exemplary method of the embodiment of the present invention can also be controlled by control nano-catalyst particles content
Loading capacity and loading efficiency, in catalyst content 0-50%, catalyst granules loading capacity and loading efficiency with its content increasing
Add and improve, solves in the prior art since catalyst metal salts amount in a solvent is by the limit of solubility and solution viscosity
System, so the problem of loading capacity difficult to realize to catalyst controls.
2, the battery electricity being prepared using the preparation method of solid oxide electrolysis cell electrode catalyst coating of the present invention
Pole carries out CO2Electrolysis, electrolytic cell have been run 220 hours, and in addition to the battery normal attenuation in 10 hours, battery is electrolysed performance
It tends towards stability, reports that battery performance has reached stabilization within 10 hours for the first time.
Detailed description of the invention
Fig. 1 is that the preparation method of the exemplary solid oxide electrolysis cell electrode catalyst coating of the embodiment of the present invention is prepared into
The solid oxide electrolysis cell electrolysis CO arrived2When, in Faradaic current 0.5A/cm2Under, decomposition voltage changes with time
Figure.
Specific embodiment
In order to be better understood by technical solution of the present invention, with reference to the accompanying drawings of the specification with specific embodiment to the present invention
It is described further.
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The application is described in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
The embodiment of the present application provides a kind of preparation method of solid oxide electrolysis cell electrode catalyst coating, including with
Lower step:
It is dispersed in the liquid such as water, alcohol using commercial catalysts nano granule suspension or by nano-catalyst particles, it will
The above-mentioned liquid containing catalyst nano-particles is added to the surface of porous electrode, it is preferred that is added in a manner of dropwise addition, Ke Yichong
It is multiple to be repeatedly added dropwise, to increase the loading capacity of catalyst nano-particles, catalyst nano-particles suspension is added using capillary force
It is loaded in porous electrode, and excludes bubble by means of vacuum, improve load effect;Then solvent is steamed on boiling temperature
Hair, catalyst nano-particles can be uniformly coated on electrode skeleton surface, and the loading capacity and loading efficiency of catalyst can benefits
It is controlled with the solid content in solution, in catalyst content 0-50%, catalyst granules loading capacity and loading efficiency contain with it
The increase of amount and improve.Since the amount of catalyst metal salts in a solvent is limited by solubility and solution viscosity, to catalyst
Loading capacity control it is limited.
This application provides a kind of preparation methods of completely new solid oxide electrolysis cell electrode catalyst, by this
New method solves a kind of serious hope solution in solid oxide electrolysis cell field of catalyst preparation but does not solve effectively
The certainly technical problem of scheme: existing electrode catalyst preparation method be easy to cause catalyst granules to reunite, and needs using a small amount of
Multiple repeated impregnations method is reunited to reduce, and is increased preparation cost and is extended preparation time.The present inventor is studying
In overcome and to solve the problems, such as that catalyst granules is easy to appear reunion from budget metals salting liquid in preparation in the prior art
Concentration and dipping time the technology prejudice that solves the problems, such as of angle, use in this field from original method, both
It solves the problems, such as catalyst granules reunion, and realizes and can control catalyst by adjusting the content of catalyst to realize
The problem of loading capacity and loading efficiency.
Solid oxide electrolysis cell prepared by the embodiment of the present application carries out CO2Electrolysis, electrode skeleton material is NiO/
YSZ (Y stable ZrO2), catalyst suspension is CeO2(10-20nm) is dispersed in acetic acid, is electrolysed CO2It is in 5%H2/CO2With
Faradaic current 0.5A/cm2Under, electrolytic cell has been run 220 hours, in addition to the battery normal attenuation in 10 hours, battery electrolysis
Performance tends towards stability, and is that report battery performance has reached stabilization within 10 hours for the first time, as shown in Figure 1.
The preparation method of the embodiment of the present application replaces conventional metal salt predecessor using the catalyst nano-particles of dispersion
Electrode catalyst coating is prepared, to improve the dispersibility of electrode catalyst layer preparation efficiency and catalyst.
Preferred: the partial size of the catalyst nano-particles is 5-100nm.
Preferred: the mode of solvent evaporation is drying, the condition of the drying be according to used solvent, will be
It is evaporated on the boiling point of solvent.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Claims (6)
1. a kind of preparation method of solid oxide electrolysis cell electrode catalyst coating, it is characterized in that: the following steps are included: (1)
Prepare nano-catalyst particles suspension;(2) suspension of step (1) is added in porous electrode surface, it will using capillary force
Load in porous electrode to uniform suspension;(3) solvent is evaporated, catalyst nano-particles can be uniformly coated on electrode bone
Frame surface,
Loading capacity and loading efficiency are controlled by control nano-catalyst particles content, in catalyst content 0-50%, is urged
Catalyst particles loading capacity and loading efficiency are improved with the increase of its content.
2. preparation method as described in claim 1, it is characterized in that: the partial size of nano-catalyst particles is in the step (1)
5-100nm。
3. preparation method as described in claim 1, it is characterized in that: the nano-catalyst particles suspension in the step (1)
It is that nano-catalyst particles dispersion is made in a liquid.
4. preparation method as described in claim 1, it is characterized in that: by the hanging drop in porous electricity in the step (2)
Pole surface.
5. preparation method as described in claim 1, it is characterized in that: the step (2) is carried out by means of vacuum.
6. a kind of solid oxide electrolysis cell electrode, it is characterized in that: including any soild oxide of claim 1-5
The catalyst coatings that the preparation method of electrolytic cell electrode catalyst coating is prepared.
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CN109468661B (en) * | 2018-12-18 | 2020-06-30 | 中南大学 | Composite oxygen electrode for solid oxide electrolytic cell and preparation method thereof |
CN112250437B (en) * | 2019-11-05 | 2022-08-05 | 济南大学 | Solid oxide electrolytic cell supported by oxygen electrode and preparation method thereof |
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Effective date of registration: 20240102 Address after: Room 13530, No. 260 Jiangshu Road, Xixing Street, Binjiang District, Hangzhou City, Zhejiang Province (self declared) Patentee after: Zhejiang Zhongxin Degu New Material Technology Co.,Ltd. Address before: Jinan University West Campus, no.336, nanxinzhuang West Road, Shizhong District, Jinan City, Shandong Province, 250022 Patentee before: University of Jinan |
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