CN108273495A - A kind of preparation method of multi-pore channel graphite paper - Google Patents
A kind of preparation method of multi-pore channel graphite paper Download PDFInfo
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- CN108273495A CN108273495A CN201711385674.8A CN201711385674A CN108273495A CN 108273495 A CN108273495 A CN 108273495A CN 201711385674 A CN201711385674 A CN 201711385674A CN 108273495 A CN108273495 A CN 108273495A
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- China
- Prior art keywords
- graphite paper
- preparation
- reaction
- kmno
- solution
- Prior art date
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 74
- 239000010439 graphite Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011148 porous material Substances 0.000 title abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 229910016978 MnOx Inorganic materials 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
- 239000004575 stone Substances 0.000 claims abstract description 4
- 238000009991 scouring Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims 1
- 229910052748 manganese Inorganic materials 0.000 claims 1
- 239000011572 manganese Substances 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 8
- 239000012286 potassium permanganate Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 13
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 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
- 239000011149 active material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance 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
- B01J23/16—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—
-
- 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
- B01J37/12—Oxidising
Abstract
A kind of preparation method of porous graphite paper, includes the following steps：(1) graphite paper is cut into rectangle, cleaned up, dried, put in polytetrafluoroethylene (PTFE) bottle；(2) KMnO is configured4Solution；(3) KMnO is taken4Solution is added into being placed in the polytetrafluoroethylene (PTFE) bottle of graphite paper into step (1), then the bottle is put into stainless steel water heating kettle again, seals, reaction；(4) it allows reaction kettle to naturally cool to room temperature, the graphite paper after reaction is washed through deionized water, it is dry, obtain MnOx/ GP electrodes；(5) MnO for obtaining step (4)x/ GP electrodes, which are placed in HCL solution, to be stood, until the Mn oxide dissolving on graphite paper surface is complete, then is used deionized water scouring stone ink paper, is dried, obtain porous graphite paper electrode.The present invention utilizes KMnO4Direct oxidation graphite paper, after the oxide that surface is adhered to is washed off with acid so that many apertures occurs in graphite paper surface, makes its surface area increase, the electrocatalysis characteristic of electrode can be promoted using this multi-pore channel graphite paper as substrate.
Description
Technical field
The invention belongs to electrode material preparing technical fields, and in particular to a kind of preparation method of porous graphite paper.
Background technology
In general, the effect of substrate is chiefly to facilitate the transmission of electronics, and provides in cyclic process and stablize support.Greatly
Most business conductive substrates do not have electro catalytic activity, therefore the catalytic activity of electrode is contributed by the active material loaded, is caused
The quality utilization rate of electrode is relatively low.It is contemplated that if conductive substrates also have electro catalytic activity, it is based on the active substrate
Its electrode surface utilization rate of the electrode constructed will improve, and then enhance its electrocatalysis characteristic.Graphite paper (graphite
Paper, GP) it is the good sheeting of flexibility made of one kind is suppressed by powdered graphite, it is cheap.Make about graphite paper
Research for elctro-catalyst or electro-catalysis substrate has not been reported.Material can be effectively improved by preparing the nano material of porous structure
Electrocatalysis characteristic expands and the area of the contact of reactant because such structure possesses the active area of bigger.
In the method, by heated oxide process, a large amount of nano-pore of graphite paper Surface Creation.Nano-pore can be steady
It is fixed to exist.After so that oxide on surface is removed by pickling method, nano surface hole can be fully exposed.Surface exists a large amount of
The substrate of pore passage structure the active area of material will be made to greatly increase, increase the contact area of material and electrolyte.
Currently, not yet using heating with KMnO4Direct oxidation graphite paper obtains the related report of multi-pore channel graphite paper
Road.
Being disclosed in the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without answering
It has been the prior art well known to persons skilled in the art when being considered as recognizing or imply that the information is constituted in any form.
Invention content
The present invention provides a kind of preparation method of porous graphite paper, makes potassium permanganate oxidation graphite paper with the method for heating,
Its surface is set porous structure occur, surface area increases, and this method is simple for process, mild condition, at low cost.
To achieve the goals above, the present invention is realized using following technical scheme：
A kind of preparation method of porous graphite paper, includes the following steps：
(1) graphite paper is cut into rectangle, is 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 are put in polytetrafluoroethylene (PTFE) bottle；
(2) KMnO is configured4Solution；
(3) KMnO of 20mL is taken4Solution is added into being placed in the polytetrafluoroethylene (PTFE) bottle of graphite paper into step (1),
Then the bottle is put into stainless steel water heating kettle again, is sealed, reaction；
(4) it waits for after reaction, reaction kettle being allowed to naturally cool to room temperature, the graphite paper after reaction is washed through deionized water
It is 4-5 times, dry in 60 DEG C of baking ovens, obtain MnOx/ GP electrodes；
(5) MnO for obtaining step (4)x/ GP electrodes, which are placed in HCL solution, stands 30min, until graphite paper surface
Mn oxide dissolving is complete, then with deionized water scouring stone ink paper 4-5 times, is placed on 60 DEG C of drying in oven at least 6h,
Obtain porous graphite paper electrode.
Preferably, the rectangular area described in step (1) is not less than 1cm2。
Preferably, KMnO in step (2)4A concentration of 0.01-2mol L of solution-1。
Preferably, the temperature reacted in step (3) is 120-160 DEG C；The time of reaction is 4-16h.
Preferably, the time dry in step (4) is 0.1-12h.
Preferably, in step (5) HCL solution a concentration of 3-10molL-1。
Compared with prior art, the present invention has the advantages that：
(1) present invention directly utilizes KMnO4Oxidized graphite paper, after the oxide that surface is adhered to is washed off with acid so that stone
There are many apertures in black paper surface, so that its surface area is increased, can be promoted as substrate using this multi-pore channel graphite paper
The electrocatalysis characteristic of electrode.
(2) method and process of the invention is simple, and mild condition is at low cost.
Description of the drawings
Fig. 1 is the electron microscope of empty graphite paper；
Fig. 2 is the electron microscope that porous graphite paper is prepared in method in embodiment 1；
Fig. 3 is the electron microscope that porous graphite paper is prepared in method in embodiment 2；
Fig. 4 is that porous and empty graphite paper LSV curves are prepared in method in embodiment 2.
Specific implementation mode
The specific implementation mode of the present invention is described in detail with reference to specific embodiment, it is to be understood that of the invention
Protection domain be not restricted by specific implementation.
Embodiment 1：
A kind of preparation method of porous graphite paper, includes the following steps：
(1) at room temperature, graphite paper is cut to 1 × 2.3cm2The rectangle of specification is cleaned by acetone, deionized water
Totally, it is placed at least 6h in 60 DEG C of baking ovens；Graphite paper after drying is placed into 25mL polytetrafluoroethylliner liners；
(2) suitable KMnO is weighed4And stirring and dissolving is dissolved in deionized water in 100mL volumetric flasks surely, is configured to dense
Degree is 0.05mol L-1Solution；
(3) the ready KMnO of 20mL are measured4The stainless steel water heating kettle sealing for having placed graphite paper is added in solution, 120
6h is reacted at DEG C；
(4) after reaction, it allows reaction kettle to naturally cool to room temperature, the graphite paper after reaction is washed into 4- through deionized water
5 times, dry 6h, obtains MnOx/GP electrodes in 60 DEG C of baking ovens；
(5) at room temperature, MnOx/GP electrodes obtained above are placed in 3molL-1In HCl solution, 30min is stood, directly
Mn oxide dissolving to graphite paper surface is complete, and graphite paper is cleaned 4-5 times with deionized water, after be placed in 60 DEG C of baking ovens extremely
Few 6h, finally obtains porous graphite paper electrode.
Embodiment 2：
A kind of preparation method of porous graphite paper, includes the following steps：
(1) at room temperature, graphite paper is cut to 1 × 2.3cm2The rectangle of specification is cleaned by acetone, deionized water
Totally, it is placed at least 6h in 60 DEG C of baking ovens, the graphite paper after drying is placed into 25mL polytetrafluoroethylliner liners；
(2) suitable KMnO is weighed4And stirring and dissolving is dissolved in deionized water in 100mL volumetric flasks surely, is configured to dense
Degree is 0.05mol L-1Solution；
(3) the ready KMnO of 20mL are measured4The stainless steel water heating kettle sealing for having placed graphite paper is added in solution, 160
6h is reacted at DEG C；
(4) after reaction, it allows reaction kettle to naturally cool to room temperature, the graphite paper after reaction is washed into 4- through deionized water
5 times, dry 6h, obtains MnO in 60 DEG C of baking ovensx/ GP electrodes；
(5) at room temperature, MnOx/GP electrodes obtained above are placed in 3molL-1In HCl solution, 30min is stood, directly
Mn oxide dissolving to graphite paper surface is complete, and graphite paper is cleaned 4-5 times with deionized water, after be placed in 60 DEG C of baking ovens extremely
Few 6h, finally obtains porous graphite paper electrode.
Embodiment 3：
A kind of preparation method of porous graphite paper, includes the following steps：
(1) at room temperature, graphite paper is cut to 1 × 2.3cm2The rectangle of specification is cleaned by acetone, deionized water
Totally, it is placed at least 6h in 60 DEG C of baking ovens, the graphite paper after drying is placed into 25mL polytetrafluoroethylliner liners；
(2) suitable KMnO is weighed4And stirring and dissolving is dissolved in deionized water in 100mL volumetric flasks surely, is configured to dense
Degree is 0.05mol L-1Solution；
(3) the ready KMnO of 20mL are measured4The stainless steel water heating kettle sealing for having placed graphite paper is added in solution, 140
6h is reacted at DEG C；
(4) after reaction, it allows reaction kettle to naturally cool to room temperature, the graphite paper after reaction is washed into 4- through deionized water
5 times, dry 6h, obtains MnO in 60 DEG C of baking ovensx/ GP electrodes；
(5) at room temperature, MnOx/GP electrodes obtained above are placed in 3molL-1In HCl solution, 30min is stood, directly
Mn oxide dissolving to graphite paper surface is complete, and graphite paper is cleaned 4-5 times with deionized water, after be placed in 60 DEG C of baking ovens extremely
Few 6h, finally obtains porous graphite paper electrode.
All electricity are carried out to the porous graphite paper electrode obtained in embodiment 1-3 using CHI 660D electrochemical workstations
Chemical property is tested.At 30 DEG C of constant temperature, using three-electrode system, (3.5molL is inside filled using AgCl/Ag electrodes-1Saturation
KCl solution) it is used as reference electrode, platinum plate electrode is as auxiliary electrode, and graphite paper electrode is as working electrode, according to working electrode
Property to select suitable electrolyte, the electrolyte that this example is selected be alkaline KOH solution (1molL-1).Before the test begins
It is continually fed into high pure oxygen into electrolytic cell 30 minutes, electrolyte is made to reach oxygen saturation.
As shown in Figure 4, the porous graphite paper electrode electro catalytic activity obtained after oxidized is significantly improved, 10 values of η
466mV is reduced to by original 493mV, illustrates the electrocatalysis characteristic for the porous graphite paper electrode that the method for the present invention obtains more
It is good.
The description of the aforementioned specific exemplary embodiment to the present invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining the specific principle of the present invention and its actually answering
With so that those skilled in the art can realize and utilize the present invention a variety of different exemplary implementation schemes and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (6)
1. a kind of preparation method of porous graphite paper, which is characterized in that include the following steps：
(1) graphite paper is cut into rectangle, is 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 are put in polytetrafluoroethylene (PTFE) bottle；
(2) KMnO is configured4Solution；
(3) KMnO of 20mL is taken4Solution is added into being placed in the polytetrafluoroethylene (PTFE) bottle of graphite paper into step (1), then
The bottle is put into stainless steel water heating kettle again, is sealed, reaction；
(4) it waits for after reaction, reaction kettle being allowed to naturally cool to room temperature, the graphite paper after reaction is washed into 4-5 through deionized water
It is secondary, it is dry in 60 DEG C of baking ovens, obtain MnOx/ GP electrodes；
(5) MnO for obtaining step (4)x/ GP electrodes, which are placed in HCL solution, stands 30min, until the manganese on graphite paper surface aoxidizes
Object dissolving is complete, then with deionized water scouring stone ink paper 4-5 times, is placed on 60 DEG C of drying in oven at least 6h, obtains more
Hole graphite paper electrode.
2. the preparation method of porous graphite paper according to claim 1, which is characterized in that rectangular described in step (1)
The area of shape is not less than 1cm2。
3. the preparation method of porous graphite paper according to claim 1, which is characterized in that KMnO in step (2)4Solution
A concentration of 0.01-2mol L-1。
4. the preparation method of porous graphite paper according to claim 1, which is characterized in that the temperature reacted in step (3)
It is 120-160 DEG C；The time of reaction is 4-16h.
5. the preparation method of porous graphite paper according to claim 1, which is characterized in that the dry time in step (4)
For 0.1-12h.
6. the preparation method of porous graphite paper according to claim 1, which is characterized in that HCL solution is dense in step (5)
Degree is 3-10molL-1。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711385674.8A CN108273495B (en) | 2017-12-20 | 2017-12-20 | Preparation method of multi-pore-passage graphite paper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711385674.8A CN108273495B (en) | 2017-12-20 | 2017-12-20 | Preparation method of multi-pore-passage graphite paper |
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| Publication Number | Publication Date |
|---|---|
| CN108273495A true CN108273495A (en) | 2018-07-13 |
| CN108273495B CN108273495B (en) | 2020-08-18 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1724861A1 (en) * | 2005-05-17 | 2006-11-22 | Nicholas M. Abson | Novel materials for alkaline electrolysers and alkaline fuel cells |
| US20090185327A1 (en) * | 2008-01-17 | 2009-07-23 | Fraser Wade Seymour | Composite electrode comprising a carbon structure coated with a thin film of mixed metal oxides for electrochemical energy storage |
| CN102757036A (en) * | 2011-04-26 | 2012-10-31 | 海洋王照明科技股份有限公司 | Preparation method of porous graphene |
| CN103854876A (en) * | 2013-12-23 | 2014-06-11 | 燕山大学 | Preparation method for self-supporting graphene-manganese oxide composite electrode materials |
| CN104261387A (en) * | 2014-09-16 | 2015-01-07 | 中山大学 | Method for large-area preparation of graphene based carbon paper and graphene based carbon paper prepared thereby |
| US20160240841A1 (en) * | 2015-02-18 | 2016-08-18 | Hui He | Pre-sulfurized cathode for alkali metal-sulfur secondary battery and production process |
-
2017
- 2017-12-20 CN CN201711385674.8A patent/CN108273495B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1724861A1 (en) * | 2005-05-17 | 2006-11-22 | Nicholas M. Abson | Novel materials for alkaline electrolysers and alkaline fuel cells |
| US20090185327A1 (en) * | 2008-01-17 | 2009-07-23 | Fraser Wade Seymour | Composite electrode comprising a carbon structure coated with a thin film of mixed metal oxides for electrochemical energy storage |
| CN102757036A (en) * | 2011-04-26 | 2012-10-31 | 海洋王照明科技股份有限公司 | Preparation method of porous graphene |
| CN103854876A (en) * | 2013-12-23 | 2014-06-11 | 燕山大学 | Preparation method for self-supporting graphene-manganese oxide composite electrode materials |
| CN104261387A (en) * | 2014-09-16 | 2015-01-07 | 中山大学 | Method for large-area preparation of graphene based carbon paper and graphene based carbon paper prepared thereby |
| US20160240841A1 (en) * | 2015-02-18 | 2016-08-18 | Hui He | Pre-sulfurized cathode for alkali metal-sulfur secondary battery and production process |
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