CN109161924A - A kind of Fe of bivalve layer2O3The preparation of/NiS nanocomposite - Google Patents
A kind of Fe of bivalve layer2O3The preparation of/NiS nanocomposite Download PDFInfo
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- CN109161924A CN109161924A CN201811336599.0A CN201811336599A CN109161924A CN 109161924 A CN109161924 A CN 109161924A CN 201811336599 A CN201811336599 A CN 201811336599A CN 109161924 A CN109161924 A CN 109161924A
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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
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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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- 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
Abstract
The invention discloses a kind of Fe of bivalve layer2O3The preparation of/NiS nanocomposite, specific step include: to prepare Fe using solvent-thermal method first using iron chloride as molysite2O3Nanoparticle；Then with Fe2O3For carrier, nickel salt metal salt prepares Fe using hydro-thermal method2O3@Ni(OH)2Then core-shell material prepares the Fe of bivalve layer using vulcanized sodium as sulphur source hydro-thermal method2O3/ NiS nanocomposite.Preparation method is simple, easy to operate, with good performance in terms of Hydrogen Evolution Performance.
Description
Technical field
The present invention relates to a kind of Fe of bivalve layer2O3The preparation of/NiS nanocomposite, and in particular to pervasive using three steps
Hydro-thermal method prepares Fe2O3/ NiS nanocomposite.
Background technique
With a large amount of uses of limited fossil fuel, energy crisis and environmental pollution increasingly sharpen, renewable energy and each
The exploitation of kind of new energy has been subjected to the great attention of every country, and ideal green of the Hydrogen Energy as future substitute fossil fuels
One of energy has the advantages that abundance, renewable and storable, is considered as ideal energy carrier.However although
Protium is the most abundant element of content on the earth, but is not with free H2Molecular forms exist, therefore develop effectively and
Sustainable hydrogen producing technology is the important research content for pushing Hydrogen Energy development.The electrolysis water liberation of hydrogen in current numerous hydrogen producing technology
Reaction (HER) has great value for solving energy crisis and environmental problem.During water electrolysis hydrogen production, hydrogen is obtained
Key reaction is exactly evolving hydrogen reaction, since the development of evolving hydrogen reaction is largely influenced by its catalyst performance, so
The development of liberation of hydrogen approximate can also regard the development of liberation of hydrogen catalyst as.The most effective catalyst of evolving hydrogen reaction is noble metal at present
Platinum, but expensive price and poor stability make it cannot function as the water electrolysis hydrogen production of large-scale industrial production catalysis material
Material, thus develop abundance and cheap high activated catalyst be still one challenge.In recent years, researcher exists always
The electrocatalysis characteristic of transient metal sulfide is studied, these including but not limited to following materials: molybdenum disulfide (MoS2), curing
Iron (FeS2), cobalt disulfide (CoS2) and curing nickel (NiS2).The synthesis of nano material risen in recent years simultaneously also allows research
Personnel have found new direction, and nano structural material has bigger specific surface area and higher surface-active site density, lead to
It crosses the HER catalyst that nano materials obtain and shows higher catalytic activity, the research about nano material will pole
The big development for promoting liberation of hydrogen catalyst.Patent CN106328930A discloses a kind of high capacity file ion battery cathode material.a-
Fe2O3Preparation method, its step are as follows: (1) by FeCl3Solution and ethylene glycol are stirred at room temperature, and uniformly mix, obtain molten
Liquid A；(2) NaOH solution and deionized water are added in solution A, stirring obtains solution B；(3) dodecane is added in solution B
Base benzene sulfonic acid sodium salt, obtains solution C；(4) solution C is transferred in autoclave, reacts 20- under conditions of 200-250 DEG C, 5-6MPa
30h, by products therefrom FeOOH centrifuge separation, vacuum drying, heat treatment obtains cathode material for high capacity lithium ion battery a-
Fe2O3.Patent CN107746081A discloses a kind of two-dimensional nano piece form.a--Fe2O3The preparation method of material, the preparation side
Method is placed in Iron(III) chloride hexahydrate in aluminium oxide mandarin orange pot, is then placed in the tube furnace equipped with alundum tube, after sealed
It is passed through inert gas, and is warming up to 380-450 DEG C under protecting under an inert gas, is kept for 8-24 hours, is then cooled to room temperature,
Again after deionized water washing, dry, two-dimensional nano piece form a-Fe is obtained2O3Material.Compared with prior art, the present invention uses
Iron(III) chloride hexahydrate reagent thermally decomposes oxidation reaction preparation two-dimensional nano piece form a-Fe under inert atmosphere protection2O3Material,
Used reagent price is cheap, and preparation process is easier, it can be achieved that prepare with scale, and obtained di-iron trioxide pattern is
Two-dimensional nano piece.Patent CN106953093A utilizes colloid core-shell structure a-Fe the invention discloses a kind of2O3Material prepare lithium from
The method of sub- galvanic anode belongs to the preparation technical field of anode of lithium ion battery.Technical solution of the present invention main points are as follows: with sweet
Propylhomoserin prepares colloid core-shell structure a-Fe as structure directing agent, using water, alcohol mixed solvent thermal method2O3Material；It will be active
Substance a-Fe2O3Material, acetylene black and Kynoar are uniformly mixed, and are added N monomethyl and are adjoined pyrrolidone and are modulated into slurry, are made
Slurry is uniformly laid on copper foil with film instrument, in 120 DEG C of vacuum drying 12h, slice obtains anode of lithium ion battery.The present invention
Anode of lithium ion battery obtained has the characteristics that specific capacity is big, nontoxic, from a wealth of sources and low in cost, therefore has important
Potential practical value.Patent CN105329951A discloses a kind of a-Fe2O3The preparation method of nanotube.Preparation includes following step
It is rapid: (1) will be with NH4、H2P4And FeCl3Mixed aqueous solution be sufficiently stirred；Hydro-thermal process 48h at (2) 220 DEG C, after reaction
By precipitation and centrifugal separation；(3) it is successively cleaned with deionized water, ethyl alcohol；(4) it is dried in vacuo at 80 DEG C to get a-Fe is arrived2O3It is single
Brilliant nanotube.A kind of a-Fe of the present invention2O3The product that the preparation method of nanotube is prepared has one-dimentional structure form, height
Specific surface area, incident photon-to-electron conversion efficiency with higher and photocatalysis performance.Patent CN105289692A discloses a kind of g-C3N4/
Fe2O3Composite material and preparation method and application belong to material preparation and energetic material field.The composite material is by quality
Than the g-C for 95: 5-50: 503N4And nanometer Fe2O3It is combined, preparation step is as follows: by nanometer Fe2O3It is placed in ethanol solution
Middle ultrasonic disperse, is then added g-C3N4Continue ultrasonic disperse, is stirred continuously in ultrasonic procedure, it is slow in the agate mortar after the completion
Slowly it is ground to object and is put into vacuum drying oven in the pasty state and dry, obtain g-C in tubular type kiln roasting3N4/Fe2O3Composite material.This hair
The bright g-C prepared3N4/Fe2O3Composite material shows good catalytic effect to the thermal decomposition of ammonium perchlorate (AP), widens
The application field of graphite phase carbon nitride；Preparation process of the invention is simple, and time-consuming short, preparation efficiency is high, is suitble to industrialization big
Large-scale production has broad application prospects in energetic material field.
In the above patent, most of patent prepares Fe using various methods2O3And its compound, it has no and utilizes pervasive hydro-thermal
Method prepares Fe2O3The core-shell material of@NiS.
Summary of the invention
Provided technical solution is to realize the present invention:
(1) FeCl of certain mass is accurately weighed3.6H2O is dissolved in 48ml ethyl alcohol, and magnetic agitation 30min shifts solution
Into reaction kettle, 120~180 DEG C of reaction 4h are cooled to room temperature, and are separated by solid-liquid separation, are washed with deionized water repeatedly to neutrality, and 60 DEG C true
The dry 12h of sky, obtains Fe2O3；
(2) the product Fe of precise step (1)2O3And NiCl2·6H2O, mass ratio 2: 1~1: 4 are added 50ml and go
Ionized water, magnetic agitation 30min, then the urea and amine fluoride of certain mass are weighed, continue to stir 15min, then turns solution
It moves on in reaction kettle, 120~200 DEG C of reaction 5h wait its cooled to room temperature, are separated by solid-liquid separation, are washed with deionized water repeatedly
To neutrality, temperature is 60 DEG C of dry 12h, obtains predecessor；
(3) Na of 0.1~1mol/L of 50ml is accurately configured2S aqueous solution is put into reaction kettle, by the predecessor of step (2)
It is put into Na2In S aqueous solution, then reaction kettle is put into baking oven, temperature setting is 100-180 DEG C, 2-10h is reacted respectively,
It waits reaction kettle to be cooled to room temperature, is separated by solid-liquid separation, and washed repeatedly with deionized water, 60 DEG C of dry 12h, obtain in vacuum oven
To the Fe of final product bivalve layer2O3@NiS nanocomposite.
To be best understood from the present invention, the present invention will be described in further detail with reference to the following examples, but of the invention
Claimed range is not limited to the range of embodiment expression.
Embodiment 1:
(1) FeCl of certain mass is accurately weighed3.6H2O is dissolved in 48ml ethyl alcohol, and magnetic agitation 30min shifts solution
Into reaction kettle, 140 DEG C of reaction 4h are cooled to room temperature, and are separated by solid-liquid separation, are washed with deionized water repeatedly to neutrality, and 60 DEG C of vacuum are dry
Dry 12h, obtains Fe2O3；
(2) the product Fe of precise step (1)2O3And NiCl2·6H250ml deionization is added in O, mass ratio 1: 1
Water, magnetic agitation 30min, then the urea and amine fluoride of certain mass are weighed, continue to stir 15min, then transfer the solution into
In reaction kettle, 120 DEG C of reaction 5h wait its cooled to room temperature, are separated by solid-liquid separation, and are washed with deionized water repeatedly to neutrality, temperature
Degree is 60 DEG C of dry 12h, obtains predecessor；
(3) Na of the 0.1mol/L of 50ml is accurately configured2S aqueous solution is put into reaction kettle, and the predecessor of step (2) is put into
To Na2In S aqueous solution, then reaction kettle is put into baking oven, temperature setting is 120 DEG C, reacts 6h respectively, waits reaction kettle cold
But it to room temperature, is separated by solid-liquid separation, and is washed repeatedly with deionized water, 60 DEG C of dry 12h in vacuum oven, it is double to obtain final product
The Fe of shell2O3@NiS nanocomposite.
Embodiment 2: Fe in (2) is changed the step2O3And NiCl2·6H2The mass ratio of O is 1: 2, the same embodiment of other steps
1 to get bivalve layer Fe2O3@NiS nanocomposite.
Embodiment 3: Fe in (2) is changed the step2O3And NiCl2·6H2The mass ratio of O is 1: 3, the same embodiment of other steps
1 to get bivalve layer Fe2O3@NiS nanocomposite.
Embodiment 4: Na in (3) is changed the step2The concentration of S is 0.5mol/L's, other steps are with embodiment 1 to get double
The Fe of shell2O3@NiS nanocomposite.
Claims (1)
1. a kind of Fe of bivalve layer2O3The preparation of/NiS nanocomposite, the specific steps are as follows:
(1) FeCl of certain mass is accurately weighed3.6H2O is dissolved in 48ml ethyl alcohol, and solution is transferred to instead by magnetic agitation 30min
It answers in kettle, 120~180 DEG C of reaction 4h are cooled to room temperature, and are separated by solid-liquid separation, are washed with deionized water repeatedly to neutrality, and 60 DEG C of vacuum are dry
Dry 12h, obtains Fe2O3；
(2) the product Fe of precise step (1)2O3And NiCl2·6H250ml deionization is added in O, mass ratio 2: 1~1: 4
Water, magnetic agitation 30min add the urea and amine fluoride of certain mass, continue to stir 15min, then transfer the solution into
In reaction kettle, 120~200 DEG C of reaction 5h wait its cooled to room temperature, are separated by solid-liquid separation, are washed with deionized water repeatedly into
Property, temperature is 60 DEG C of dry 12h, obtains predecessor；
(3) Na of 0.1~1mol/L of 50ml is accurately configured2S aqueous solution is put into reaction kettle, and the predecessor of step (2) is put into
Na2In S aqueous solution, then reaction kettle is put into baking oven, temperature setting is 100~180 DEG C, reacts 2~10h respectively, is waited
Reaction kettle is cooled to room temperature, and is separated by solid-liquid separation, and washed repeatedly with deionized water, 60 DEG C of dry 12h, obtain most in vacuum oven
The Fe of final product bivalve layer2O3@NiS nanocomposite.
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Cited By (4)
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| CN109794264A (en) * | 2019-02-02 | 2019-05-24 | 河北工业大学 | A kind of micron of flower ball-shaped high-performance complete solution water bifunctional electrocatalyst FeOOH/Ni3S2Preparation method |
| CN110694646A (en) * | 2019-10-22 | 2020-01-17 | 上海交通大学 | Bimetallic sulfide composite electrocatalyst and preparation method and application thereof |
| CN112547107A (en) * | 2020-12-04 | 2021-03-26 | 江南大学 | alpha-Fe2O3/Ni@2D g-C3N4Process for preparing catalyst |
| CN113046765A (en) * | 2021-03-22 | 2021-06-29 | 南京大学 | Foamed nickel loaded Fe2O3@Ni3S2Preparation method of OER (organic electroluminescent) electrocatalyst with composite structure |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109794264A (en) * | 2019-02-02 | 2019-05-24 | 河北工业大学 | A kind of micron of flower ball-shaped high-performance complete solution water bifunctional electrocatalyst FeOOH/Ni3S2Preparation method |
| CN109794264B (en) * | 2019-02-02 | 2022-02-08 | 河北工业大学 | Micro-popcorn-shaped high-performance full-hydrolysis bifunctional electrocatalyst FeOOH/Ni3S2Preparation method of (1) |
| CN110694646A (en) * | 2019-10-22 | 2020-01-17 | 上海交通大学 | Bimetallic sulfide composite electrocatalyst and preparation method and application thereof |
| CN112547107A (en) * | 2020-12-04 | 2021-03-26 | 江南大学 | alpha-Fe2O3/Ni@2D g-C3N4Process for preparing catalyst |
| CN113046765A (en) * | 2021-03-22 | 2021-06-29 | 南京大学 | Foamed nickel loaded Fe2O3@Ni3S2Preparation method of OER (organic electroluminescent) electrocatalyst with composite structure |
| CN113046765B (en) * | 2021-03-22 | 2022-07-12 | 南京大学 | Foamed nickel loaded Fe2O3@Ni3S2Preparation method of OER (organic electroluminescent) electrocatalyst with composite structure |
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