CN109972160A - A kind of preparation method of novel double-function catalyzing electrolysis water electrode - Google Patents

A kind of preparation method of novel double-function catalyzing electrolysis water electrode Download PDF

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Publication number
CN109972160A
CN109972160A CN201910326339.3A CN201910326339A CN109972160A CN 109972160 A CN109972160 A CN 109972160A CN 201910326339 A CN201910326339 A CN 201910326339A CN 109972160 A CN109972160 A CN 109972160A
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preparation
electrode
electrolysis water
cfp
hours
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杨强斌
敬玉娟
彭琴
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • 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
    • 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
    • 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
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention discloses a kind of preparation method of novel double-function catalyzing electrolysis water electrode, the present invention realizes a kind of novel composite catalyst MoxCo by the easy to operate and not high hydro-thermal method of equipment requirement, a step1‑xS2It is grown on carbon fiber paper, to obtain the working electrode with two-functional electrolytic catalytic activity, which has long-term catalytic stability.It is simple with preparation, at low cost, easy industrialized advantage.

Description

A kind of preparation method of novel double-function catalyzing electrolysis water electrode
Technical field
The present invention relates to electrolysis water electrode technical fields, refer specifically to a kind of system of novel double-function catalyzing electrolysis water electrode Preparation Method.
Background technique
As the technology of new energy materials develops, nano molybdenum disulfide (MoS2) urged as a kind of efficient electrolysis water liberation of hydrogen Agent, nano molybdenum disulfide are its exposed edges active sites to obtain its catalytic activity.Since electrolysis water process is by two Half-reaction composition: the evolving hydrogen reaction of cathode and the oxygen evolution reaction of anode, the MoS prepared at present2Catalyst achieves excellent electricity Water catalytic activity for hydrogen evolution is solved, but does not have the Oxygen anodic evolution catalytic activity of electrolysis water, so modified molybdenum disulfide is needed to have Double-function catalyzing activity.In addition, after obtaining the nano powder catalyst that has excellent performance, how catalyst is applied to working electrode On also become one of the factor that is limited in the actual process of powder catalyst.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of novel double-function catalyzing electrolysis water electrode, solve existing The MoS of preparation method preparation2Catalyst does not have the Oxygen anodic evolution catalytic activity of electrolysis water and powder catalyst is applied to work On electrode be limited the problem of.
To achieve the goals above, technical solution of the invention are as follows: the novel double-function catalyzing electricity of described one kind The preparation method for solving water electrode, specifically comprises the following steps:
(1) solution is prepared, and weighs two molybdic acid hydrate sodium (Na2MoO4·2H2O) 0 ~ 1.0mmol weighs two hydration cobaltous dichlorides (CoCl2∙2H2O) 0 ~ 1.0mmol, thiocarbamide 2mmol are sequentially added into the pure water of 70 ml, and stirring 1 ~ 2 hour strongly makes It is uniformly mixed；
(2) is by CFP(carbon fiber paper) rectangle of 2cm × 1cm is cut into, and kept for 2~2.5 hours at 350 ~ 400 DEG C, Keep its surface more hydrophilic；
(3) pours into prepared solution in the reaction kettle of the polytetrafluoroethyllining lining of 100ml, then by CFP(carbon fiber Paper) it is vertically placed on centre, reaction kettle is kept for 16 ~ 20 hours at 220 DEG C；Natural cooling reaction kettle takes out carbon paper sample with pure Water rinses repeatedly, then under a nitrogen 60 DEG C after drying 12 hours to get double-function catalyzing electrolysis water electrode.
The beneficial effects of the present invention are: the present invention, by the easy to operate and not high hydro-thermal method of equipment requirement, a step is realized A kind of novel composite catalyst MoxCo1-xS2It is grown on carbon fiber paper, so that obtaining, there is two-functional electrolytic catalysis to live Property working electrode, the working electrode have long-term catalytic stability.It is simple with preparation, it is at low cost, it is easily industrialized excellent Point.
Detailed description of the invention
Attached drawing 1 is the SEM figure of different samples prepared by the embodiment of the present invention 1~3；
Attached drawing 2 is Mo made from the embodiment of the present invention 2xCo1-xS2The distribution diagram of element of carbon fiber surface in/CFP；
Attached drawing 3 is the catalytic activity of hydrogen evolution polarization curve of different samples prepared by the embodiment of the present invention 1~3；
Attached drawing 4 is Mo prepared by the embodiment of the present invention 2xCo1-xS2Current-time curvel figure under the constant potential test of/CFP.
Specific embodiment
The present invention is further described With reference to embodiment.
Embodiment 1
A kind of preparation method of novel double-function catalyzing electrolysis water electrode；The following steps are included:
(1) solution is prepared, and weighs two molybdic acid hydrate sodium (Na2MoO4·2H2O) 1.0mmol weighs thiocarbamide 2mmol, respectively In the pure water for sequentially adding 70 ml, stirring strongly is uniformly mixed it；
(2) is by CFP(carbon fiber paper) rectangle of 2cm × 1cm is cut into, and kept for 2.5 hours at 350 DEG C, make its table Face is more hydrophilic；
(3) pours into prepared solution in the reaction kettle of the polytetrafluoroethyllining lining of 100ml, then by CFP(carbon fiber Paper) it is vertically placed on centre, reaction kettle is kept for 16 hours at 220 DEG C；Natural cooling reaction kettle takes out carbon paper sample and is rushed with pure water Wash repeatedly, then under a nitrogen 60 DEG C after drying 12 hours to get double-function catalyzing electrolysis water electrode.
The MoS of preparation2/ CFP electrode surface catalyst form is the MoS to reunite2Nanometer sheet.
Embodiment 2
A kind of preparation method of novel electrocatalytic hydrogen evolution electrode, specifically comprises the following steps:
(1) solution is prepared, and weighs two molybdic acid hydrate sodium (Na2MoO4·2H2O) 0.9 mmol weighs two hydration cobaltous dichlorides (CoCl2∙2H2O) 0.1 mmol weighs thiocarbamide 2mmol, is sequentially added into the pure water of 70 ml, stirs 1 ~ 2 hour strongly It is uniformly mixed it；
(2) is by CFP(carbon fiber paper) rectangle of 2cm × 1cm is cut into, and kept for 2 hours at 400 DEG C, make its surface It is more hydrophilic；
(3) pours into prepared solution in the reaction kettle of the polytetrafluoroethyllining lining of 100ml, then by CFP(carbon fiber Paper) it is vertically placed on centre, reaction kettle is kept for 18 hours at 220 DEG C；Natural cooling reaction kettle takes out carbon paper sample and is rushed with pure water Wash repeatedly, then under a nitrogen 60 DEG C after drying 12 hours to get double-function catalyzing electrolysis water electrode.
The Mo of preparationxCo1-xS2/ CFP (1:1) electrode surface catalyst form is MoxCo1-xS2Nanometer sheet and form is equal One.
Embodiment 3
A kind of preparation method of novel electrocatalytic hydrogen evolution electrode, specifically comprises the following steps:
(1) solution is prepared, and weighs two hydration cobaltous dichloride (CoCl2∙2H2O) 1 mmol weighs thiocarbamide 2mmol, respectively according to In the secondary pure water that 70 ml are added, stirring strongly is uniformly mixed it；
(2) is by CFP(carbon fiber paper) rectangle of 2cm × 1cm is cut into, and kept for 15 minutes 2 hours at 370 DEG C, make Its surface is more hydrophilic；
(3) pours into prepared solution in the reaction kettle of the polytetrafluoroethyllining lining of 100ml, then by CFP(carbon fiber Paper) it is vertically placed on centre, reaction kettle is kept for 20 hours at 220 DEG C；Natural cooling reaction kettle takes out carbon paper sample and is rushed with pure water Wash repeatedly, then under a nitrogen 60 DEG C after drying 12 hours to get double-function catalyzing electrolysis water electrode.
The CoS of the preparation of preparation2/ CFP electrode surface catalyst form is some isolated CoS2Tufted form and at micron Grade.
The different samples of Examples 1 to 3 preparation, corresponding sample are included in table 1, carry out SEM table to different samples
Table 1. prepares different catalyst: MoS2, MoxCo1-xS2 and CoS2 on CFP
Drug Na2MoO4·2H2O CoCl2·2H2O Thiocarbamide
MoS2/CFP 1 mmol - 2 mmol
MoxCo1-xS2/CFP 0.9 mmol 0.1 mmol 2 mmol
CoS2/CFP - 1 mmol 2 mmol
Sign, discovery table face grown the catalyst of different shape.In the case where the only Mo precursor of embodiment 1, preparation MoS2/ CFP electrode surface catalyst form is the MoS to reunite2Nanometer sheet (a sample in attached drawing 1)；In the Mo precursor of embodiment 2 With Co precursor ratio be 9:1 when, the Mo of preparationxCo1-xS2/ CFP (1:1) electrode surface catalyst form is MoxCo1-xS2It receives Rice piece and form is uniform (b sample in attached drawing 1), carries out element surface sweeping discovery to its surface, Mo, Co and S element is uniformly distributed In its carbon fiber surface (attached drawing 2)；In the only Co precursor of embodiment 3, the CoS of preparation2/ CFP electrode surface catalyst Form is some isolated CoS2Tufted form and at micron order (c sample in attached drawing 1).
Embodiment 4
Common three-electrode system electro-chemical test is carried out to the catalysis electrode of different surface configurations: in the sulfuric acid solution of 0.5M In, platinum carbon electrode is auxiliary electrode, and saturation potassium chloride calomel electrode is reference electrode, and different catalysis electrode samples are exposed 1 Square centimeter is used as working electrode, and test result is as shown in Fig. 3, it is found that the uniform Mo of configuration of surfacexCo1-xS2/ CFP electrode With good double-function catalyzing liberation of hydrogen and oxygen evolution activity (as shown in Fig. 4).
The above, embodiment is only that preferred embodiments of the present invention will be described, not to of the invention Range is defined, and under the premise of not departing from the spirit of the technology of the present invention, this field engineers and technicians are to skill of the invention The various changes and improvements that art scheme is made, should fall within the scope of protection determined by the claims of the present invention.

Claims (1)

1. a kind of preparation method of novel double-function catalyzing electrolysis water electrode, it is characterized in that: double function that described one kind is novel The preparation method of energy catalytic electrolysis water electrode, specifically comprises the following steps:
Solution is prepared, and two molybdic acid hydrate sodium (Na are weighed2MoO4·2H2O) 0 ~ 1.0mmol weighs two hydration cobaltous dichloride (CoCl2 ∙2H2O) 0 ~ 1.0mmol, thiocarbamide 2mmol are sequentially added into the pure water of 70 ml, and stirring 1 ~ 2 hour strongly makes its mixing Uniformly；
By CFP(carbon fiber paper) rectangle of 2cm × 1cm is cut into, and kept for 2~2.5 hours at 350 ~ 400 DEG C, make it Surface is more hydrophilic；
Prepared solution is poured into the reaction kettle of the polytetrafluoroethyllining lining of 100ml, then by CFP(carbon fiber paper) it is vertical It is placed on centre, reaction kettle is kept for 16 ~ 20 hours at 220 DEG C；It is more to take out carbon paper sample pure water rinsing for natural cooling reaction kettle It is secondary, then under a nitrogen 60 DEG C after drying 12 hours to get double-function catalyzing electrolysis water electrode.
CN201910326339.3A 2019-04-23 2019-04-23 A kind of preparation method of novel double-function catalyzing electrolysis water electrode Pending CN109972160A (en)

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CN113430560A (en) * 2021-07-09 2021-09-24 北京化工大学 Bimetal monatomic loaded MoS2Carbon paper base material and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN113430560A (en) * 2021-07-09 2021-09-24 北京化工大学 Bimetal monatomic loaded MoS2Carbon paper base material and preparation method and application thereof
CN113430560B (en) * 2021-07-09 2022-11-15 北京化工大学 Bimetal monatomic loaded MoS 2 Carbon paper base material and preparation method and application thereof

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Application publication date: 20190705