CN110201670A - Based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent, preparation method and application - Google Patents
Based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent, preparation method and application Download PDFInfo
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- CN110201670A CN110201670A CN201910547975.9A CN201910547975A CN110201670A CN 110201670 A CN110201670 A CN 110201670A CN 201910547975 A CN201910547975 A CN 201910547975A CN 110201670 A CN110201670 A CN 110201670A
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- Prior art keywords
- urea
- metal hydroxide
- eutectic solvent
- foam
- nickel
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 188
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000004202 carbamide Substances 0.000 title claims abstract description 82
- 239000002904 solvent Substances 0.000 title claims abstract description 61
- 230000005496 eutectics Effects 0.000 title claims abstract description 58
- 229910000863 Ferronickel Inorganic materials 0.000 title claims abstract description 52
- 229910000000 metal hydroxide Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 32
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 title claims abstract description 23
- 239000006260 foam Substances 0.000 claims abstract description 83
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 74
- 239000003054 catalyst Substances 0.000 claims abstract description 52
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 19
- 230000003197 catalytic effect Effects 0.000 claims abstract description 15
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000007868 Raney catalyst Substances 0.000 claims description 9
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002057 nanoflower Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000011017 operating method Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- 230000010287 polarization Effects 0.000 description 6
- 238000002203 pretreatment Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- 235000019743 Choline chloride Nutrition 0.000 description 2
- 229910016874 Fe(NO3) Inorganic materials 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical group [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 2
- 229960003178 choline chloride Drugs 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- 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
- B01J25/00—Catalysts of the Raney type
- B01J25/02—Raney nickel
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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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
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- C25B11/031—Porous electrodes
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- 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
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- 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
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Abstract
The present invention provides a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent, preparation method and application.The present invention prepares ferronickel double-metal hydroxide/foamed nickel catalyst agent using eutectic solvent prepared by Iron(III) chloride hexahydrate and urea, it is raw materials used cheap and easy to get, at low cost, operating procedure is extremely simple, reaction condition is easily achieved, hot conditions are not needed, energy consumption is few, and short preparation period, is suitable for industrialized production.Obtained catalyst is the ferronickel double-metal hydroxide being carried in nickel foam, and catalytic active component therein is ferronickel double-metal hydroxide (NiFe-LDH), with hierarchical structure, i.e. the nano flower-like structure of nanometer sheet composition.Gained catalyst has the performance of preferable electro-catalysis electrolysis water and urea.
Description
Technical field
The present invention relates to a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/nickel foam
Catalyst, preparation method and application, belong to technical field of energy material.
Background technique
Currently, causing extremely serious environmental pollution using petroleum, coal as the excessive use of the traditional energy of representative, simultaneously
The problems such as risk of energy depletion, environmental pollution, energy shortage, arouses widespread concern.For this reason, it may be necessary to develop green
The energy is to meet human demand and reduce environmental pollution.Wherein, Hydrogen Energy has many advantages, such as clean and effective, and electro-catalysis water-splitting is system
One of important method of hydrogen.However, during electro-catalysis water-splitting, due to the presence of oxygen evolution reaction (OER), needed for water-splitting
The theoretical voltage wanted is 1.23V, significantly limits the application of electrolysis water.So people need electricity required for reducing hydrogen manufacturing
Pressure, therefore be electrolysed urea application and give birth to.It is electrolysed urea (UOR, CO (NH2)2+H2O===N2+3H2+CO2) required for theory
Voltage is only 0.37V；More it is noted that electrolysis urea can also handle urea waste water, there is higher application value.
For more efficient electrolysis water and urea, the research of elctro-catalyst becomes hot spot.Ferronickel double-metal hydroxide
It (NiFe-LDH) is a kind of common electrolysis water oxygen-separating catalyst, it is good to possess catalytic performance, easily prepared, and it is excellent that structure is adjustable etc.
Point；Preparation method has hydro-thermal method, electrodeposition process, infusion process etc..Chinese patent literature CN108283926A discloses one kind
The preparation method of ferronickel double-metal hydroxide of the growth in situ in nickel foam with layer structure；Using six nitric hydrates
Nickel, Fe(NO3)39H2O, urea, ammonium fluoride and nickel foam are primary raw material, by Nickelous nitrate hexahydrate, Fe(NO3)39H2O, urine
Element and ammonium fluoride are added to the water uniformly mixed, and treated nickel foam is then added, is most made afterwards through hydro-thermal reaction.This method is adopted
It with hydro-thermal method, consumes energy higher, and preparation time is longer；Gained catalyst produces VPO catalysts as electro-catalysis and mentions to a certain extent
OER catalytic performance under high alkaline condition, but OER catalytic performance is still wait further increase.
It meanwhile currently based on report of the double-metal hydroxide in terms of being electrolysed urea being still blank.
Eutectic solvent refer to by certain stoichiometric ratio hydrogen bond receptor (such as quaternary ammonium salt) and hydrogen-bond donor (such as amide,
The compounds such as carboxylic acid and polyalcohol) two components that are composed or three component eutectic mixtures, freezing point it is substantially less than each
The freezing point of a component pure material.One of the most common eutectic solvent is choline chloride/urea, choline chloride/glycerine etc..
As ionic liquid analog, the advantages of eutectic solvent possesses ionic liquid, while eutectic solvent also have it is easily prepared,
Good biocompatibility, the low equal unique advantage of toxicity.Therefore eutectic solvent is widely used in the preparation of inorganic nano material.
But currently without the report for preparing ferronickel double-metal hydroxide (NiFe-LDH) using eutectic solvent.
Summary of the invention
In view of the deficienciess of the prior art, the present invention provide it is a kind of based on ferric trichloride/urea eutectic solvent nickel
Iron double metal hydroxide/foamed nickel catalyst agent and preparation method thereof.The present invention is prepared using Iron(III) chloride hexahydrate and urea
Eutectic solvent prepare ferronickel double-metal hydroxide/foamed nickel catalyst agent, raw materials used cheap and easy to get, at low cost, behaviour
It is extremely simple to make technique, reaction condition is easily achieved, and does not need hot conditions, and energy consumption is few, and short preparation period, is suitable for industrialization
Production.Obtained catalyst is the ferronickel double-metal hydroxide being carried in nickel foam, and catalytic active component is ferronickel
Double-metal hydroxide (NiFe-LDH).Ferronickel double-metal hydroxide prepared by the present invention has hierarchical structure, i.e. nanometer
The nano flower-like structure of piece composition, the performance with biggish specific surface area and preferable electro-catalysis electrolysis water and urea.
The present invention also provides a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foam
Raney nickel is electrolysed the application in urea and water in electro-catalysis.
Term explanation:
Ferronickel double-metal hydroxide/foamed nickel catalyst agent: refer to that ferronickel double-metal hydroxide (NiFe-LDH) is carried on
In nickel foam, electro catalytic activity ingredient is ferronickel double-metal hydroxide (NiFe-LDH)；Nickel foam is mainly carrier, electro-catalysis
Activity is poor.
Technical scheme is as follows:
It is a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent, it is described
Ferronickel double-metal hydroxide in catalyst is catalytic active component, and nickel foam is carrier, and ferronickel double-metal hydroxide is negative
It is loaded in foam nickel surface；The microscopic appearance of the ferronickel double-metal hydroxide is the nano flower-like structure of nanometer sheet composition,
The diameter of middle nano flower be 0.8-1.2 μm, nanometer sheet with a thickness of 11-14nm.
Preferred according to the present invention, the catalyst is that nickel foam is placed in reaction in eutectic solvent to be prepared；Institute
Stating eutectic solvent is to be prepared by Iron(III) chloride hexahydrate and urea for raw material.
It is above-mentioned based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent system
Preparation Method, comprising steps of
(1) Iron(III) chloride hexahydrate and urea are mixed, heats 10min-1h at 40-100 DEG C, obtains eutectic solvent；
(2) pure nickel foam is immersed in the eutectic solvent that step (1) obtains, reacts 10s- at 40-100 DEG C
1min；Then washed, be drying to obtain ferronickel double-metal hydroxide/foamed nickel catalyst agent.
Preferred according to the present invention, the molar ratio of Iron(III) chloride hexahydrate described in step (1) and urea is 1:3-3:1；
Preferably, the molar ratio of the Iron(III) chloride hexahydrate and urea is 2:1.
Preferred according to the present invention, heating temperature described in step (1) is 60 DEG C, heating time 30min.
Preferred according to the present invention, pure nickel foam is the preparation method is as follows: nickel foam is successively set described in step (2)
In the hydrochloric acid of 0.5-3mol/L ultrasound 5-20min, be placed in water ultrasonic 5-15min, be placed in ultrasound 5-15min in ethyl alcohol, with
The impurity such as foam surface oxides are removed, are then drying to obtain through room temperature in vacuo.
Preferably, the nickel foam is having a size of 0.5*0.5cm2-2*2cm2Square；It is further preferred that the bubble
The size of foam nickel is 1*1cm2。
Preferably, the molar concentration of the hydrochloric acid is 1mol/L, and the ultrasonic time in hydrochloric acid is 10min；Yu Shuizhong's
Ultrasonic time is 10min；Ultrasonic time in ethyl alcohol is 10min；Room temperature in vacuo drying time is 12h.
Preferred according to the present invention, reaction temperature described in step (2) is 60 DEG C, reaction time 30s.
Preferred according to the present invention, washing is respectively washed 3 times with second alcohol and water described in step (2)；The drying be
It is dried in vacuo 12h at room temperature.
It is above-mentioned to be answered based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent
With applied to electro-catalysis electrolysis urea or electrolysis water.As electrolysis urea or electrolysis water catalyst, it is applied to electro-catalysis, photoelectricity
Catalysis, the processing of basic hydrolysis hydrogen generator, urea waste water etc..
It technical characterstic of the invention and has the beneficial effect that:
1, eutectic solvent is quickly prepared by the way that Iron(III) chloride hexahydrate and urea to be simply mixed in the present invention；Then
Pure nickel foam is briefly dipped into, ferronickel double-metal hydroxide/foamed nickel catalyst agent is quickly prepared.Institute of the present invention
It is cheap and easy to get, at low cost with raw material；Technique is extremely simple, easy to operate, and reaction condition is easily achieved, and does not need hot conditions,
Energy consumption is few, and manufacturing cycle is extremely short, is conducive to large-scale industrial production.
2, the present invention utilizes this kind of specific eutectic solvent of Iron(III) chloride hexahydrate/urea, had not only done source of iron but also had made solvent,
Be used as carrier again while using nickel foam as nickel source, successfully prepare inorganic nano material ferronickel double-metal hydroxide/
Foamed nickel catalyst agent.
Reaction equation of the present invention is as follows:
CO(NH2)2+H2O→2NH3+CO2 (1)
NH3+H2O→NH4 ++OH- (2)
2Fe3++Ni→2Fe2++Ni2+ (3)
Ni2++Fe3++OH-→NiFe-LDH (4)
H in urea and Iron(III) chloride hexahydrate2O reaction, hydrolyzable is at NH4+And OH-(equation (1) and (2)).Work as bubble
When foam nickel is as template and substrate immersion eutectic solvent is sacrificed, it can be by Fe therein3+It is oxidized to Ni2+.Then in nickel foam
Upper Ni2+、Fe3+And OH-Fabricated in situ NiFe-LDH nanostructure.During the reaction, the color of nickel foam is from initial silver grey
Discoloration is dark yellow.The ferronickel bimetallic hydrogen for being carried on foam nickel surface is prepared using specific eutectic solvent by the present invention
Oxide.The wherein nanometer that ferronickel double-metal hydroxide is made of as catalytic active component, microscopic appearance nanometer sheet
Flower-like structure has biggish specific surface area；And nickel foam can further increase specific surface area primarily as carrier, and have
Conducive to the transmitting of electronics, but catalytic activity itself is weaker.
3. the performance that catalyst prepared by the present invention has excellent electrolysis urea and electrolysis water.Especially urea oxidation and
It is electrolysed the performance of elutriation oxygen, is better than the catalyst of current most of reports.Under alkaline condition, current density 10mA/cm2
When, voltage required for urea aoxidizes is down to 1.32V, and voltage needed for being electrolysed elutriation oxygen is down to 1.39V, required for urea electrolysis
Voltage is down to 1.52V, and full water electrolysis voltage is down to 1.61V；It can be seen from the above, voltage needed for urea oxidation is less than electrolysis water
Voltage needed for analysing oxygen illustrates compared to conventional electrolyzed alkaline water hydrogen manufacturing, catalyst alkaline electrolysis urea reaction tool of the present invention
There is lower voltage, significantly reduces the power consumption of electrolytic hydrogen production, improve the market competitiveness.Meanwhile present invention gained catalysis
The electrocatalysis characteristic of agent is better than illustrating the specific eutectic of the present invention without using catalyst obtained by eutectic solvent (being replaced with water)
The superiority of solvent is conducive to prepare the high catalyst of electro catalytic activity.Catalyst prepared by the present invention is applied to electro-catalysis
Not only catalytic performance is good for electrolysis water or urea, also with good stability.
Detailed description of the invention
Fig. 1 is the x-ray powder of the NiFe-LDH of nickel foam area load in 1 gained catalyst of embodiment 1 and comparative example
Diffracting spectrum；Wherein, the NiFe-LDH in embodiment 1 is referred to as NiFe-LDH_D, and the NiFe-LDH in comparative example 1 is referred to as
NiFe-LDH_W。
Fig. 2 is that the scanning electron microscope of NiFe-LDH in the catalyst of embodiment 1 (Fig. 2 a) and comparative example 1 (Fig. 2 b) preparation is shone
Piece.
Fig. 3 is the electrocatalytic oxidation urea and electrolysis elutriation oxygen of 2 gained catalyst of embodiment 1, comparative example 1 and comparative example
It can comparison diagram and stability test figure.
Fig. 4 is the polarization curve comparison diagram and stability of the electrolysis urea and full water electrolysis of 1 gained catalyst of embodiment
Test chart.
Specific embodiment
The present invention will be further described combined with specific embodiments below, but not limited to this.
Experimental method described in embodiments following simultaneously is unless otherwise specified conventional method；The reagent and material
Material, unless otherwise specified, commercially obtains.
In embodiment, the nickel foam, Liyuan New Material Co Ltd, Changsha is on sale.
Embodiment 1
It is a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent system
Preparation Method, comprising steps of
(1) synthesis of eutectic solvent: Iron(III) chloride hexahydrate and urea are mixed with the molar ratio of 2:1, subsequent oil bath
At 60 DEG C, 30min is heated, a kind of viscosity of the larger liquid of rufous is obtained, is cooled to room temperature, is i.e. successfully six hydration three of synthesis
Iron chloride/urea eutectic solvent.
(2) pre-treatment of nickel foam: it is 1*1cm that nickel foam, which is cut into size,2Square, then use 1mol/L hydrochloric acid
It is ultrasonically treated 10min, water and ethyl alcohol ultrasound 10min respectively are reused, to remove the oxide and impurity on surface.Last room temperature
12h is dried in vacuo up to pure nickel foam.
(3) above-mentioned pure nickel foam the preparation of NiFe-LDH/ foamed nickel catalyst agent: is immersed in what step (1) obtained
In eutectic solvent, 30s is reacted at 60 DEG C.Nickel foam is then taken out into (nickel foam area load has NiFe-LDH), uses ethyl alcohol
It is respectively washed with water 3 times, is dried in vacuo 12h at room temperature to get NiFe-LDH/ foamed nickel catalyst agent (referred to as NiFe-LDH_D/
NF)。
The powder of nickel foam area load in catalyst of the present invention is taken, X-ray powder diffraction pattern is as shown in Figure 1.By
Fig. 1 is it is found that the substance of nickel foam area load is NiFe-LDH, and pure, free from admixture in catalyst of the present invention.
The stereoscan photograph of NiFe-LDH is as shown in Figure 2 a in the catalyst that the present embodiment is prepared.It can by Fig. 2 a
Know, the microscopic appearance of the NiFe-LDH of nickel foam area load is the nano flower-like structure of nanometer sheet composition, wherein nano flower
Diameter is at 1 μm or so, and the thickness of nanometer sheet is about 11.5-13.4nm.
The catalyst that the present embodiment is prepared is aoxidized applied to urea, and concrete application method is as follows:
Electrochemical workstation model Shanghai Chen Hua 760E used in the present invention.Wherein, electrolyte be 1mol/L KOH,
The aqueous solution of 0.5mol/L urea.For gained NiFe-LDH_D/NF of the invention directly as working electrode, saturated calomel electrode is ginseng
Than electrode, carbon-point is to electrode.Electro-chemical test, sweep speed 5mV/s are carried out using polarization curve.
The urea oxidation susceptibility (UOR) of catalyst obtained by the present embodiment as shown in Figure 3a, by Fig. 3 a it is found that current density
It is 10mA/cm2When, required current potential is only 1.32V, illustrates that catalyst activity prepared by the present invention is higher.
Catalyst urea oxidation prepared by the present invention simultaneously has good stability, such as Fig. 3 c it is found that its starting
The polarization curve polarization curve later with 1000 circle of scanning essentially coincides, and illustrates the good steady of catalyst prepared by the present invention
It is qualitative.
Catalyst prepared by the present embodiment is applied to electrolysis elutriation oxygen (OER), concrete application method is as follows:
In addition to used electrolyte is 1mol/LKOH, other test conditions and method are identical as urea oxidation.
The electrolysis elutriation oxygen performance of catalyst obtained by the present embodiment is as shown in Figure 3b, by Fig. 3 b it is found that current density is
10mA/cm2When, required current potential is only 1.39V, illustrates that catalyst activity prepared by the present invention is higher.
Catalyst prepared by the present invention produces oxygen and has good stability simultaneously, such as Fig. 3 d, by Fig. 3 d it is found that it is originated
Polarization curve essentially coincided with the 1000 later polarization curve of circle of scanning, illustrate the good steady of catalyst prepared by the present invention
It is qualitative.
The catalyst that the present embodiment is prepared is applied to electrolysis urea or full water electrolysis, concrete application method are as follows:
Used electrochemical workstation is Shanghai Chen Hua 760E, and prepared catalyst had not only made cathode but also made anode.Make
Electrolyte is 1mol/L KOH, 0.5mol/L aqueous solution of urea or 1mol/L KOH aqueous solution, sweep speed 5mV/s.
The performance map of the electrolysis urea of catalyst obtained by the present embodiment is as shown in Figs. 4a and 4b.By Fig. 4 a it is found that carrying out
When being electrolysed urea, current density 10mA/cm2When, required current potential is only 1.52V.By Fig. 4 b it is found that in scanning 1000
Curve obtained is essentially coincided with virgin curve after circle, illustrates that catalyst prepared by the present invention can carry out urea electrolytic experiment, and
And there is good stability.
The performance map of the electrolysis water of catalyst obtained by the present embodiment is as shown in Fig. 4 a and 4c.By Fig. 4 a it is found that carrying out electricity
When solving water, current density is 10mA/cm2When, required current potential is only 1.61V.By Fig. 4 c it is found that after the circle of scanning 1000
Curve obtained is essentially coincided with virgin curve, illustrates that catalyst prepared by the present invention can carry out full water electrolysis experiment, and
There is good stability.
Embodiment 2
It is a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent system
Preparation Method, comprising steps of
(1) synthesis of eutectic solvent: Iron(III) chloride hexahydrate and urea are mixed with the molar ratio of 1:1, subsequent oil bath
At 60 DEG C, 30min is heated, a kind of viscosity of the larger liquid of rufous is obtained, is cooled to room temperature, is i.e. successfully six hydration three of synthesis
Iron chloride/urea eutectic solvent.
(2) nickel foam the pre-treatment of nickel foam: is cut into 0.5*0.5cm2Square, subsequent processing steps and condition
As described in Example 1, pure nickel foam is obtained.
(3) above-mentioned pure nickel foam the preparation of NiFe-LDH/ foamed nickel catalyst agent: is immersed in what step (1) obtained
In eutectic solvent, 10s is reacted at 40 DEG C.Then take out nickel foam (nickel foam area load has NiFe-LDH), with ethyl alcohol and
Water respectively washs 3 times, is dried in vacuo 12h at room temperature to get NiFe-LDH/ foamed nickel catalyst agent.
Embodiment 3
It is a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent system
Preparation Method, comprising steps of
(1) synthesis of eutectic solvent: Iron(III) chloride hexahydrate and urea are mixed with the molar ratio of 3:1, subsequent oil bath
At 60 DEG C, 30min is heated, a kind of viscosity of the larger liquid of rufous is obtained, is cooled to room temperature, is i.e. successfully six hydration three of synthesis
Iron chloride/urea eutectic solvent.
(2) nickel foam the pre-treatment of nickel foam: is cut into 2*2cm2Square, subsequent processing steps and condition are strictly according to the facts
It applies and obtains pure nickel foam described in example 1.
(3) above-mentioned pure nickel foam the preparation of NiFe-LDH/ foamed nickel catalyst agent: is immersed in what step (1) obtained
In eutectic solvent, 40s is reacted at 80 DEG C.Then take out nickel foam (nickel foam area load has NiFe-LDH), with ethyl alcohol and
Water respectively washs 3 times, is dried in vacuo 12h at room temperature to get NiFe-LDH/ foamed nickel catalyst agent.
Embodiment 4
It is a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent system
Preparation Method, comprising steps of
(1) synthesis of eutectic solvent: Iron(III) chloride hexahydrate and urea are mixed with the molar ratio of 1:2, subsequent oil bath
At 60 DEG C, 30min is heated, a kind of viscosity of the larger liquid of rufous is obtained, is cooled to room temperature, is i.e. successfully six hydration three of synthesis
Iron chloride/urea eutectic solvent.
(2) nickel foam the pre-treatment of nickel foam: is cut into 1*1cm2Square, subsequent processing steps and condition are strictly according to the facts
It applies and obtains pure nickel foam described in example 1.
(3) above-mentioned pure nickel foam the preparation of NiFe-LDH/ foamed nickel catalyst agent: is immersed in what step (1) obtained
In eutectic solvent, 30s is reacted at 60 DEG C.Then take out nickel foam (nickel foam area load has NiFe-LDH), with ethyl alcohol and
Water respectively washs 3 times, is dried in vacuo 12h at room temperature to get NiFe-LDH/ foamed nickel catalyst agent.
Comparative example 1
A kind of preparation method of ferronickel double-metal hydroxide/foamed nickel catalyst agent, comprising steps of
(1) Iron(III) chloride hexahydrate is dissolved in water, at 60 DEG C of subsequent oil bath, heats 30min, it is (described to obtain mixed liquor
The volume of mixed liquor is identical as the gained volume of eutectic solvent in embodiment 1, the quality and reality of the Iron(III) chloride hexahydrate
It is identical to apply example 1).
(2) pre-treatment of nickel foam is as described in Example 1, obtains pure nickel foam.
(3) above-mentioned pure nickel foam the preparation of NiFe-LDH/ foamed nickel catalyst agent: is immersed in what step (1) obtained
In mixed liquor, 30s is reacted at 60 DEG C.Nickel foam (nickel foam area load has ferronickel double-metal hydroxide) then is taken out, is used
Second alcohol and water respectively washs 3 times, is dried in vacuo 12h at room temperature to get ferronickel double-metal hydroxide/foamed nickel catalyst agent (letter
Referred to as NiFe-LDH_W/NF).
The powder of nickel foam area load in this comparative example catalyst is taken, X-ray powder diffraction pattern is as shown in Figure 1.
As shown in Figure 1, the powder of nickel foam area load is NiFe-LDH, but in addition to the peak of NiFe-LDH, there is also have nickel
Peak, nickel derive from nickel foam, illustrate that the skeleton of nickel foam receives destruction.
The stereoscan photograph of NiFe-LDH is as shown in Figure 2 b in the catalyst that this comparative example is prepared.It can by Fig. 2 b
Know, the microscopic appearance of the NiFe-LDH of nickel foam area load is flaky nanometer structure, and structure is uneven.
Catalyst obtained by this comparative example is applied in urea oxidation by the method for the embodiment of the present invention 1；By Fig. 3 a it is found that
Current density is 10mA/cm2When, required current potential is 1.37V, is higher than the embodiment of the present invention 1, and it is low to illustrate that the present invention uses
The catalyst of congruent melting solvent preparation has the performance of better electrocatalytic oxidation urea.
Catalyst obtained by this comparative example is applied in electrolysis elutriation oxygen by the method for the embodiment of the present invention 1；It can by Fig. 3 b
Know, current density is 10mA/cm2When, required current potential is 1.41V, is higher than the embodiment of the present invention 1, illustrates that the present invention makes
With catalyst prepared by eutectic solvent there is better electro-catalysis to be electrolysed elutriation oxygen performance.
As the above comparative experiments it is found that the electrocatalysis characteristic of catalyst obtained by the embodiment of the present invention 1 is better than in comparative example 1
The electrocatalysis characteristic of gained catalyst illustrates the superiority of low cosolvent, is conducive to prepare the high catalyst of catalytic activity.
Comparative example 2
Pre-treatment is carried out to nickel foam by the method for 1 step of embodiment (2), obtains pure nickel foam (referred to as NF).
NF obtained by this comparative example is applied to urea oxidation by the method for the embodiment of the present invention 1 and is electrolysed in elutriation oxygen.
Such as Fig. 3 a, 3b is it is found that either urea oxidation or electrolysis elutriation oxygen, the electrocatalysis characteristic of pure nickel foam can be ignored not
Meter.Illustrate in catalyst prepared by the present invention, catalytic active component is ferronickel double-metal hydroxide, and nickel foam therein is main
Play carrier, and ferronickel double-metal hydroxide can effectively reduce current potential, electro catalytic activity with higher.
Claims (10)
1. a kind of based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foamed nickel catalyst agent, feature
It is, the ferronickel double-metal hydroxide in the catalyst is catalytic active component, and nickel foam is carrier, ferronickel bimetallic hydrogen
It is oxide carried in foam nickel surface；The microscopic appearance of the ferronickel double-metal hydroxide is the nano flower-like of nanometer sheet composition
Structure, wherein the diameter of nano flower be 0.8-1.2 μm, nanometer sheet with a thickness of 11-14nm.
2. according to claim 1 based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foam
Raney nickel, which is characterized in that the catalyst is that nickel foam is placed in reaction in eutectic solvent to be prepared；It is described low total
Molten solvent is to be prepared by Iron(III) chloride hexahydrate and urea for raw material.
3. as claims 1 or 2 is described in any item based on ferric trichloride/urea eutectic solvent ferronickel bimetal hydroxide
Object/foamed nickel catalyst agent preparation method, comprising steps of
(1) Iron(III) chloride hexahydrate and urea are mixed, heats 10min-1h at 40-100 DEG C, obtains eutectic solvent；
(2) pure nickel foam is immersed in the eutectic solvent that step (1) obtains, reacts 10s-1min at 40-100 DEG C；So
By washing, be drying to obtain ferronickel double-metal hydroxide/foamed nickel catalyst agent.
4. according to claim 3 based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foam
The preparation method of Raney nickel, which is characterized in that the molar ratio of Iron(III) chloride hexahydrate described in step (1) and urea is 1:3-
3:1；Preferably, the molar ratio of the Iron(III) chloride hexahydrate and urea is 2:1.
5. according to claim 3 based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foam
The preparation method of Raney nickel, which is characterized in that heating temperature described in step (1) is 60 DEG C, heating time 30min.
6. according to claim 3 based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foam
The preparation method of Raney nickel, which is characterized in that pure nickel foam is the preparation method is as follows: by nickel foam described in step (2)
It is sequentially placed into ultrasound 5-20min in the hydrochloric acid of 0.5-3mol/L, ultrasonic 5-15min is placed in water, is placed in ultrasound 5- in ethyl alcohol
Then 15min is drying to obtain through room temperature in vacuo.
7. according to claim 6 based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foam
The preparation method of Raney nickel, which is characterized in that the nickel foam is having a size of 0.5*0.5cm2-2*2cm2Square；
Preferably, the molar concentration of the hydrochloric acid is 1mol/L, and the ultrasonic time in hydrochloric acid is 10min；The ultrasound of Yu Shuizhong
Time is 10min；Ultrasonic time in ethyl alcohol is 10min；Room temperature in vacuo drying time is 12h.
8. according to claim 3 based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foam
The preparation method of Raney nickel, which is characterized in that reaction temperature described in step (2) is 60 DEG C, reaction time 30s.
9. according to claim 3 based on ferric trichloride/urea eutectic solvent ferronickel double-metal hydroxide/foam
The preparation method of Raney nickel, which is characterized in that washing is respectively washed 3 times with second alcohol and water described in step (2)；The drying
It is to be dried in vacuo 12h at room temperature.
10. as claims 1 or 2 is described in any item based on ferric trichloride/urea eutectic solvent ferronickel bimetallic hydrogen-oxygen
Compound/foamed nickel catalyst agent application is applied to electro-catalysis electrolysis urea or electrolysis water.
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| CN113604834B (en) * | 2021-07-13 | 2022-09-27 | 武汉工程大学 | NiCo-LDH/(Ni, Fe) (OH) with core-shell structure 2 Foamed nickel composite electrode |
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| CN114988493A (en) * | 2022-04-27 | 2022-09-02 | 中国石油大学(华东) | Preparation method of ferronickel bimetal hydroxide, product and application thereof |
| CN115805077A (en) * | 2022-11-08 | 2023-03-17 | 无锡科技职业学院 | Preparation method of modified foamed nickel |
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