CN104888811A - Transition metal sulfide oxygen reduction catalyst and preparation method thereof - Google Patents
Transition metal sulfide oxygen reduction catalyst and preparation method thereof Download PDFInfo
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- CN104888811A CN104888811A CN201510264272.7A CN201510264272A CN104888811A CN 104888811 A CN104888811 A CN 104888811A CN 201510264272 A CN201510264272 A CN 201510264272A CN 104888811 A CN104888811 A CN 104888811A
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- oxygen reduction
- reduction catalyst
- catalyst
- metal sulfide
- agent
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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
- Y02E60/50—Fuel cells
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Abstract
The invention discloses a transition metal sulfide oxygen reduction catalyst which is presented as MSx, wherein M is Zn, Ni, Co, Fe, Cu or Mn, and x is more than or equal to 1.0 and less than or equal to 2.0. The transition metal sulfide oxygen reduction catalyst has the advantages of high efficiency, low cost, good stability, and easiness in industrial production.
Description
Technical field
The present invention relates to a kind of transient metal sulfide oxygen reduction catalyst agent and preparation method thereof.
Background technology
New energy development and environmental protection are the significant challenge that national economy sustainable development faces.Fuel cell and metal-air battery power generation process do not relate to oxyhydrogen combustion, and thus not by the restriction of Carnot cycle, energy conversion rate is high; Do not produce pollution during generating, power generating modules, reliability is high, noiselessness during work, assembling and easy to maintenance, is considered to future automobile power and the most promising electrochmical power source of other vehicles, is subject to people's extensive concern.Wherein, the redox reactions that fuel cell and metal-air battery negative electrode occur is because relate to multielectron transfer process, and kinetic rate is very slow, becomes the bottleneck restricting whole battery charging and discharging.At present in order to improve the efficiency of redox reactions on negative electrode, general use Pt/C catalyst.But on the earth, Pt reserves are rare, expensive, the commercialization seriously constraining fuel cell and metal-air battery uses.Therefore, developing the new catalyst of alternative Pt, improve catalyst to the catalytic activity of oxygen reduction and CO tolerance catalysts ability, reduce catalyst price, is emphasis and the focus of fuel cell and metal-air battery research.
The report of more existing oxygen reduction catalyst agent patents at present.(the application number: a kind of method 201310452053) reporting synthesis redox reactions eelctro-catalyst in enormous quantities such as the Wang Xiaojuan of Peking University, transition metal salt and containing n-donor ligand are mixed according to certain mol proportion, use ball-milling method dry grinding said mixture, after dry grinding, high-temperature calcination obtains oxygen reduction catalyst agent under anaerobic.The Ye Jianshan (publication number: CN 101745426A) of East China University of Science discloses compound oxygen reduction electro-catalyst of nitrogenous carbon nano materials modified by macrocyclic compound and preparation method thereof.This catalyst has good catalytic activity and stability.The oxygen reduction catalyst agent that Changzhou Institute of Advanced Material, Beijing University of Chemical Technology's silver Fengxiang etc. (publication number: CN 103035930A) disclose a kind of tool perovskite crystalline structure (is specially Ba
0.9co
0.7fe
0.2nb
0.1O3, La
0.6sr
0.4co
0.2fe
0.8O3, Pr
0.4sr
0.6co
0.2fe
0.7nb
0.1O3or Ba
0.5sr
0.5co
0.8fe
0.2O3), this catalyst application, in lithium-air battery, can effectively reduce battery cost.
In above-mentioned patent, some needs to use containing n-donor ligand or nitrogen-containing compound, and in the process of synthetic catalyst, in catalyst, the existence form of nitrogen and content are difficult to control, and this kind of catalyst stability is not high simultaneously.In addition, although perovskite type catalyst has good stability, they can only use under middle hot conditions, and catalytic performance is poor at low temperatures.The transition metal sulfide catalyst that this patent proposes can overcome the shortcoming of these catalyst in above-mentioned patent, not only has high stability, and has high catalytic activity at low temperatures, be suitable for automobile fuel battery or metal-air battery.
Summary of the invention
The object of this invention is to provide a kind of efficient, low cost, good stability, the transient metal sulfide oxygen reduction catalyst agent being easy to suitability for industrialized production and preparation method thereof.
Transient metal sulfide oxygen reduction catalyst of the present invention agent is expressed as MS
x(1.0≤x≤2.0) wherein M=Zn, Ni, Co, Fe, Cu or Mn.
The present invention obtains metal sulfide M S by anion exchange
x, different owing to relating to the species of metal ion coexisted in exchange process, the reason that reaction temperature is different with the time, cause state of cure (vulcanization) different, have-1, the sulphur of-divalent coexists.Therefore sulfide M S
xmiddle X value can change in 1.0-2.0 numerical value.
Specific embodiment of the invention step is as follows:
(1) stir soluble in water for soluble M slaine, obtain 0.4-10g/L metal salt solution;
(2) complexometric reagent, additive to be added successively in M metal salt solution and to stir;
(3) above-mentioned solution is moved on in reactor, be heated to 90-150 DEG C, reaction 2-5h, solid collected by filtration, and spend deionized water;
(4) by washing after solid dispersal in 0.1-0.4mol/L sulfide solution, in 70-90 DEG C, reaction 8-12h, filtration washing obtains catalyst powder.
Soluble M slaine as above is the one in nitrate, halide salt, acetate;
Complexometric reagent as above is the one of sodium fluoride, ammonium fluoride, sodium chloride, ammonium chloride;
Additive as above is the one in hexamethylenetetramine, urea, polyethylene glycol;
Sulfide as above is the one in potassium sulfide, vulcanized sodium, ammonium sulfide;
The present invention compared with prior art tool has the following advantages: the preparation method that the present invention proposes a kind of non-noble metal fuel-cell catalyst.This catalyst obtains a kind of transient metal sulfide by hydro-thermal method and anion exchange.This sulfide particles size is homogeneous, is evenly distributed, and shows good oxygen reduction activities.The preparation of this catalyst is easy, environmental protection, safety; Catalyst performance is good, stable, is easy to industrialization large-scale production; It is a catalyst having market application foreground.
Detailed description of the invention
Under normal temperature, oxygen reduction catalyst agent generally carries out linear scan test in the saturated KOH solution of oxygen, and by hydrogen reduction take-off potential, positive and negative and limiting current density size carrys out the active height of the catalytic reduction oxygen of evaluate catalysts.The take-off potential of best at present Pt/C catalyst (be 20% containing Pt) reduction oxygen is about-0.12V vs.Ag/AgCl, and limiting current density can reach 3.4mA/cm
2.The take-off potential of the catalyst reduction oxygen obtained by this patent method is-0.16--0.11V vs.Ag/AgCl, and limiting current density is 3.0-3.6mA/cm
2, show that this catalyst has the ability of good catalytic reduction oxygen, be expected to replace commercial Pt/C catalyst.Below in conjunction with embodiment, the present invention is described in detail, but the embodiment of the invention is not restricted to.
Embodiment 1
1, take 2.5g iron chloride to be dissolved in 500ml water, stir and obtain solution;
2, take 0.5g ammonium chloride, 1.3g urea, join successively in above-mentioned solution, stir;
3, gained solution is moved in hydrothermal reaction kettle, be heated to 110 DEG C, isothermal reaction 4h;
4, by product centrifugation, spend deionized water clean, be redispersed in the Na of 0.1mol/L
2in S solution, and move on to 70 DEG C of reaction 8h in reactor, it is FeS that filtration washing obtains catalyst powder
1.0;
5, using on above-mentioned for 5mg catalyst cupport to glass-carbon electrode as working electrode, take Ag/AgCl as reference electrode, Pt is to electrode, at O
2its chemical property is tested in saturated 1M KOH solution.Electrochemistry linear sweep test shows, take-off potential is-0.16V, and limiting current density is 3.0mA/cm
2.
Embodiment 2
1, take 1.2g cobalt acetate to be dissolved in 500ml water, stir and obtain solution;
2, take 0.5 ammonium fluoride, 1.5g six methine four ammonium, joins successively in above-mentioned solution, stirs;
3, gained solution is moved in hydrothermal reaction kettle, be heated to 130 DEG C, isothermal reaction 3h;
4, by product centrifugation, spend deionized water clean, be redispersed in the Na of 0.2mol/L
2in S solution, and move on to 80 DEG C of reaction 10h in reactor, it is CoS that filtration washing obtains catalyst powder
2.0;
5, using on above-mentioned for 5mg catalyst cupport to glass-carbon electrode as working electrode, take Ag/AgCl as reference electrode, Pt is to electrode, at O
2its chemical property is tested in saturated 1M KOH solution.Electrochemistry linear sweep test shows, take-off potential is-0.13V, and limiting current density is 3.4mA/cm
2.
Embodiment 3
1, take 0.2g nickel nitrate to be dissolved in 500ml water, stir and obtain solution;
2, take 0.5g ammonium fluoride, 1.25g urea joins in above-mentioned solution successively, stirs;
3, gained solution is moved in hydrothermal reaction kettle, be heated to 150 DEG C, isothermal reaction 2h;
4, by product centrifugation, spend deionized water clean, be redispersed in the Na of 0.3mol/L
2in S solution, and move on to 90 DEG C of reaction 8h in reactor, it is NiS that filtration washing obtains catalyst powder
1.7;
5, using on above-mentioned for 5mg catalyst cupport to glass-carbon electrode as working electrode, take Ag/AgCl as reference electrode, Pt is to electrode, at O
2its chemical property is tested in saturated 1M KOH solution.Electrochemistry linear sweep test shows, and take-off potential is-0.14V, and limiting current density is 3.3mA/cm
2.
Embodiment 4
1, take 1.6g cobalt acetate to be scattered in 500ml water, stir and obtain solution;
2, take 0.7g ammonium chloride, 1 gram of triethylenediamine joins in above-mentioned solution, stir;
3, gained solution is moved in hydrothermal reaction kettle, be heated to 90 DEG C, isothermal reaction 5h;
4, by product centrifugation, spend deionized water clean, be redispersed in the Na of 0.4mol/L
2in S solution, and move on to 90 DEG C of reaction 8h in reactor, it is CoS that filtration washing obtains catalyst powder
1.8;
5, using on above-mentioned for 5mg catalyst cupport to glass-carbon electrode as working electrode, take Ag/AgCl as reference electrode, Pt is to electrode, in the 1M KOH solution that O2 is saturated, test its chemical property.Electrochemistry linear sweep test shows, take-off potential is-0.11V, and limiting current density is 3.6mA/cm
2.
Embodiment 5
1, take 5g zinc acetate to be dissolved in 500ml water, stir and obtain solution;
2, take 0.6g ammonium nitrate, 1.2g six methine four ammonium, joins successively in above-mentioned solution, stirs;
3, gained solution is moved in hydrothermal reaction kettle, be heated to 130 DEG C, isothermal reaction 3h;
4, by product centrifugation, spend deionized water clean, be redispersed in the K of 0.2mol/L
2in S solution, and move on to 80 DEG C of reaction 10h in reactor, it is ZnS that filtration washing obtains catalyst powder
1.3;
5, using on above-mentioned for 5mg catalyst cupport to glass-carbon electrode as working electrode, take Ag/AgCl as reference electrode, Pt is to electrode, at O
2its chemical property is tested in saturated 1M KOH solution.Electrochemistry linear sweep test shows, take-off potential is-0.16V, and limiting current density is 3.0mA/cm
2.
Embodiment 6
1, take 0.8g manganese nitrate to be dissolved in 500ml water, stir and obtain solution;
2, take 0.4g ammonium chloride, 1.0g urea, join successively in above-mentioned solution, stir;
3, gained solution is moved in hydrothermal reaction kettle, be heated to 150 DEG C, isothermal reaction 2h;
4, by product centrifugation, spend deionized water clean, be redispersed in the K of 0.4mol/L
2in S solution, and move on to 70 DEG C of reaction 12h in reactor, it is MnS that filtration washing obtains catalyst powder
1.6;
5, using on above-mentioned for 5mg catalyst cupport to glass-carbon electrode as working electrode, take Ag/AgCl as reference electrode, Pt is to electrode, at O
2its chemical property is tested in saturated 1M KOH solution.Electrochemistry linear sweep test shows, take-off potential is-0.14V, and limiting current density is 3.2mA/cm
2.
Embodiment 7
1, take 2.5g copper acetate to be dissolved in 500ml water, stir and obtain solution;
2, take 0.8g ammonium chloride, 1.5g triethylenediamine, join successively in above-mentioned solution, stir;
3, gained solution is moved in hydrothermal reaction kettle, be heated to 90 DEG C, isothermal reaction 5h;
4, by product centrifugation, spend deionized water clean, be redispersed in the K of 0.1mol/L
2in S solution, and move on to 70 DEG C of reaction 12h in reactor, it is CuS that filtration washing obtains catalyst powder
1.6;
5, using on above-mentioned for 5mg catalyst cupport to glass-carbon electrode as working electrode, take Ag/AgCl as reference electrode, Pt is to electrode, in the 1M KOH solution that O2 is saturated, test its chemical property.Electrochemistry linear sweep test shows, take-off potential is-0.15V, and limiting current density is 3.1mA/cm
2.
Embodiment 8
1, take 3.4g ferric nitrate to be dissolved in 500ml water, stir and obtain solution;
2, take 0.6g ammonium fluoride, 1.1g six methine four ammonium, joins successively in above-mentioned solution, stirs;
3, gained solution is moved in hydrothermal reaction kettle, be heated to 110 DEG C, isothermal reaction 4h;
4, by product centrifugation, spend deionized water clean, be redispersed in the K2S solution of 0.3mol/L, and move on to 80 DEG C of reaction 10h in reactor, it is FeS that filtration washing obtains catalyst powder
1.9;
5, using on above-mentioned for 5mg catalyst cupport to glass-carbon electrode as working electrode, take Ag/AgCl as reference electrode, Pt is to electrode, at O
2its chemical property is tested in saturated 1M KOH solution.Electrochemistry linear sweep test shows, take-off potential is-0.14V, and limiting current density is 3.2mA/cm
2.
Claims (6)
1. a transient metal sulfide oxygen reduction catalyst agent, is characterized in that the agent of transient metal sulfide oxygen reduction catalyst is expressed as MS
x, wherein M=Zn, Ni, Co, Fe, Cu or Mn, 1.0≤x≤2.0.
2. the preparation method of a kind of transient metal sulfide oxygen reduction catalyst as claimed in claim 1 agent, is characterized in that comprising the steps:
(1) stir soluble in water for soluble M slaine, obtain 0.4-10 g/L metal salt solution;
(2) complexometric reagent, additive to be added successively in M metal salt solution and to stir;
(3) above-mentioned solution is moved on in reactor, be heated to 90-150
0c, reaction 2-5 h, solid collected by filtration, and spend deionized water;
(4) by washing after solid dispersal in 0.1-0.4 mol/L sulfide solution, in 70-90
oc, reaction 8-12h, filtration washing obtains catalyst powder.
3. the preparation method of a kind of transient metal sulfide oxygen reduction catalyst as claimed in claim 2 agent, is characterized in that described soluble M slaine is the one in nitrate, halide salt, acetate.
4. the preparation method of a kind of transient metal sulfide oxygen reduction catalyst as claimed in claim 2 agent, is characterized in that described complexometric reagent is the one of sodium fluoride, ammonium fluoride, sodium chloride, ammonium chloride.
5. the preparation method of a kind of transient metal sulfide oxygen reduction catalyst as claimed in claim 2 agent, is characterized in that described additive is the one in hexamethylenetetramine, urea, polyethylene glycol.
6. the preparation method of a kind of transient metal sulfide oxygen reduction catalyst as claimed in claim 2 agent, is characterized in that described sulfide is the one in potassium sulfide, vulcanized sodium, ammonium sulfide.
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Cited By (8)
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| CN109161924A (en) * | 2018-11-09 | 2019-01-08 | 天津工业大学 | A kind of Fe of bivalve layer2O3The preparation of/NiS nanocomposite |
| CN109161925A (en) * | 2018-11-09 | 2019-01-08 | 天津工业大学 | A kind of preparation and Hydrogen Evolution Performance research of 3D structure Zn-Co-S nanocomposite |
| CN109167074A (en) * | 2018-08-08 | 2019-01-08 | 东华大学 | The nitrogen-doped carbon nanocomposite of hollow additive Mn cobalt oxide nickel coated and preparation |
| CN113224330A (en) * | 2021-05-08 | 2021-08-06 | 上海交通大学 | Application of copper-based compound multifunctional catalyst in lithium air battery |
| CN113764631A (en) * | 2020-06-01 | 2021-12-07 | 南京航空航天大学 | FeS for sodium ion battery0.5Se0.5/CF composite negative electrode material and preparation method thereof |
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| CN105551812A (en) * | 2016-01-19 | 2016-05-04 | 南京理工大学 | NiCo2S4 supercapacitor material and preparation method therefor |
| CN105551812B (en) * | 2016-01-19 | 2018-07-31 | 南京理工大学 | A kind of NiCo2S4Super capacitor material and preparation method thereof |
| CN110383550A (en) * | 2017-03-24 | 2019-10-25 | 昭和电工株式会社 | Oxygen reduction catalyst, electrode, membrane-electrode assembly and fuel cell |
| WO2018174142A1 (en) * | 2017-03-24 | 2018-09-27 | 昭和電工株式会社 | Oxygen reduction catalyst, electrode, membrane electrode assembly, and fuel cell |
| JP6403933B1 (en) * | 2017-03-24 | 2018-10-10 | 昭和電工株式会社 | Oxygen reduction catalyst, electrode, membrane electrode assembly, and fuel cell |
| JP6403934B1 (en) * | 2017-03-24 | 2018-10-10 | 昭和電工株式会社 | Oxygen reduction catalyst, electrode, membrane electrode assembly, and fuel cell |
| WO2018174143A1 (en) * | 2017-03-24 | 2018-09-27 | 昭和電工株式会社 | Oxygen reduction catalyst, electrode, membrane electrode assembly, and fuel cell |
| CN110446549A (en) * | 2017-03-24 | 2019-11-12 | 昭和电工株式会社 | Oxygen reduction catalyst, electrode, membrane-electrode assembly and fuel cell |
| US10720649B2 (en) | 2017-03-24 | 2020-07-21 | Showa Denko K.K. | Oxygen reduction catalyst, electrode, membrane electrode assembly, and fuel cell |
| US10727514B2 (en) | 2017-03-24 | 2020-07-28 | Showa Denko K.K. | Oxygen reduction catalyst, electrode, membrane electrode assembly, and fuel cell |
| CN109167074A (en) * | 2018-08-08 | 2019-01-08 | 东华大学 | The nitrogen-doped carbon nanocomposite of hollow additive Mn cobalt oxide nickel coated and preparation |
| CN109161924A (en) * | 2018-11-09 | 2019-01-08 | 天津工业大学 | A kind of Fe of bivalve layer2O3The preparation of/NiS nanocomposite |
| CN109161925A (en) * | 2018-11-09 | 2019-01-08 | 天津工业大学 | A kind of preparation and Hydrogen Evolution Performance research of 3D structure Zn-Co-S nanocomposite |
| CN113764631A (en) * | 2020-06-01 | 2021-12-07 | 南京航空航天大学 | FeS for sodium ion battery0.5Se0.5/CF composite negative electrode material and preparation method thereof |
| CN113224330A (en) * | 2021-05-08 | 2021-08-06 | 上海交通大学 | Application of copper-based compound multifunctional catalyst in lithium air battery |
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Application publication date: 20150909 |