CN108588742A - A method of preparing electrolysis water base metal bifunctional catalyst - Google Patents
A method of preparing electrolysis water base metal bifunctional catalyst Download PDFInfo
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- CN108588742A CN108588742A CN201810487534.XA CN201810487534A CN108588742A CN 108588742 A CN108588742 A CN 108588742A CN 201810487534 A CN201810487534 A CN 201810487534A CN 108588742 A CN108588742 A CN 108588742A
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- 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
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- 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
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- 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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Abstract
The present invention provides a kind of method preparing electrolysis water non-precious metal catalyst, including：（a）Layered double hydroxide is put into reaction solution, is stirred under the environmental protection of protective gas；（b）Single layer layered double hydroxide is obtained after centrifugation；（c）The single layer double-metal hydroxide and carbon carrier are mixed in proportion, after stirring, processing obtains carbon and carries layered double hydroxide catalyst.Catalyst prepared by this method can reduce the content of metal, have good catalytic effect simultaneously to evolving hydrogen reaction and oxygen evolution reaction.Compared with prior art, it by the self assembly of layered double hydroxide and carbon carrier under certain condition, realizes and prepares the purpose that the carbon with preferable catalytic activity carries layered double hydroxide catalyst.
Description
Technical field
The present invention relates to electrolysis water catalyst material fabricating technology field, especially a kind of electrolysis water for preparing is with non-
The method of noble metal catalyst.
Background technology
Electrolysis water is water (H2O) by the process of direct current electrolytically generated hydrogen and oxygen, electric current passes through water (H2When O), in the moon
Pole forms hydrogen (H by reductive water2), in anode oxygen (O is formed by aoxidizing water2).The oxygen that electrolysis water generates can be used for making
Oxygen equipment, hydrogen production quantity are about twice of oxygen, and industrialization hydrogen manufacturing can be realized by electrolysis water, is applied to fuel cell etc.
New energy field.Electrolyzed alkaline water hydrogen manufacturing is the main method of current industrialization electrolytic hydrogen production, but maximum existing for the technology is asked
Topic is to cause power consumption big, and to make, increased production cost.Operating current is lower to be primarily due in water electrolysis mistake
Cheng Zhong, Oxygen anodic evolution reaction need to slough four protons formation O -- O bonds from hydrone, and dynamic process is slow, therefore at
For the step of limiting entire electrolysis water reaction rate.
Catalyst can be such that the activation energy of electrolysis water substantially reduces, to reduce the overpotential of electrolysis water.Catalyst it is excellent
The bad transformation efficiency for determining the required total voltage of electrolysis water and electric energy and being converted to Hydrogen Energy.Currently, anode of electrolytic water analyses oxygen
Catalyst material mainly uses noble metal Ir and Ru, cathode hydrogen evolution catalyst material mainly to use precious metals pt.Due to noble metal
Distribution is rare, expensive so that the cost of electrolysis water still can not reduce, therefore there is an urgent need to develop efficient electrolysis water is non-
Precious metal catalyst agent material is electrolysed the dynamic process of elutriation oxygen to push, and the consumption of electric energy is reduced, to realize Cheap highly effective
Hydrogen manufacturing.Transition metal phosphide, sulfide, selenides and carbide etc. are successfully synthesized and are applied to effective at present
Catalyst is precipitated as oxygen in cathode hydrogen evolution catalyst, metal phosphide, sulfide, oxide/hydroxide etc., but about same
When have the report of the bifunctional catalyst of good catalytic effect less evolving hydrogen reaction and oxygen evolution reaction.It explores and preparation has
The base metal bifunctional catalyst of high catalytic activity becomes the research hotspot in the field.
Invention content
The object of the present invention is to provide a kind of methods preparing electrolysis water non-precious metal catalyst.Technical solution is as follows：
A method of electrolysis water non-precious metal catalyst is prepared, including：
（a）Layered double hydroxide is put into reaction solution, is stirred under the environmental protection of protective gas；
（b）Single layer layered double hydroxide is obtained after centrifugation；
（c）The single layer double-metal hydroxide and carbon carrier are mixed in proportion, after stirring, processing obtains carbon carrier layer shape
Double-metal hydroxide catalyst.
Preferably, the step（a）Laminate double-metal hydroxide is stratiform Ni-Al hydroxide, stratiform Mn-Co hydrogen
Oxide, stratiform Ni-Co hydroxide or Fe-Co hydroxide.
Preferably, the step（c）Middle carbon carrier is graphene, doped graphene, graphene oxide, carbon nanotube or charcoal
It is black.
Preferably, the step（a）Described in reaction solution be formamide solution.
Preferably, the step（a）Described in protective gas be nitrogen.
The step（c）Middle single layer double-metal hydroxide and carbon carrier mixed proportion are 1：1~10：1.
The step（a）Described in mixing time be 10~48 hours.
The step（b）Described in centrifugation rate be 600-2400 revs/min, time of centrifugation is 0.5~1 hour.
The step（c）Described in mixing time be 0.5~5 hour.
The step（c）In processing include centrifugation, filtering and drying.
Advantageous effect
In method provided by the invention, by layered double hydroxide carry out single layer separation after and carbon carrier in certain condition
Lower mixing, using centrifugation, filtering, drying the step of, obtain carbon carry layered double hydroxide catalyst.The present invention utilizes
Electrostatic Absorption between electropositive single layer double-metal hydroxide and electronegative carbon carrier forms carbon and carries layered bi-metal hydrogen
Oxide catalyst, catalyst prepared by such method can reduce the content of metal, have simultaneously to evolving hydrogen reaction and oxygen evolution reaction
There is good catalytic effect.Compared with prior art, by layered double hydroxide under certain condition and carbon carrier from
Assembling is realized and prepares the purpose that the carbon with preferable catalytic activity carries layered double hydroxide catalyst.
Description of the drawings
Fig. 1：The surface topography of graphene carrier layer shape Ni-Al hydroxide catalysts；
Fig. 2（a）~（b）：Graphene carrier layer shape Ni-Al, Mn-Co, Ni-Co, Fe-Co hydroxide（Ni-Al LDH@G、Mn-Co
LDH@G、Ni-Co LDH@G、Fe-Co LDH@G）With Ir/C catalyst to oxygen evolution reaction（OER）And evolving hydrogen reaction（HER）Urge
Change the performance test results；
Fig. 3：1.5V photovoltaics are electrolysed water installations schematic diagram.
Specific implementation mode
It elaborates to the present invention with reference to embodiment, but protection scope of the present invention is not limited only to following implementation
Example：
Embodiment one：
Using stratiform Ni-Al hydroxide as layered double hydroxide, using graphene as carbon carrier, with formamide solution
A kind of method preparing electrolysis water non-precious metal catalyst is provided using nitrogen as protective gas for reaction solution, including：
（a）Stratiform Ni-Al hydroxide is put into formamide solution, is stirred 10 hours under nitrogen protection environment；
（b）It uses rotating speed for 1200 revs/min of centrifugation rate, centrifuges 0.5 hour, single layer stratiform is obtained after centrifugation
Ni-Al layered hydroxides；
（c）The single layer Ni-Al hydroxide and graphene are pressed 5：1 ratio mixes, after stirring 0.5 hour, centrifuge, detach,
Graphene carrier layer shape Ni-Al hydroxide catalysts are obtained after drying.
Surface topography is observed：Using transmission electron microscope (TEM) to graphene carrier layer shape Ni-Al hydroxide obtained
Catalyst surface pattern is observed, and the results are shown in Figure 1：Single layer stratiform Ni-Al hydroxide is distributed on graphene.
Catalytic performance test：Fig. 2（a）~（b）It is graphene carrier layer shape Ni-Al, Mn-Co, Ni-Co, Fe-Co hydrogen-oxygen respectively
Compound（Ni-Al LDH@G、Mn-Co LDH@G、Ni-Co LDH@G、Fe-Co LDH@G）With Ir/C catalyst to oxygen evolution reaction
（OER）And evolving hydrogen reaction（HER）Catalytic performance test result.As seen from the figure：In Ir/C catalyst to oxygen evolution reaction（OER）It surveys
In examination, graphene carries starting point the becoming smaller compared with Ir/C catalyst of layered double hydroxide；In evolving hydrogen reaction（HER）It surveys
In examination, graphene carries the current density and take-off potential higher of layered double hydroxide catalyst, illustrates to pass through this method
The catalytic performance of the metal layer hydroxide of preparation is better than Ir and Pt catalyst.Fig. 3 is electrolysed using 1.5V photovoltaics
The schematic device of water can generate a large amount of hydrogen and oxygen by the device, after placing 0.5 minute, according to electrode liberation of hydrogen and
Analyse oxygen situation, it is known that the dynamic process of the electrolysis water process is improved.
Embodiment two：
Using stratiform Mn-Co hydroxide as layered double hydroxide, with doped graphene（N, S, B, P are adulterated）As carbon
Carrier, using nitrogen as protective gas, provides using formamide solution as reaction solution and a kind of preparing electrolysis water Non-precious Metal Catalysts
The method of agent, including：
（a）Stratiform Mn-Co hydroxide is put into formamide solution, is stirred 18 hours under nitrogen protection environment；
（b）It uses rotating speed for 1600 revs/min of rate, centrifuges 0.75 hour, single layer stratiform Mn-Co is obtained after centrifugation
Layered hydroxide；
（c）By the single layer Mn-Co hydroxide and doped graphene（N, S, B, P are adulterated）By 1：1 ratio mixes, stirring 1.5
After hour, doped graphene carrier layer shape Mn-Co hydroxide catalysts are obtained after centrifugation, separation, drying.
Embodiment three：
Using stratiform Ni-Co hydroxide as layered double hydroxide, using graphene oxide as carbon carrier, with formamide
Solution is reaction solution, using nitrogen as protective gas, provides a kind of method preparing electrolysis water non-precious metal catalyst, packet
It includes：
（a）Stratiform Ni-Co hydroxide is put into formamide solution, is stirred 28 hours under nitrogen protection environment；
（b）It uses rotating speed for 2400 revs/min of centrifugation rate, centrifuges 1 hour, single layer stratiform Ni- is obtained after centrifugation
Co layered hydroxides；
（c）The single layer Ni-Co hydroxide and graphene oxide are pressed 8：1 ratio mixes, and after stirring 2.5 hours, centrifugation divides
From, drying after obtain graphene oxide carrier layer shape Ni-Co hydroxide catalysts.
Example IV：
It is molten with formamide using carbon nanotube as carbon carrier using stratiform Fe-Co hydroxide as layered double hydroxide
Liquid is reaction solution, using nitrogen as protective gas, provides a kind of method preparing electrolysis water non-precious metal catalyst, including：
（a）Stratiform Fe-Co hydroxide is put into formamide solution, is stirred 38 hours under nitrogen protection environment；
（b）It uses rotating speed for 800 revs/min of centrifugation rate, centrifuges 0.8 hour, single layer stratiform Fe- is obtained after centrifugation
Co layered hydroxides；
（c）The single layer Fe-Co hydroxide and carbon nanotube are pressed 10：1 ratio mixes, and after stirring 3.5 hours, centrifugation divides
From, drying after obtain carbon nanotube carrier layer shape Fe-Co hydroxide catalysts.
Embodiment five：
Using stratiform Ni-Co hydroxide as layered double hydroxide, using carbon black as carbon carrier, it is with formamide solution
Reaction solution provides a kind of method preparing electrolysis water non-precious metal catalyst using nitrogen as protective gas, including：
（a）Stratiform Ni-Co hydroxide is put into formamide solution, is stirred 48 hours under nitrogen protection environment；
（b）It uses rotating speed for 600 revs/min of centrifugation rate, centrifuges 1 hour, single layer stratiform Ni-Co is obtained after centrifugation
Layered hydroxide；
（c）The single layer Ni-Co hydroxide and carbon black are pressed 3：1 ratio mixes, after stirring 5 hours, centrifugation, separation, drying
Carbon black carrier layer shape Ni-Co hydroxide catalysts are obtained afterwards.
Claims (10)
1. a kind of method preparing electrolysis water non-precious metal catalyst, which is characterized in that including：
（a）Layered double hydroxide is put into reaction solution, is stirred under the environmental protection of protective gas；
（b）Single layer layered double hydroxide is obtained after centrifugation；
（c）The single layer double-metal hydroxide and carbon carrier are mixed in proportion, after stirring, processing obtains carbon carrier layer shape
Double-metal hydroxide catalyst.
2. according to the method described in claim 1, it is characterized in that, the step（a）Laminate double-metal hydroxide is layer
Shape Ni-Al hydroxide, stratiform Mn-Co hydroxide, stratiform Ni-Co hydroxide or Fe-Co hydroxide.
3. according to the method described in claim 1, it is characterized in that, the step（c）Middle carbon carrier is graphene, doped graphite
Alkene, graphene oxide, carbon nanotube or carbon black.
4. according to the method described in claim 1, it is characterized in that, the step（a）Described in reaction solution be formamide it is molten
Liquid.
5. according to the method described in claim 1, it is characterized in that, the step（a）Described in protective gas be nitrogen.
6. according to the method described in claim 1, it is characterized in that, the step（c）Middle single layer double-metal hydroxide and carbon
Carrier mixed proportion is 1：1~10：1.
7. according to the method described in claim 1, it is characterized in that, the step（a）Described in mixing time be 10~48 small
When.
8. according to the method described in claim 1, it is characterized in that, the step（b）Described in centrifugation rate be 600-2400
Rev/min, the time of centrifugation is 0.5~1 hour.
9. according to the method described in claim 1, it is characterized in that, the step（c）Described in mixing time be 0.5~5 small
When.
10. according to the method described in claim 1, it is characterized in that, the step（c）In processing include centrifugation, filtering and
Drying.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201069A (en) * | 2018-11-01 | 2019-01-15 | 陕西科技大学 | A kind of ternary metal hydroxide elctro-catalyst and preparation method thereof |
| CN109225233A (en) * | 2018-10-26 | 2019-01-18 | 陕西科技大学 | A kind of layered double hydroxide/carbon quantum dot elctro-catalyst and preparation method thereof |
| CN109371420A (en) * | 2018-12-19 | 2019-02-22 | 中国科学院理化技术研究所 | A kind of single layered porous nickel-ferric spinel base electro-catalysis analysis oxygen electrode with and its preparation method and application |
| CN110152673A (en) * | 2019-05-10 | 2019-08-23 | 安徽师范大学 | Iron nickel layered double hydroxide/nickel foam composite material and preparation method and application |
| CN111135832A (en) * | 2020-01-13 | 2020-05-12 | 北京大学深圳研究生院 | Preparation method of porous structure catalyst for producing oxygen by electrolyzing water |
| CN112359373A (en) * | 2019-07-24 | 2021-02-12 | 中国科学院福建物质结构研究所 | Amorphous composite material, preparation method and application thereof |
| CN114653376A (en) * | 2022-03-29 | 2022-06-24 | 浙江工业大学绍兴研究院 | Method for removing ofloxacin by activating persulfate through composite material |
| CN114717585A (en) * | 2022-03-07 | 2022-07-08 | 华南农业大学 | Double-transition metal electrode material, preparation method thereof and application thereof in hydrogen production by photovoltaic electrolysis of water |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109225233A (en) * | 2018-10-26 | 2019-01-18 | 陕西科技大学 | A kind of layered double hydroxide/carbon quantum dot elctro-catalyst and preparation method thereof |
| CN109225233B (en) * | 2018-10-26 | 2021-08-13 | 陕西科技大学 | Layered double metal hydroxide/carbon quantum dot electrocatalyst and preparation method thereof |
| CN109201069A (en) * | 2018-11-01 | 2019-01-15 | 陕西科技大学 | A kind of ternary metal hydroxide elctro-catalyst and preparation method thereof |
| CN109371420A (en) * | 2018-12-19 | 2019-02-22 | 中国科学院理化技术研究所 | A kind of single layered porous nickel-ferric spinel base electro-catalysis analysis oxygen electrode with and its preparation method and application |
| CN109371420B (en) * | 2018-12-19 | 2020-08-25 | 中国科学院理化技术研究所 | Single-layer porous nickel-iron hydrotalcite-based electrocatalytic oxygen evolution electrode and preparation method and application thereof |
| CN110152673A (en) * | 2019-05-10 | 2019-08-23 | 安徽师范大学 | Iron nickel layered double hydroxide/nickel foam composite material and preparation method and application |
| CN112359373A (en) * | 2019-07-24 | 2021-02-12 | 中国科学院福建物质结构研究所 | Amorphous composite material, preparation method and application thereof |
| CN112359373B (en) * | 2019-07-24 | 2022-06-10 | 中国科学院福建物质结构研究所 | Amorphous composite material, preparation method and application thereof |
| CN111135832A (en) * | 2020-01-13 | 2020-05-12 | 北京大学深圳研究生院 | Preparation method of porous structure catalyst for producing oxygen by electrolyzing water |
| CN114717585A (en) * | 2022-03-07 | 2022-07-08 | 华南农业大学 | Double-transition metal electrode material, preparation method thereof and application thereof in hydrogen production by photovoltaic electrolysis of water |
| CN114717585B (en) * | 2022-03-07 | 2023-09-22 | 华南农业大学 | Double-transition metal electrode material, preparation method thereof and application thereof in hydrogen production by photovoltaic water electrolysis |
| CN114653376A (en) * | 2022-03-29 | 2022-06-24 | 浙江工业大学绍兴研究院 | Method for removing ofloxacin by activating persulfate through composite material |
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