CN107335433A - A kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst - Google Patents
A kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst Download PDFInfo
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- CN107335433A CN107335433A CN201710672453.2A CN201710672453A CN107335433A CN 107335433 A CN107335433 A CN 107335433A CN 201710672453 A CN201710672453 A CN 201710672453A CN 107335433 A CN107335433 A CN 107335433A
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- molybdenum oxide
- molybdenum
- hydrogen evolution
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- platinum
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- 239000001257 hydrogen Substances 0.000 title claims abstract description 27
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 27
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 20
- 239000011733 molybdenum Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 28
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 22
- 239000006229 carbon black Substances 0.000 claims abstract description 12
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 8
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000013019 agitation Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 5
- QYSYEILYXGRUOM-UHFFFAOYSA-N [Cl].[Pt] Chemical compound [Cl].[Pt] QYSYEILYXGRUOM-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 235000016768 molybdenum Nutrition 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000004502 linear sweep voltammetry Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910015675 MoO3−x Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002256 photodeposition Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- PTISTKLWEJDJID-UHFFFAOYSA-N sulfanylidenemolybdenum Chemical class [Mo]=S PTISTKLWEJDJID-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/652—Chromium, molybdenum or tungsten
- B01J23/6525—Molybdenum
-
- B01J35/23—
-
- B01J35/33—
-
- B01J35/393—
-
- B01J35/399—
-
- 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
- B01J37/16—Reducing
-
- 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
-
- 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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
- C25B11/061—Metal or alloy
Abstract
The invention belongs to electrocatalytic hydrogen evolution catalyst preparation technical field, discloses a kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst.Prepare the molybdenum oxide of substoichiometric；Under light protected environment, molybdenum oxide and platinum acid chloride solution magnetic agitation are reacted into 1 ~ 5 h, carbon black is then added into the reaction solution, ultrasonic disperse is uniform, drying, produces oxidation molybdenum base efficient electric catalytic hydrogen evolution catalyst；Wherein, the mass percent that the amount of institute's platiniferous accounts for molybdenum oxide in platinum acid chloride solution is 1 ~ 10%, and the mass ratio for the carbon black that molybdenum oxide adds with the later stage is 1: 9 ~ 9: 1.The present invention breaks through traditional platinum carrying method, realizes that platinum deposits under light protected environment, and the compound high usage that ensure that pt atom of carbon black, abundant raw material and technology of preparing is environment friendly and pollution-free.
Description
Technical field
The invention belongs to electrocatalytic hydrogen evolution catalyst preparation technical field, and in particular to one kind oxidation molybdenum base efficient electric catalysis
The preparation method of liberation of hydrogen catalyst.
Background technology
Hydrogen is a kind of clean new energy, is water using its accessory substance after consumption, environmentally safe, is current ideal
One of the new energy of substitute fossil fuels.Production hydrogen main method is divided into electro-catalysis production hydrogen and Photocatalyzed Hydrogen Production, from practical application
Upper electro-catalysis hydrogen generation efficiency is high, easily implements.But electrocatalytic hydrogen evolution efficiency depends on the selection of elctro-catalyst, current commercialized height
Catalyst is imitated still based on platinum carbon catalyst, but the utilization ratio of its platinum is low.People are preparing efficient platinum load electro-catalysis
Using traditional preparation methods such as reducing agent reduction sedimentation, Photodepositions during agent.Platinum supported electrocatalyst preparation and should
In, in order to reduce production cost and reach green purpose, to utilize raw material simple and easy to get and explore one kind more
Simple technology of preparing, this is still a kind of challenge.
The content of the invention
It is an object of the invention to provide a kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst.
To achieve the above object, the technical scheme that the present invention takes is as follows：
A kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst, step are as follows：
（1）Prepare the molybdenum oxide of substoichiometric；The molybdenum oxide of substoichiometric refers to that molybdenum oxide is not for stoichiometry
MoO3, not only contain the molybdenum of+6 valencys, the also molybdenum containing lower valency, i.e. its molecular formula is not MoO3, but MoO3-x；
（2）Under light protected environment, by step（1）Gained molybdenum oxide reacts 1 ~ 5 h with platinum acid chloride solution magnetic agitation, then to this
Carbon black is added in reaction solution, ultrasonic disperse is uniform, drying, produces oxidation molybdenum base efficient electric catalytic hydrogen evolution catalyst；Wherein, chlorine platinum
The mass percent that the amount of institute's platiniferous accounts for molybdenum oxide in acid solution is 1 ~ 10 %, the mass ratio for the carbon black that molybdenum oxide adds with the later stage
For 1: 9 ~ 9: 1.
Preferably, the concentration of platinum acid chloride solution is 46.6 mmol/L.
Preferably, the mass percent that the amount of institute's platiniferous accounts for molybdenum oxide in platinum acid chloride solution is 6 %, and molybdenum oxide adds with the later stage
The mass ratio of the carbon black entered is 1: 1.
The step of the present invention（1）It can be prepared by prior art, for example but be not limited to applicant December 12 in 2016
Patent of invention filed in day（Application number 201611140260.4）Disclosed in amorphous oxide molybdenum nanometer piece preparation method, the preparation
The amorphous oxide molybdenum nanometer sheet that method obtains is exactly the molybdenum oxide of substoichiometric.
The present invention is supplied to a kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst.Substoichiometric
Molybdenum oxide is rich in oxygen defect, and oxidation reaction easily occurs, and has certain reproducibility, the reducible platinum acid chloride solution subsequently added, from
And the Pt nanocrystal body that high dispersive type is loaded on oxidation Mo substrate is realized, it ensure that high catalytic activity.The carbon of high conductivity
The introducing of black-materials further improves the electric conductivity of material, while improves the utilization rate of catalyst, in platinum low-load amount
Under the premise of ensure that the high efficiency of catalyst.From whole preparation process, the present invention breaks through traditional platinum carrying method, in lucifuge
Realize that platinum deposits under environment, and the compound high usage that ensure that pt atom of carbon black, abundant raw material and technology of preparing environmental protection is without dirt
Dye, there is great application prospect in energy conversion field.
Brief description of the drawings
The XPS that Fig. 1 is the Mo of the molybdenum oxide of the substoichiometric prepared by the embodiment of the present invention 1 characterizes picture.
Fig. 2 is the HRTEM pictures of the brilliant molybdenum oxide nanometer sheet of the supported platinum nano synthesized by the embodiment of the present invention 1.
Fig. 3 is the electrocatalytic hydrogen evolution LSV of the oxidation molybdenum base efficient electric catalytic hydrogen evolution catalyst prepared by the embodiment of the present invention 1
Figure.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.It should be understood that following examples are merely to illustrate this
Invention is not for limitation the scope of the present invention.
Embodiment 1
A kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst, step are as follows：
（1）The molybdenum oxide of substoichiometric is prepared by the method for embodiment in CN201611140260.4 1, detailed process is：
Load 10ml 45% in beaker（Volume ratio, similarly hereinafter）Ethanol, 100mg molybdenum sulfides are scattered in the ethanol of 10ml 45%, so
Afterwards by the beaker water bath sonicator 4h containing solution, calcined after being dried in baking oven in retort under 350 DEG C of air ambients
90min, heating rate are 10 DEG C per minute；Product after calcining is redispersed in 45% ethanol, ultrasonic 1h is uniformly dispersed again
After be transferred in reactor, into reactor inject carbon dioxide reach supercriticality（16Mpa, 80 DEG C）, magnetic force stirs
Mix lower reaction 3h；Sample after first supercritical processing is transferred to 50ml centrifuge tubes, with the rotating speed of 6000 turns per minute of centrifuge from
Heart 5min takes supernatant, and the molybdenum oxide of substoichiometric is obtained after drying, and its Mo XPS phenograms are shown in Fig. 1；In terms of XPS collection of illustrative plates
It is not the MoO for stoichiometry to go out sample3, molybdenum (the corresponding two basic change energy in sample not only containing 6 valencys：235.6 eV and
232.4 eV), and 5 valency molybdenums (the corresponding two basic change energy also containing certain lower valency：234.4 eV and 231.2 eV), this
Confirm the property of the substoichiometric of the molybdenum oxide of preparation；
（2）Under room temperature light protected environment, by 10 mg steps（1）The chloroplatinic acid of gained molybdenum oxide and the mmol/L of 66 μ L 46.6 is molten
Liquid mixes, and magnetic agitation reacts 3 h, and now sampling carries out transmission electron microscope sign, and business is then added into remaining reaction solution
The carbon black of change, ultrasonic disperse 30min, now sampling carry out electrocatalytic hydrogen evolution sign, and remainder is then dried, and produces oxidation molybdenum base
Efficient electrocatalytic hydrogen evolution catalyst；Wherein, the mass percent that the amount of institute's platiniferous accounts for molybdenum oxide in platinum acid chloride solution is 6 %, oxygen
The mass ratio for changing the carbon black that molybdenum adds with the later stage is 1: 1.
Sample is supported to be characterized with transmission electron microscope on film in carbon, and its HRTEM is shown in Fig. 2, is clearly seen from high-resolution transmission plot：
Dispersed the nanocrystal of platinum on the matrix of molybdenum oxide nanometer sheet, size are 2nm or so, and this explanation is under the conditions of lucifuge
Chloroplatinic acid generates simple substance platinum by successfully reduction.
Sample electrochemical workstation（CHI 660E）Electrocatalytic hydrogen evolution sign is carried out, electrolyte is 0.5mol/L sulphur
Acid, carbon-point are used as to electrode, and Ag/AgCl is reference electrode, and working electrode is glass-carbon electrode, catalyst loadings on working electrode
For 0.1 mg/cm2（Simultaneously using commercialized 20% Pt/C catalyst as comparative catalyst, Pt quality hundred in comparative catalyst
It is 20% to divide content, and when loading 20% Pt/C catalyst, dispersant is used as by the use of absolute ethyl alcohol）, use linear sweep voltammetry（LSV）
Liberation of hydrogen test is carried out, its LSV is shown in Fig. 3, it is known that：It is -10mA/cm that prepared catalyst of the present invention, which reaches current density,2When mistake
Current potential is with commercialized identical, but take-off potential will be less than 20% Pt/C, and this illustrates inventive samples in the same of platinum low content
Shi Yiran presents excellent electrocatalytic hydrogen evolution performance.
Claims (3)
- A kind of 1. preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst, it is characterised in that：Step is as follows：（1）Prepare the molybdenum oxide of substoichiometric；（2）Under light protected environment, by step（1）Gained molybdenum oxide reacts 1 ~ 5 h with platinum acid chloride solution magnetic agitation, then to this Carbon black is added in reaction solution, ultrasonic disperse is uniform, drying, produces oxidation molybdenum base efficient electric catalytic hydrogen evolution catalyst；Wherein, chlorine platinum The mass percent that the amount of institute's platiniferous accounts for molybdenum oxide in acid solution is 1 ~ 10 %, the mass ratio for the carbon black that molybdenum oxide adds with the later stage For 1: 9 ~ 9: 1.
- 2. preparation method as claimed in claim 1, it is characterised in that：The concentration of platinum acid chloride solution is 46.6 mmol/L.
- 3. preparation method as claimed in claim 1 or 2, it is characterised in that：The amount of institute's platiniferous accounts for molybdenum oxide in platinum acid chloride solution Mass percent be 6 %, the mass ratio for the carbon black that molybdenum oxide adds with the later stage is 1: 1.
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|---|---|---|---|
| CN201710672453.2A CN107335433B (en) | 2017-08-08 | 2017-08-08 | Preparation method of molybdenum oxide-based efficient electrocatalytic hydrogen evolution catalyst |
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| CN201710672453.2A CN107335433B (en) | 2017-08-08 | 2017-08-08 | Preparation method of molybdenum oxide-based efficient electrocatalytic hydrogen evolution catalyst |
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| CN107335433A true CN107335433A (en) | 2017-11-10 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110773162A (en) * | 2019-11-04 | 2020-02-11 | 青岛大学 | Preparation method and application of carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal |
| CN110961101A (en) * | 2019-12-24 | 2020-04-07 | 西南大学 | Platinum-based catalyst, preparation method and application thereof |
| CN110967331A (en) * | 2019-12-06 | 2020-04-07 | 华东理工大学 | Oxidation-reduction-resistant amorphous MoO for SERS substrate3-xPreparation method and application of nanosheet |
| CN113198455A (en) * | 2021-05-17 | 2021-08-03 | 南昌航空大学 | Molybdenum trioxide/molybdenum mesh photocatalyst and preparation method and application thereof |
| CN113750987A (en) * | 2021-09-16 | 2021-12-07 | 南京信息工程大学 | Quadrature phase MoO3Electrocatalyst and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110773162A (en) * | 2019-11-04 | 2020-02-11 | 青岛大学 | Preparation method and application of carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal |
| CN110967331A (en) * | 2019-12-06 | 2020-04-07 | 华东理工大学 | Oxidation-reduction-resistant amorphous MoO for SERS substrate3-xPreparation method and application of nanosheet |
| CN110967331B (en) * | 2019-12-06 | 2022-06-10 | 华东理工大学 | Oxidation-reduction-resistant amorphous MoO for SERS substrate3-xPreparation method and application of nanosheet |
| CN110961101A (en) * | 2019-12-24 | 2020-04-07 | 西南大学 | Platinum-based catalyst, preparation method and application thereof |
| CN110961101B (en) * | 2019-12-24 | 2022-12-06 | 西南大学 | Platinum-based catalyst, preparation method and application thereof |
| CN113198455A (en) * | 2021-05-17 | 2021-08-03 | 南昌航空大学 | Molybdenum trioxide/molybdenum mesh photocatalyst and preparation method and application thereof |
| CN113750987A (en) * | 2021-09-16 | 2021-12-07 | 南京信息工程大学 | Quadrature phase MoO3Electrocatalyst and preparation method and application thereof |
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| CN107335433B (en) | 2020-10-27 |
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