CN107754786A - One kind utilizes KMnO4The method that electrocatalytic oxidation is improved on direct oxidation graphite paper - Google Patents
One kind utilizes KMnO4The method that electrocatalytic oxidation is improved on direct oxidation graphite paper Download PDFInfo
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- CN107754786A CN107754786A CN201710960262.6A CN201710960262A CN107754786A CN 107754786 A CN107754786 A CN 107754786A CN 201710960262 A CN201710960262 A CN 201710960262A CN 107754786 A CN107754786 A CN 107754786A
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- Prior art keywords
- graphite paper
- kmno
- improved
- direct oxidation
- electrocatalysis characteristic
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 56
- 239000010439 graphite Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000003647 oxidation Effects 0.000 title claims abstract description 21
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 15
- 229910016978 MnOx Inorganic materials 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 3
- 230000004044 response Effects 0.000 claims abstract description 3
- 239000011149 active material Substances 0.000 abstract description 10
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- B01J35/33—
Abstract
One kind utilizes KMnO4The method that electrocatalysis characteristic is improved on direct oxidation graphite paper, comprises the following steps：(1) graphite paper is cut into rectangle, cleaned up by acetone, deionized water, placed drying in oven, the graphite paper after being dried, put in polytetrafluoroethylene (PTFE) bottle；(2) KMnO is configured4Solution；(3) KMnO is taken4Solution, being placed with the polytetrafluoroethylene (PTFE) bottle of graphite paper into step (1) is added into, then the bottle is put into stainless steel water heating kettle again, sealed, reaction；(4) after question response terminates, allow reactor to naturally cool to room temperature, reacted graphite paper is washed through deionized water, dry, obtain MnOx/ GP electrodes.The method of the present invention directly utilizes KMnO4Direct oxidation graphite paper, graphite paper be both reducing agent may act as again support active material base material, reduzate MnOxIt will be grown on graphite paper sheet so that manganese dioxide can improve electrocatalysis characteristic with graphite paper with strong bonded, and active material is difficult for drop-off so that electrocatalysis characteristic is stable.
Description
Technical field
The invention belongs to electrode material preparing technical field, and in particular to one kind utilizes KMnO4Direct oxidation graphite paper, is obtained
To active material MnOx, the material can be with strong bonded, so as to obtain the MnO of high activity with graphite paper substratesx/ GP electrodes, improve
The method of electro-catalysis.
Background technology
Manganese element abundance, discussion are attached to the Mn oxide of collection liquid surface its electrocatalysis characteristic, and research improves manganese
The electrocatalysis characteristic of oxide has important practical significance.The main reason for restricting Mn oxide electrocatalysis characteristic is electric conductivity
Difference.It is compound by being carried out with carbon nanomaterial, its conductive capability is improved, is expected to strengthen its electrocatalysis characteristic.
Hydro-thermal method building-up process is betided in reactor, using solution as medium, by the heating to reactor, builds height
Temperature, the environment of high pressure so that under normal circumstances indissoluble or some insoluble materials can dissolve, and undergo dissolving, tie again
Brilliant or curing process, is ultimately formed with nano structural material.The electro-deposition active material on active substrate, it can show
High OER electro catalytic activities, but by after loop test, active material easily comes off, and electrocatalysis characteristic has dropped
It is low.Therefore adhesive force of the enhancing active material on surface plays a key effect to improving its performance.Chemically reacted with substrate,
Make strong coupling relation between active material and conductive substrates be present, the active electrode for obtaining adhesion-tight is that one kind can effectively improve
The means of material OER electrocatalysis characteristics.
In the method, we use hydro-thermal method with KMnO4It is anti-with substrate graphite paper chemistry to occur for solution as oxidant
Should, obtain active material MnOx, the material can be with strong bonded, so as to obtain the MnO of high activity with graphite paper substratesx/ GP electricity
Pole, the method for improving electro-catalysis.
At present, it there is no both at home and abroad and utilize KMnO4Direct oxidation graphite paper, manganese dioxide is promoted firmly to be tied with graphite paper
Close, improve the relevant report of electrocatalysis characteristic.
The information for being disclosed in the background section is merely intended to understanding of the increase to the general background of the present invention, without answering
It has been the prior art well known to persons skilled in the art when being considered as recognizing or implying the information structure in any form.
The content of the invention
One of the technical problem to be solved in the present invention is to utilize simple technique so that elctro-catalyst is firmly tied with substrate
Close；The second technical problem to be solved by the present invention is to have used hydro-thermal method to obtain effective elctro-catalyst sedimentary；The present invention will
The three of the technical problem of solution are the electrocatalysis characteristics that electrode is improved using simple technique.To achieve these goals, originally
Invention is realized using following technical scheme：
One kind utilizes KMnO4The method that electrocatalysis characteristic is improved on direct oxidation graphite paper, comprises the following steps：
(1) graphite paper is cut into rectangle, cleaned up by acetone, deionized water, be placed on 60 DEG C of drying in oven
At least 6h, the graphite paper after being dried, put in polytetrafluoroethylene (PTFE) bottle；
(2) KMnO is configured4Solution；
(3) 20mL KMnO is taken4Solution, being placed with the polytetrafluoroethylene (PTFE) bottle of graphite paper into step (1) is added into,
Then the bottle is put into stainless steel water heating kettle again, sealed, reaction；
(4) after question response terminates, allow reactor to naturally cool to room temperature, reacted graphite paper is washed through deionized water
4-5 times, dried in 60 DEG C of baking ovens, obtain MnOx/ GP electrodes.
Preferably, the area of described graphite paper is not less than 1cm2。
Preferably, KMnO in step (2)4The concentration of solution is 0.01-2mol L-1。
Preferably, the temperature of reaction is 100-180 DEG C in step (3)；The time of reaction is 4-16h.
Preferably, the time dried in step (4) is 0.1-12h.
Compared with prior art, the present invention has the advantages that：
(1) method of the invention directly utilizes KMnO4Direct oxidation graphite paper, graphite paper are both that reducing agent may act as propping up again
Support the base material of active material, reduzate MnOxIt will be grown on graphite paper sheet so that manganese dioxide can with graphite paper
With strong bonded, electrocatalysis characteristic is improved.Active material is difficult for drop-off so that electrocatalysis characteristic is stable.
(2) method technique of the invention is simple, mild condition, and cost is low.
Brief description of the drawings
Accompanying drawing 1 is the electron microscope for the graphite paper not reacted；
Accompanying drawing 2 is the obtained MnO of embodiment 1xThe electron microscope of/GP electrodes；
Accompanying drawing 3 be contrasted MnO is deposited on graphite paperxLSV curves；
Accompanying drawing 4 is that embodiment 1 obtains MnOxThe LSV curves of/GP electrodes；
Accompanying drawing 5 is that embodiment 2 obtains MnOxThe LSV curves of/GP electrodes；
Accompanying drawing 6 is that embodiment 3 obtains MnOxThe LSV curves of/GP electrodes.
Embodiment
The embodiment of the present invention is described in detail with reference to specific embodiment, it is to be understood that of the invention
Protection domain do not limited by embodiment.
Embodiment 1：
One kind utilizes KMnO4The method that electrocatalytic oxidation is improved on direct oxidation graphite paper, comprises the following steps：
(1) at room temperature, graphite paper is cut to 1 × 2.3cm2The rectangle of specification, cleaned by acetone, deionized water
Totally, it is placed at least 6h in 60 DEG C of baking ovens；
(2) dried graphite paper is placed into 25mL polytetrafluoroethylliner liners；
(3) appropriate KMnO is weighed4And stirring and dissolving is dissolved in 100mL volumetric flasks surely in deionized water, is configured to dense
Spend for 0.05mol L-1Solution；
(4) the ready KMnO of 20mL are measured4Solution adds the stainless steel water heating kettle sealing of placing graphite paper, 140
6h is reacted at DEG C.After reaction terminates, allow reactor to naturally cool to room temperature, reacted graphite paper is washed into 4- through deionized water
5 times, 6h is dried in 60 DEG C of baking ovens, obtains MnOx/ GP electrodes.
Embodiment 2：
One kind utilizes KMnO4The method that electrocatalytic oxidation is improved on direct oxidation graphite paper, comprises the following steps：
(1) at room temperature, graphite paper is cut to 1 × 2.3cm2The rectangle of specification, cleaned by acetone, deionized water
Totally, it is placed at least 6h in 60 DEG C of baking ovens；
(2) dried graphite paper is placed into 25mL polytetrafluoroethylliner liners；
(3) appropriate KMnO is weighed4And stirring and dissolving is dissolved in 100mL volumetric flasks surely in deionized water, is configured to dense
Spend for 0.05mol L-1Solution.Measure the ready KMnO of 20mL4Solution adds the stainless steel water heating kettle of placing graphite paper
Sealing, reacts 6h at 120 DEG C；
(4) after reaction terminates, allow reactor to naturally cool to room temperature, reacted graphite paper is washed into 4- through deionized water
5 times, 6h is dried in 60 DEG C of baking ovens, obtains MnOx/ GP electrodes.
Embodiment 3：
One kind utilizes KMnO4The method that electrocatalytic oxidation is improved on direct oxidation graphite paper, comprises the following steps：
(1) at room temperature, graphite paper is cut to 1 × 2.3cm2The rectangle of specification, cleaned by acetone, deionized water
Totally, it is placed at least 6h in 60 DEG C of baking ovens；
(2) dried graphite paper is placed into 25mL polytetrafluoroethylliner liners；
(3) appropriate KMnO is weighed4And stirring and dissolving is dissolved in 100mL volumetric flasks surely in deionized water, is configured to dense
Spend for 0.05mol L-1Solution；
(4) the ready KMnO of 20mL are measured4Solution adds the stainless steel water heating kettle sealing of placing graphite paper, 200
6h is reacted at DEG C.After reaction terminates, allow reactor to naturally cool to room temperature, reacted graphite paper is washed into 4- through deionized water
5 times, 6h is dried in 60 DEG C of baking ovens, obtains MnOx/ GP electrodes.Using CHI 660D electrochemical workstations in embodiment 1-3
The MnO being preparedx/ GP electrodes carry out all electrochemical property tests.
At 30 DEG C of constant temperature, using three-electrode system, (3.5molL is inside filled using AgCl/Ag electrodes-1Saturation KCl is molten
Liquid) reference electrode is used as, platinum plate electrode is as auxiliary electrode, and graphite paper electrode is as working electrode, according to the property of working electrode
Matter selects suitable electrolyte, and the electrolyte that this example is selected is alkaline KOH solution (1molL-1).Before the test begins to electricity
Xie Chizhong is continually fed into high pure oxygen 30min, electrolyte is reached oxygen saturation.
In addition, it is necessary to supplemented in embodiment the present invention method obtain electrode performance measurement (high specific capacitance it is specific
Numerical value), preferably compared with the electrode (control) that conventional method obtains.
The method of the present invention of table 1 obtains the performance measurement of electrode
Note：Compare to deposit MnOx on graphite paper, other are identical with the method for the present invention.
As shown in Table 1, the MnO that method of the invention obtainsxThe electrocatalysis characteristic of/GP electrodes is more preferable.
The description of the foregoing specific illustrative embodiment to the present invention is to illustrate and the purpose of illustration.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to above-mentioned teaching, can be much changed
And change.The purpose of selecting and describing the exemplary embodiment is that explain that the certain principles of the present invention and its reality should
With so that those skilled in the art can realize and utilize the present invention a variety of exemplaries and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (5)
1. one kind utilizes KMnO4The method that electrocatalysis characteristic is improved on direct oxidation graphite paper, it is characterised in that including following step
Suddenly：
(1) graphite paper is cut into rectangle, cleaned up by acetone, deionized water, be placed on 60 DEG C of drying in oven at least
6h, the graphite paper after being dried, put in polytetrafluoroethylene (PTFE) bottle；
(2) KMnO is configured4Solution；
(3) 20mL KMnO is taken4Solution, being placed with the polytetrafluoroethylene (PTFE) bottle of graphite paper into step (1) is added into, then
The bottle is put into stainless steel water heating kettle again, sealed, reaction；
(4) after question response terminates, allow reactor to naturally cool to room temperature, reacted graphite paper is washed into 4-5 through deionized water
It is secondary, dried in 60 DEG C of baking ovens, obtain MnOx/ GP electrodes.
2. according to claim 1 utilize KMnO4The method that electrocatalysis characteristic is improved on direct oxidation graphite paper, its feature
It is, the area of described graphite paper is not less than 1cm2。
3. according to claim 1 utilize KMnO4The method that electrocatalysis characteristic is improved on direct oxidation graphite paper, its feature
It is, KMnO in step (2)4The concentration of solution is 0.01-2mol L-1。
4. according to claim 1 utilize KMnO4The method that electrocatalysis characteristic is improved on direct oxidation graphite paper, its feature
It is, the temperature of reaction is 100-180 DEG C in step (3)；The time of reaction is 4-16h.
5. according to claim 1 utilize KMnO4The method that electrocatalysis characteristic is improved on direct oxidation graphite paper, its feature
It is, the time dried in step (4) is 0.1-12h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710960262.6A CN107754786B (en) | 2017-10-16 | 2017-10-16 | By using KMnO4Method for improving electrocatalytic oxidation on direct oxidized graphite paper |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710960262.6A CN107754786B (en) | 2017-10-16 | 2017-10-16 | By using KMnO4Method for improving electrocatalytic oxidation on direct oxidized graphite paper |
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| Publication Number | Publication Date |
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| CN107754786A true CN107754786A (en) | 2018-03-06 |
| CN107754786B CN107754786B (en) | 2020-06-16 |
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Cited By (2)
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| CN112981453A (en) * | 2021-02-05 | 2021-06-18 | 常熟理工学院 | Method for preparing water oxidation electrode by using waste stainless steel as base material |
| CN115472443A (en) * | 2022-08-18 | 2022-12-13 | 浙江理工大学 | Method for loading graphene quantum dots on graphite paper by hydrothermal method and application of method in preparation of planar micro supercapacitor |
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| CN115472443A (en) * | 2022-08-18 | 2022-12-13 | 浙江理工大学 | Method for loading graphene quantum dots on graphite paper by hydrothermal method and application of method in preparation of planar micro supercapacitor |
| CN115472443B (en) * | 2022-08-18 | 2023-12-15 | 浙江理工大学 | Method for loading graphene quantum dots on graphite paper by hydrothermal method and application of method in aspect of preparing planar miniature supercapacitor |
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