CN105609790B - A kind of preparation method of nickel cobalt/carbon nanotube aerogel zinc and air cell catalyst - Google Patents
A kind of preparation method of nickel cobalt/carbon nanotube aerogel zinc and air cell catalyst Download PDFInfo
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- CN105609790B CN105609790B CN201510943911.2A CN201510943911A CN105609790B CN 105609790 B CN105609790 B CN 105609790B CN 201510943911 A CN201510943911 A CN 201510943911A CN 105609790 B CN105609790 B CN 105609790B
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 42
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 23
- 239000011701 zinc Substances 0.000 title claims abstract description 23
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000004964 aerogel Substances 0.000 title claims abstract description 18
- 239000003054 catalyst Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 25
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000661 sodium alginate Substances 0.000 claims abstract description 24
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 24
- 230000001588 bifunctional effect Effects 0.000 claims abstract 4
- 239000000243 solution Substances 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 235000010443 alginic acid Nutrition 0.000 claims description 9
- 229920000615 alginic acid Polymers 0.000 claims description 9
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 8
- 229960001126 alginic acid Drugs 0.000 claims description 8
- 239000000783 alginic acid Substances 0.000 claims description 8
- 150000004781 alginic acids Chemical class 0.000 claims description 8
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 6
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 6
- 229910001453 nickel ion Inorganic materials 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 claims description 3
- VMWYVTOHEQQZHQ-UHFFFAOYSA-N methylidynenickel Chemical compound [Ni]#[C] VMWYVTOHEQQZHQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000005518 electrochemistry Effects 0.000 claims description 2
- 239000000017 hydrogel Substances 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims 2
- 238000001354 calcination Methods 0.000 claims 1
- 238000004108 freeze drying Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 abstract description 2
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 abstract 1
- ZCGHZHINDNSWEL-UHFFFAOYSA-N [C].[Co].[Ni] Chemical compound [C].[Co].[Ni] ZCGHZHINDNSWEL-UHFFFAOYSA-N 0.000 description 5
- 239000000499 gel Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 3
- 241001474374 Blennius Species 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- AEMOLEFTQBMNLQ-SYJWYVCOSA-N (2s,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-SYJWYVCOSA-N 0.000 description 1
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- GWBWGPRZOYDADH-UHFFFAOYSA-N [C].[Na] Chemical compound [C].[Na] GWBWGPRZOYDADH-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229940072056 alginate Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- XIKYYQJBTPYKSG-UHFFFAOYSA-N nickel Chemical compound [Ni].[Ni] XIKYYQJBTPYKSG-UHFFFAOYSA-N 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9008—Organic or organo-metallic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a kind of preparation methods of nickel cobalt/carbon nanotube aerogel zinc and air cell catalyst, are used for zinc-air battery field.The catalyst uses sodium alginate, cobalt chloride hexahydrate, Nickel dichloride hexahydrate and carbon nanotube for raw material, is successfully prepared out nanometer nickel-cobalt/carbon nanotube aerogel bifunctional catalyst of zinc and air cell.The bifunctional catalyst shows excellent oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) catalytic performance, and OER take-off potentials are early, and current density is big;Its ORR take-off potential is early, limiting current density is big, and stability is good;And zinc and air cell tests the front and back voltage difference that is charged and discharged of long circulating and changes small, the energy efficiency height after long circulating.Preparation method of the present invention is simple, swift to operate, environmentally protective, and sodium alginate abundance, and gained bifunctional catalyst is had excellent performance, and is very promising zinc and air cell catalyst.
Description
Technical field
The invention belongs to zinc and air cell fields, and in particular to a kind of nanometer nickel-cobalt/carbon nanotube aerogel zinc and air cell is urged
The preparation method of agent..
Background technology
Metal-air battery is considered a kind of novel, non-environmental-pollution energy conversion device, and its efficiency is apparent
Higher than traditional generator, and zinc-air battery shows good application prospect in recent years.But zinc-air battery will reach
The problems such as also needing to solve the cost and performance of ORR and OER catalyst to real commercial applications.Ruthenium, iridium and platinum group catalysis
Agent is the most common catalyst of cash, but the factors such as it is expensive, rare, stability is poor seriously limit zinc and air cell
Using and development.Therefore, develop a kind of novel, the zinc and air cell catalyst that derives from a wealth of sources for realizing the extensive of zinc and air cell
Using being a difficulty that must be captured.
Sodium alginate is extracted as a kind of marine biomass macromolecule from brown alga, resourceful, be by
Beta-D-mannuronic acid (abbreviation M) and α-L- guluronic acids (abbreviation G) are formed by 1-4 glucosides key connections, the difference of the two
For the difference of carboxyl site on C-5, the structural formula of two kinds of uronic acids is as shown in formula a.Solely there are one be characterized in when chance for alginate
Gel can be formed such as nickel ion and cobalt ions to bivalent metal ion, this gel structure is described as " Egg tray structure ", such as
Shown in formula b, many applications of sodium alginate are all based on this special property.
Specific surface area of carbon nanotube is big, electric conductivity is excellent, stable chemical performance, and has to catalyst granules very strong
Adhesive ability, these excellent performances are all conducive to the reaction in zinc and air cell, and therefore, carbon nanotube can be as one well
Carbon carrier.But carbon nanotube itself is there is also many shortcoming and defect, for example carbon nanotube is easy to tangle, and aeroge can be with
It solves these problems, because the three-dimensional structure of aeroge can effectively prevent the winding of carbon nanotube, to maintain its high ratio
Surface area and excellent performance, and then better catalytic action can be played to zinc and air cell.
Invention content
The present invention is prepared for having that very high OER and ORR is difunctional receives using the sodium alginate of abundance as raw material
Rice nickel cobalt/carbon nanotube aerogel.
Preparation process of the present invention is simple, does not need expensive device, products obtained therefrom quality high-performance is good, in zinc and air cell in future
Large-scale application in there is bright foreground.
A kind of preparation method of nanometer nickel-cobalt/carbon nanotube aerogel zinc and air cell catalyst, manufacturing process includes following
Step:
1) sodium alginate soln that 1~3wt% is prepared with secondary deionized water, stirs 4~6 hours, is uniformly mixed
Sodium alginate soln;
2) be added into above-mentioned sodium alginate soln carbon nanotube (sodium alginate and carbon nanotube mass ratio be about 25: 1~
2: 1), stirring 4~6 hours, obtain the uniformly mixed mixed liquor of sodium alginate and carbon nanotube;
3) the nickel cobalt mixed solution that mass fraction is 5wt%, the mixing secondary deionized water of nickel chloride and cobalt chloride are prepared
Solution (sodium alginate and nickel chloride/cobalt chloride mass ratio be 1: 5), stirring make it fully dissolve, wherein nickel and cobalt ions mole
Than being 1: 1 or 1: 2.
4) sodium alginate and the mixed liquor of carbon nanotube are instilled to be formed in above-mentioned nickel chloride and cobalt chloride mixed solution and is coagulated
Glue after the completion of instillation, stands 2 hours;
5) above-mentioned gel is separated, is used in combination secondary deionized water concussion cleaning multiple, until without free in cleaning solution
The presence of state nickel and cobalt ions after the completion of cleaning, puts it into freeze drier and is freeze-dried 12 hours formation aeroges;
6) above-mentioned aeroge is put into tube furnace and is calcined, calcined 1~2 hour for 700 DEG C in ammonia atmosphere, then in air
In 400 DEG C of oxidations obtain final product nanometer nickel-cobalt/carbon nanotube aerogel zinc and air cell catalyst within 1~2 hour;
7) OER the and ORR performances that above-mentioned product is tested with electrochemical workstation and rotating disk electrode (r.d.e) are test-manufactured with blue electrical measurement
The zinc and air cell performance of object.
The present invention has the following advantages:
The raw material that the present invention uses is mainly sodium alginate, and sodium alginate is extracted from seaweed, derive from a wealth of sources,
It is environment-friendly and green, safe.
Nanometer nickel-cobalt/carbon nanotube aerogel prepared by the method for the present invention has very high oxygen evolution reaction (OER) and oxygen also
Original reaction (ORR) performance, OER take-off potentials (1.43V vs RHE) are than the Ir/C of business in 1M KOH electrolyte
(1.485V vs RHE) is early, and current density reaches 10mA/cm2Corresponding voltage is that 1.465V ratio Ir/C 1.554V are early.
Its ORR wave inceptions potential (0.89V vs RHE), limiting current density (- 4.88mA/cm2), stability aspect
Current density reduces < 9% and stablizes than business Pt/C (current density reduces > 20%) after 21600s.
And it is that~1.95 and~1.20V fills respectively to be charged and discharged voltage in zinc and air cell test when current rate 5A/g
Electricity and electric discharge voltage difference be 0.75V, cycle 70 circle after charging and discharging voltage be respectively~1.94 and~1.14V charging and
The voltage difference of electric discharge is 0.8V, and the energy efficiency after long circulating is 58.5%.
Nanometer nickel-cobalt/carbon nanotube aerogel prepared by the method for the present invention can be synthesized largely, not need expensive device, can be wide
It is general to be used in zinc and air cell.
Description of the drawings
Fig. 1 is nanometer nickel-cobalt/carbon nanotube aerogel XRD and TEM figure that specific embodiment 1,2 obtains.
Fig. 2 is the catalytic performance characterization that specific embodiment 1,2 obtains nanometer nickel-cobalt/carbon nanotube aerogel
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment one
0.404g sodium alginates are dissolved in 40g secondary deionized water solution, are stirred 6 hours, are obtained uniformly mixed 1wt%
Sodium alginate soln, be denoted as solution 1.0.0161g carbon nanotubes are mixed into the sodium alginate soln of above-mentioned preparation, stirring 6
Hour, the mixed solution of sodium alginate carbon nanotube is obtained, solution 2 is denoted as.1.3g Nickel dichloride hexahydrates and 1.3g six are hydrated
Cobalt chloride is dissolved in 50g secondary deionized water solution, obtains nickel chloride and cobalt chloride mixed solution, is denoted as solution 3.By solution 2
It instills in nickel chloride and cobalt chloride mixed solution in ie in solution 3, forms the hydrogel of alginic acid nickel cobalt carbon nanotube, instill and complete
Afterwards, 2 hours are stood.Alginic acid nickel cobalt carbon nanotube gel obtained above is separated, secondary deionized water is used in combination to clean,
Until by solution without free state nickel and cobalt ions.It is dry that the alginic acid nickel cobalt carbon nanotube gel obtained after cleaning is put into freezing
It is freeze-dried 12 hours in dry machine, obtains alginic acid nickel cobalt carbon nanotube aerogel.By alginic acid nickel cobalt carbon nanotube aerogel
It is put into tube furnace and is carbonized, calcined 1 hour for 700 DEG C in ammonia atmosphere;400 DEG C of oxidations obtain for 1 hour in air again
Nanometer nickel nickel/cobalt acid nickel carbon nanotube aerogel catalyst.By above-mentioned obtained final product nano nickel/oxidation
Nickel cobalt acid nickel carbon nanotube aeroge zinc and air cell catalyst is carried out using electrochemical workstation, rotating disk electrode (r.d.e) and blue electricity
Electrochemistry and zinc and air cell test.
Embodiment two
In addition to 0.1616g carbon nanotubes to be mixed into the sodium alginate soln of above-mentioned preparation, stirs 6 hours, obtain seaweed
The mixed solution of sour sodium carbon nanotube, is denoted as solution 2.Remaining step is identical with embodiment 1.
Claims (7)
1. a kind of preparation method of nickel cobalt/carbon nanotube aerogel zinc and air cell catalyst, it is characterised in that the method includes
Following steps:
1) sodium alginate secondary deionized water solution is prepared, a certain amount of carbon nanotube is added in the solution, and is stirred equal
It is even, obtain the mixed solution of sodium alginate carbon nanotube;
2) above-mentioned mixed solution is added dropwise in the secondary deionized water solution that cobalt chloride and nickel chloride mix, forms alginic acid nickel
Cobalt/carbon nanotube hydrogel, is separated, and is cleaned up to no free state nickel ion and cobalt ions presence with secondary deionized water,
Then it puts it into freeze-drying in freeze drier and obtains alginic acid nickel cobalt/carbon nanotube aerogel;
3) alginic acid nickel cobalt/carbon nanotube aerogel in tube furnace through certain carbonization and oxidation technology calcining, obtain nano nickel/
Aoxidize nickel cobalt acid nickel carbon nanotube aeroge bifunctional catalyst;
4) with electrochemical workstation, the electrochemistry and zinc of rotating disk electrode (r.d.e), rotating ring disk electrode (r.r.d.e) and the above-mentioned product of blue electrical testing
Empty battery performance.
2. preparation method according to claim 1, which is characterized in that the concentration of sodium alginate soln described in step 1)
For 1~3wt%.
3. preparation method according to claim 1, which is characterized in that the mixing time described in step 1) is 4~6h.
4. preparation method according to claim 1, which is characterized in that the sodium alginate described in step 1) and carbon nanotube
Mixed solution in sodium alginate and the mass ratio of carbon nanotube be 25: 1~2: 1.
5. preparation method according to claim 1, which is characterized in that sodium alginate and nickel chloride described in step 2)/
Cobalt chloride mass ratio is 1: 5.
6. preparation method according to claim 1, which is characterized in that the nickel chloride described in step 2) and cobalt chloride mixing
Secondary deionized water liquid quality fraction is 5wt%, and wherein nickel and cobalt ions molar ratio are 1: 1 or 1: 2.
7. preparation method according to claim 1, which is characterized in that the carbonization technique described in step 3) is in ammonia atmosphere
It is calcined 1~2 hour for 700 DEG C in enclosing;Oxidation technology is to be calcined 1~2 hour for 400 DEG C in air atmosphere.
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CN104174372A (en) * | 2014-08-22 | 2014-12-03 | 韩嘉欣 | Method for preparing sodium alginate-carbon nanotube gel and method for removing phosphorus in water |
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