CN105177621A - Molybdenum-oxygen cluster modified hollow microspherical nickel disulfide catalyst and application thereof - Google Patents
Molybdenum-oxygen cluster modified hollow microspherical nickel disulfide catalyst and application thereof Download PDFInfo
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- CN105177621A CN105177621A CN201510701910.7A CN201510701910A CN105177621A CN 105177621 A CN105177621 A CN 105177621A CN 201510701910 A CN201510701910 A CN 201510701910A CN 105177621 A CN105177621 A CN 105177621A
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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 invention discloses a molybdenum-oxygen cluster modified hollow microspherical nickel disulfide catalyst and application thereof to the aspect of producing hydrogen and oxygen through electric catalytic cracking of water, belonging to the technical field of electric catalytic cracking of water. A target material can be obtained through carrying out one-step hydrothermal reaction on raw materials including a surfactant, a sulfur source, a molybdenum source and a metal nickel substrate. The preparation method is simple and controllable, the raw materials are cheap, the sample property repeatability is good, the time consumed in the synthesis process is short, the requirement for equipment is not high, and the molybdenum-oxygen cluster modified hollow microspherical nickel disulfide catalyst is suitable for large-scale production. Particularly, the material can be simultaneously subjected to water electrolysis in an alkaline electrolysis tank to generate hydrogen and oxygen (namely fully-hydrolyzed water), has the current density of 10mA/cm<2> when the voltage is 1.45V, has higher activity than fully-hydrolyzed water of precious metal platinum and ruthenium oxide, is one of best double-surface catalysts at present, can greatly increase the electric energy to chemical energy conversion efficiency and meets the national requirements for saving energy and reducing emission.
Description
Technical field
The invention belongs to electrocatalysis splitting water technical field, be specifically related to a kind of molybdenum oxygen bunch curing three nickel micrometre hollow sphere catalyzer modified and the application in electrocatalysis cracking aquatic products hydrogen and product oxygen thereof.
Background technology
Along with socioeconomic development, people depend on fossil fuel energy unduly, exacerbate environmental pollution and Global warming, and fossil oil face exhaustion, so it is extremely urgent to find a kind of alternative green energy resource, and Hydrogen Energy becomes only choosing.The electric energy conversion that can not store be transformed by sun power, wind energy and water energy etc. can be Hydrogen Energy by electrocatalysis splitting water, and the hydrogen as carrier both may be used for storing energy, also can directly as important industrial chemicals.But, need to overcome larger overpotential in the process of actual brine electrolysis, cause energy utilization rate significantly to decline, and active catalyst effectively can reduce the overpotential of brine electrolysis, thus improve the utilization ratio of electric energy.At present, the precious metal of platinum, palladium class and iridium, rhodium base oxide are the most effective electrocatalysis cracking aquatic products hydrogen respectively and produce oxygen catalyst, but the shortcoming that it is expensive, reserves are extremely low seriously have impact on the widespread use of such material, therefore, the non-precious metal catalyst of exploitation high reactivity, earth's crust rich reserves causes extensively barring up of people.
In recent years, occurred more highly active base metal electrochemical cleavage water catalyzer, such as, hydrogen catalyst molybdenumdisulphide (J.Am.Chem.Soc.2005 127 volume 5308 pages) is produced in efficient water-splitting; And oxygen catalyst phosphatization cobalt (Science2008 32 volume 1072 pages) is produced in water-splitting.Although most eelctro-catalyst shows excellent catalytic property under strong acid or basic conditions, but produce hydrogen end due to their and can not mate completely with the working conditions of the best of product oxygen end, can not use in same electrolyzer.Therefore, synthesize and can be used for producing two-sided eelctro-catalyst that hydrogen can be used for again producing oxygen to remain a huge challenge under identical working conditions.
Summary of the invention
The present invention, to improve for the purpose of the efficiency of energy utilization that electric energy conversion is chemical energy, proposes the molybdenum oxygen bunch curing three nickel micrometre hollow sphere catalyzer modified and the application in electrocatalysis cracking aquatic products hydrogen and product oxygen thereof.
A kind of molybdenum oxygen of the present invention bunch curing three nickel micrometre hollow sphere catalyzer modified, it is characterized in that: be by soluble in water to tensio-active agent, sulphur source and molybdenum source, gained solution is loaded reactor, then adds metallic nickel substrate, prepare after reacting by heating 12h ~ 24h.
Described tensio-active agent is water-soluble triblock copolymer, includes but not limited to P123, F127 etc. and composition thereof.
Described sulphur source includes but not limited to thiocarbamide, thioacetamide and derivative thereof or its mixture.
Described molybdenum source is water-soluble molybdenum salt, includes but not limited to ammonium molybdate, Sodium orthomolybdate, four thio ammonium molybdate and composition thereof.
Described metallic nickel substrate includes but not limited to the metallic nickel materials such as nickel foam, nickel screen and nickel foil.
In described sulphur source and molybdenum source, the mol ratio of element sulphur and molybdenum element is 2.4 ~ 14.4:1; The mol ratio of element sulphur and tensio-active agent is 17.4 ~ 34.9:1, and Heating temperature is 160 ~ 220 DEG C.
The prepared molybdenum oxygen bunch curing three nickel micrometre hollow sphere catalyzer modified both as the negative pole of electrocatalysis cracking aquatic products hydrogen, can may be used for again the positive pole of electrocatalysis cracking aquatic products oxygen, was a kind of bifunctional water-splitting catalyzer.
Beneficial effect
The present invention contrasts prior art and has following innovative point:
1. synthesis material is cheap, and synthesis temperature is low, and synthesis step is simple, and controllability is high, properties of samples favorable reproducibility.
2. micrometre hollow sphere (diameter is for the 500nm ~ 1 μm) fractions distribution all constructed with ultra-thin (thickness is about 1.3nm) nanometer sheet of curing three nickel modified of gained molybdenum oxygen bunch is in metallic nickel substrate, the micrometre hollow sphere that this length is constructed at the suprabasil ultrathin nanometer sheet of metallic nickel, greatly improves electrochemical catalysis area and the mass-transfer efficiency of resulting materials.
3. resulting materials is a kind of novel electrocatalysis water-splitting catalyzer, excellent catalytic activity and stability is all shown in full pH value range (0 ~ 14), (pH is 14) electrolysis aquatic products hydrogen produces oxygen respectively when overpotential is 106mV and 136mV in the basic conditions, and current density can reach 10mA/cm
2, and stable performance.When voltage is 1.45V, current density just can reach 10mA/cm
2, be one of best at present two-sided electrocatalysis water-splitting catalyzer.
4. resulting materials is without the need to binding agent, directly can carry out water-splitting as working electrode, improve the electron transfer rate of eelctro-catalyst, reduce electric energy loss, improve the efficiency of energy utilization converting electrical energy into chemical energy.
Accompanying drawing explanation
Fig. 1: the XRD spectra of molybdenum oxygen bunch curing three nickel catalyzator modified obtained in embodiment 1;
Fig. 2: the Raman spectrogram of molybdenum oxygen bunch curing three nickel catalyzator modified obtained in embodiment 1;
Fig. 3: the SEM picture of molybdenum oxygen bunch curing three nickel catalyzator modified obtained in embodiment 1;
Fig. 4: (pH is 0 to molybdenum oxygen bunch curing three nickel catalyzator modified obtained in embodiment 1 in acidity, figure A), it is neutral that (pH is 7, figure B), alkalescence (pH is 14, figure C) electrocatalysis splitting water (deionized water) H2-producing capacity in electrolytic solution, namely current density is with relative to reversible hydrogen electrode potential change curve;
Fig. 5: (pH is 0 to molybdenum oxygen bunch curing three nickel catalyzator modified obtained in embodiment 1 in acidity, figure A), it is neutral that (pH is 7, figure B), alkalescence (pH is 14, figure C) gained catalytic stability curve in electrolytic solution, namely, under constant voltage, current density is change curve in time;
Fig. 6: the electrocatalysis splitting water (deionized water) of molybdenum oxygen bunch curing three nickel catalyzator modified in alkalescence (pH is 14) electrolytic solution obtained in embodiment 1 produces polarization curve (figure A) and the catalytic stability curve (figure B) of oxygen;
Fig. 7: curing three nickel catalyzator that the molybdenum oxygen bunch obtained in embodiment 1 is modified in alkaline electrolytic bath as the polarization curve (figure A) of two-sided eelctro-catalyst brine electrolysis and beta stability line (scheming B).
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The P123 of 10mg ammonium molybdate, 45mg thioacetamide and 0.15g is dissolved in 30mL deionized water, adds in 60mL reactor, then put into nickel foam (thickness 1.5mm, volume density 0.23mg/cm
3), 200 DEG C of reaction 24h can obtain the molybdenum oxygen bunch curing three nickel micrometre hollow sphere catalyzer modified.
Some structural characterizations have been carried out to catalyzer prepared by aforesaid method.Fig. 1 by the XRD spectra of acquisition catalyzer, go out peak position in this spectrogram consistent with PDF#44-1418, show that this catalyzer is the Ni of six sides
3s
2; Fig. 2 by the Raman spectrogram of acquisition catalyzer, can find out that gained catalyzer is MoO
xthe Ni modified
3s
2; Fig. 3, by being obtained catalyst S EM photo, can find out that this catalyzer is the micrometre hollow sphere of ultrathin nanometer sheet composition.
Electrocatalysis cracking aquatic products hydrogen product oxygen property detection is carried out in standard three-electrode cell to catalyzer prepared by aforesaid method; In electrolyzer, working electrode is the molybdenum oxygen prepared of the present invention bunch curing three nickel catalyzator modified, reference electrode is saturated calomel electrode, be carbon-point to electrode.It should be noted that, in electrocatalysis test, all electromotive forces with saturated calomel electrode being reference electrode obtains all are converted to reversible hydrogen electrode electromotive force in character figure.And the complete solution water in alkaline electrolytic bath is tested under two electrode conditions, molybdenum oxygen bunch curing three nickel catalyzator modified of synthesis is respectively as electrolysis aquatic products hydrogen end and produce oxygen end.
For this catalyzer, in acidity, (pH is 0,0.5MH to Fig. 4
2sO
4), it is neutral that (pH is 7,1MK
2hPO
4with 1MKH
2pO
4by corresponding proportion mixing), gained electrocatalysis cracking aquatic products hydrogen and produce oxygen character figure in alkalescence (pH is 14,1MKOH) electrolytic solution, can find out:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 123mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 192mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 106mV, this catalyzer current density reaches 10mA/cm
2;
The above results shows that this catalyzer all has excellent electrocatalysis and produces hydrogen activity in full pH value range.
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 136mV, this catalyzer current density reaches 10mA/cm
2.
Fig. 5 is this catalyzer gained electrolysis aquatic products hydrogen and alkalescence product oxygen catalytic stability character figure in acid (pH is 0), neutral (pH is 7), alkalescence (pH is 14) electrolytic solution, and added overpotential is respectively 0.12V, 0.19V, 0.11V, 0.15V; Can find out, (10 ~ 20mA/cm under larger current density conditions
2), material is through long-time (200 hours) work, and its catalytic performance keeps stable.
Fig. 6 is character and the stability of the electrocatalysis water-splitting of complete solution water in this catalyzer alkalescence (pH is 14,1MKOH) electrolyzer, can find out:
Under pH is 14 conditions, after composition electrolyzer, when institute's making alive is 1.45V, this catalyzer current density reaches 10mA/cm
2, and through long-time (100 hours) work, its catalytic performance is without any change.
Embodiment 2
Identical with embodiment 1, be just 60mg by the quantitative change of ammonium molybdate.The electrocatalysis characteristic of gained catalyzer:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 153mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 182mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 126mV, this catalyzer current density reaches 10mA/cm
2;
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 143mV, this catalyzer current density reaches 10mA/cm
2;
After composition electrolyzer;
Under pH is 14 conditions, when institute's making alive is 1.51V, this catalyzer current density reaches 10mA/cm
2.
Embodiment 3
Identical with embodiment 1, just temperature of reaction becomes 160 DEG C.The electrocatalysis characteristic of gained sample:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 158mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 190mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 140mV, this catalyzer current density reaches 10mA/cm
2;
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 155mV, this catalyzer current density reaches 10mA/cm
2;
After composition electrolyzer:
Under pH is 14 conditions, when institute's making alive is 1.53V, this catalyzer current density reaches 10mA/cm
2.
Embodiment 4
Identical with embodiment 1, just the consumption of tensio-active agent is become 0.3g.The electrocatalysis characteristic of gained sample:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 160mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 188mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 156mV, this catalyzer current density reaches 10mA/cm
2;
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 162mV, this catalyzer current density reaches 10mA/cm
2;
After composition electrolyzer:
Under pH is 14 conditions, when institute's making alive is 1.55V, this catalyzer current density reaches 10mA/cm
2.
Embodiment 5
Identical with embodiment 1, just the reaction times will be reduced to 12h.The electrocatalysis characteristic of gained sample:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 133mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 192mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 121mV, this catalyzer current density reaches 10mA/cm
2;
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 138mV, this catalyzer current density reaches 10mA/cm
2;
After composition electrolyzer:
Under pH is 14 conditions, when institute's making alive is 1.5V, this catalyzer current density reaches 10mA/cm
2.
Embodiment 6
Identical with embodiment 1, just ammonium molybdate is become Sodium orthomolybdate.The electrocatalysis characteristic of gained sample:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 143mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 191mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 137mV, this catalyzer current density reaches 10mA/cm
2;
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 153mV, this catalyzer current density reaches 10mA/cm
2;
After composition electrolyzer;
Under pH is 14 conditions, when institute's making alive is 1.52V, this catalyzer current density reaches 10mA/cm
2.
Embodiment 7
Identical with embodiment 1, just thioacetamide is become thiocarbamide.The electrocatalysis characteristic of gained sample:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 131mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 194mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 117mV, this catalyzer current density reaches 10mA/cm
2;
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 128mV, this catalyzer current density reaches 10mA/cm
2;
After composition electrolyzer;
Under pH is 14 conditions, when institute's making alive is 1.48V, this catalyzer current density reaches 10mA/cm
2.
Embodiment 8
Identical with embodiment 1, only nickel foam is become nickel foil sheet.The electrocatalysis characteristic of gained sample:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 156mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 206mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 146mV, this catalyzer current density reaches 10mA/cm
2;
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 183mV, this catalyzer current density reaches 10mA/cm
2;
After composition electrolyzer;
Under pH is 14 conditions, when institute's making alive is 1.57V, this catalyzer current density reaches 10mA/cm
2.
Embodiment 9
Identical with embodiment 1, only P123 is become F127.The electrocatalysis characteristic of gained sample:
Electrocatalysis cracking aquatic products hydrogen;
Under pH is 0 condition, when overpotential is 139mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 7 conditions, when overpotential is 198mV, this catalyzer current density reaches 10mA/cm
2;
Under pH is 14 conditions, when overpotential is 127mV, this catalyzer current density reaches 10mA/cm
2;
Electrocatalysis cracking aquatic products oxygen;
Under pH is 14 conditions, when overpotential is 158mV, this catalyzer current density reaches 10mA/cm
2;
After composition electrolyzer;
Under pH is 14 conditions, when institute's making alive is 1.54V, this catalyzer current density reaches 10mA/cm
2.
Above-mentioned embodiment is only preferred embodiment of the present invention; but protection scope of the present invention is not limited thereto; the change that any those skilled in the art of being familiar with can expect within the spirit and principles in the present invention easily; replace and improve, all should be encompassed in protection scope of the present invention.
Claims (9)
1. the molybdenum oxygen bunch curing three nickel micrometre hollow sphere catalyzer modified, it is characterized in that: be by soluble in water to tensio-active agent, sulphur source and molybdenum source, gained solution is loaded reactor, then adds metallic nickel substrate, prepare after reacting by heating 12h ~ 24h; In sulphur source and molybdenum source, the mol ratio of element sulphur and molybdenum element is 2.4 ~ 14.4:1, and the mol ratio of element sulphur and tensio-active agent is 17.4 ~ 34.9:1, and Heating temperature is 160 ~ 220 DEG C.
2. a kind of molybdenum oxygen as claimed in claim 1 bunch curing three nickel micrometre hollow sphere catalyzer modified, is characterized in that: tensio-active agent is water-soluble triblock copolymer.
3. a kind of molybdenum oxygen as claimed in claim 2 bunch curing three nickel micrometre hollow sphere catalyzer modified, is characterized in that: tensio-active agent is P123 or F127.
4. a kind of molybdenum oxygen as claimed in claim 1 bunch curing three nickel micrometre hollow sphere catalyzer modified, is characterized in that: sulphur source is thiocarbamide, thioacetamide and derivative thereof or its mixture.
5. a kind of molybdenum oxygen as claimed in claim 1 bunch curing three nickel micrometre hollow sphere catalyzer modified, is characterized in that: molybdenum source is water-soluble molybdenum salt.
6. a kind of molybdenum oxygen as claimed in claim 5 bunch curing three nickel micrometre hollow sphere catalyzer modified, is characterized in that: molybdenum source is ammonium molybdate, Sodium orthomolybdate, four thio ammonium molybdate or its mixture.
7. a kind of molybdenum oxygen as claimed in claim 1 bunch curing three nickel micrometre hollow sphere catalyzer modified, is characterized in that: metallic nickel substrate is nickel foam, nickel screen or nickel foil.
8. a kind of molybdenum oxygen of claim 1 ~ 7 described in any one bunch application of curing three nickel micrometre hollow sphere catalyzer in brine electrolysis of modifying.
9. a kind of molybdenum oxygen as claimed in claim 8 bunch application of curing three nickel micrometre hollow sphere catalyzer in brine electrolysis of modifying, is characterized in that: as the negative pole of electrocatalysis cracking aquatic products hydrogen or the positive pole as electrocatalysis cracking aquatic products oxygen.
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| CN107968208A (en) * | 2017-12-01 | 2018-04-27 | 吉林大学 | A kind of nano-lamellar structure of three nickel of curing/molybdenum disulfide composite material and preparation method thereof |
| CN108179433A (en) * | 2016-12-08 | 2018-06-19 | 中国科学院大连化学物理研究所 | Ordered mesopore carbon loads nanometer iridium base electrocatalytic hydrogen evolution electrode and its preparation and application |
| CN109055972A (en) * | 2018-07-20 | 2018-12-21 | 曲阜师范大学 | Mn adulterates Ni3S2Nano-array liberation of hydrogen catalyst and its preparation method and application |
| CN110931268A (en) * | 2019-11-22 | 2020-03-27 | 浙江工业大学 | Oxygen-sulfur doped Ni-Mo bimetallic material for super capacitor and preparation method thereof |
| CN111686821A (en) * | 2020-06-22 | 2020-09-22 | 南京邮电大学 | Ruthenium complex and molybdenum-sulfur cluster dye-sensitized photocatalytic hydrogen production system reaction liquid |
| CN113445072A (en) * | 2021-06-29 | 2021-09-28 | 湖北大学 | Foamed nickel composite electrode and preparation method and application thereof |
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| CN108179433A (en) * | 2016-12-08 | 2018-06-19 | 中国科学院大连化学物理研究所 | Ordered mesopore carbon loads nanometer iridium base electrocatalytic hydrogen evolution electrode and its preparation and application |
| CN108179433B (en) * | 2016-12-08 | 2019-09-06 | 中国科学院大连化学物理研究所 | Ordered mesopore carbon loads nanometer iridium base electrocatalytic hydrogen evolution electrode and its preparation and application |
| CN107968208A (en) * | 2017-12-01 | 2018-04-27 | 吉林大学 | A kind of nano-lamellar structure of three nickel of curing/molybdenum disulfide composite material and preparation method thereof |
| CN107968208B (en) * | 2017-12-01 | 2020-09-25 | 吉林大学 | Nano lamellar structure of trinickel disulfide/molybdenum disulfide composite material and preparation method thereof |
| CN109055972A (en) * | 2018-07-20 | 2018-12-21 | 曲阜师范大学 | Mn adulterates Ni3S2Nano-array liberation of hydrogen catalyst and its preparation method and application |
| CN110931268A (en) * | 2019-11-22 | 2020-03-27 | 浙江工业大学 | Oxygen-sulfur doped Ni-Mo bimetallic material for super capacitor and preparation method thereof |
| CN110931268B (en) * | 2019-11-22 | 2022-09-02 | 浙江工业大学 | Oxygen-sulfur doped Ni-Mo bimetallic material for super capacitor and preparation method thereof |
| CN111686821A (en) * | 2020-06-22 | 2020-09-22 | 南京邮电大学 | Ruthenium complex and molybdenum-sulfur cluster dye-sensitized photocatalytic hydrogen production system reaction liquid |
| CN113445072A (en) * | 2021-06-29 | 2021-09-28 | 湖北大学 | Foamed nickel composite electrode and preparation method and application thereof |
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