CN108394894A - A kind of preparation facilities and its method of graphene oxide graphite electrode - Google Patents
A kind of preparation facilities and its method of graphene oxide graphite electrode Download PDFInfo
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- CN108394894A CN108394894A CN201810392199.5A CN201810392199A CN108394894A CN 108394894 A CN108394894 A CN 108394894A CN 201810392199 A CN201810392199 A CN 201810392199A CN 108394894 A CN108394894 A CN 108394894A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 46
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 39
- 239000010439 graphite Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims description 9
- 239000004575 stone Substances 0.000 claims abstract description 21
- 230000007246 mechanism Effects 0.000 claims abstract description 17
- 230000001105 regulatory effect Effects 0.000 claims abstract description 16
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 20
- 239000012286 potassium permanganate Substances 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000010790 dilution Methods 0.000 claims description 9
- 239000012895 dilution Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 244000137852 Petrea volubilis Species 0.000 claims description 8
- 229910021382 natural graphite Inorganic materials 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000000787 lecithin Substances 0.000 claims description 3
- 229940067606 lecithin Drugs 0.000 claims description 3
- 235000010445 lecithin Nutrition 0.000 claims description 3
- 238000006396 nitration reaction Methods 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000001737 promoting effect Effects 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5001—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with carbon or carbonisable materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The invention discloses a kind of preparation facilities of graphene oxide graphite electrode, including base station and water-bath, it is provided with water-bath at the top of the base station, supporting rod is vertically equipped at the top of the water-bath, it is arranged with regulating mechanism on the supporting rod, there are two the regulating mechanism is set, two described regulating mechanism one end are respectively connected with bracket, it is provided on the bracket of top on bracket described in magnetic stirring bar and bottom and is provided with beaker, the water-bath side is provided with closed cavity, the closed cavity side is provided with motor, the closed cavity inner cavity top is provided with cylinder, the cylinder head portions are connected with locating slot, the closed cavity madial wall is provided with geometrical clamp.The present invention enhances the electronic conductivity energy of graphite electrode by coating a layer graphene film on the surface of natural stone inker, and the electronic conductivity for solving existing graphite electrode can be poor, and complex production process, the problem of being unsuitable for promoting.
Description
Technical field
The present invention relates to graphite electrode production technical field, more particularly to the preparation of a kind of graphene oxide graphite electrode fills
It sets and its method.
Background technology
Graphene is a kind of and carbon atom connects the simple substance sublayer two dimensional crystal to be formed with SP2 hydridization, is substantially separation
Monoatomic layer graphite out.Univ Manchester UK scientist Geim and Novoselov in 2004 et al. have found to exist single
The two-dimensional graphene of lamella state.Graphene is made it have excellent due to its special two-dimentional monoatomic layer crystal structure characteristic
Calorifics, optics, electrically and mechanically performance, before the fields such as composite material, catalyst carrier and environment remediation are widely used
Scape.But the electronic conductivity of existing graphite electrode can be poor, and complex production process, is unsuitable for promoting.
Therefore, inventing preparation facilities and its method of a kind of graphene oxide graphite electrode, have very much must to solve the above problems
It wants.
Invention content
The purpose of the present invention is to provide a kind of preparation facilities and its method of graphene oxide graphite electrode, by day
The surface of right graphite rod coats a layer graphene film to enhance the electronic conductivity energy of graphite electrode, to solve above-mentioned background technology
The electronic conductivity of the existing graphite electrode of middle proposition can be poor, and complex production process, the problem of being unsuitable for promoting.
To achieve the above object, the present invention provides the following technical solutions：A kind of preparation dress of graphene oxide graphite electrode
It sets, including base station and water-bath, water-bath is provided at the top of the base station, supporting rod, institute are vertically equipped at the top of the water-bath
It states and is arranged with regulating mechanism on supporting rod, there are two the regulating mechanism is set, two described regulating mechanism one end are respectively connected with support
Frame is provided on bracket described in magnetic stirring bar and bottom on the bracket of top and is provided with beaker, the water-bath side
It is provided with closed cavity, the closed cavity side is provided with motor, and the closed cavity inner cavity top is provided with cylinder, described
Cylinder head portions are connected with locating slot, and the closed cavity madial wall is provided with geometrical clamp, the motor output shaft end and fixation
Folder is sequentially connected, and the closed cavity front is provided with lid, is connected by leaf hinge between the lid and closed cavity
It connects, the closed cavity bottom, which is run through, is equipped with straight slot, and the straight slot bottom cooperation is equipped with disposal box.
Preferably, the regulating mechanism is made of left adjusting block and right adjusting block, the left adjusting block and right adjusting block one
End junction is provided with shaft and the other end is both provided with convex block, is lived by shaft between the left adjusting block and right adjusting block
Dynamic connection, the convex block side of the left adjusting block end is welded with nut, the convex block of the left adjusting block and right adjusting block end
On be provided through regulation stud.
Preferably, the locating slot is shaped to arc, and sand paper is coated on the inside of the locating slot.
Preferably, it is provided with viewing window on the lid.
The present invention also provides a kind of preparation method of graphene oxide graphite electrode, specific preparation process is as follows：
Step 1：The preparation of graphene oxide：
（1）By the concentrated sulfuric acid：Concentrated phosphoric acid=9:1 proportioning prepares mixed acid solution, and be put into it is for use in totally dry beaker,
Meanwhile to weigh suitable potassium permanganate for use for electronic scale；
（2）Electronic scale, which weighs a certain amount of natural graphite powder and is placed in, to be washed repeatedly in dry large beaker, and will be above-mentioned
Nitration mixture is slowly poured into along wall of cup in the beaker for filling natural graphite powder；
（3）Above-mentioned mixed reactant is placed in water-bath, and starts to be slowly added to potassium permanganate, in the mistake that potassium permanganate is added
Cheng Zhong is always stirred the mixture in beaker with magnetic stirring bar；
（4）After potassium permanganate adds, beaker mouth is covered with one big filter paper, and reaction system is heated under conditions of 50 DEG C
6 hours；
（5）Continue that the hydrogen peroxide after dilution is added into mixture under conditions of 50 DEG C of heating stirrings, until solution colour is by black
Discoloration eventually becomes glassy yellow, and no longer until generation bubble at purplish；
（6）It after above-mentioned reaction system is continued under conditions of being placed in 50 DEG C heating stirring 3 hours, is cooled to room temperature, waits for that centrifugation is washed
Wash processing；
（7）The product of above-mentioned reaction system is placed in beaker plus water is diluted, and by the reaction product after dilution with
9000rpm centrifuges 3-5min, is filtered after carrying out five centrifuge washings；
（8）Above-mentioned filtration product is placed in drying in baking oven and obtains graphene oxide powder, it is spare；
Step 2：The preparation of graphite electrode：
（1）Natural stone inker is subjected to polishing 3-5 times using the sand paper of 200 mesh；
（2）First the natural stone inker after polishing is rinsed with clear water immediately, then with the ethyl alcohol after dilution to natural stone inker
It is cleaned by ultrasonic；
（3）Cleaned natural stone inker is air-dried spare；
Step 3：The coating film treatment of graphite electrode：
（1）The graphene oxide powder in step 1 is taken to prepare graphene oxide solution in right amount, and to graphene oxide solution
Middle addition surfactant, to reduce the surface tension and surface free energy of graphene oxide；
（2）Natural stone inker in step 2 is placed in graphene oxide solution after being soaked for a period of time, takes out naturally dry
It can be prepared by graphene oxide graphite electrode.
Preferably, the mass concentration of the concentrated sulfuric acid in the step 1 and concentrated phosphoric acid is respectively 98% and 85%, the dioxygen
The mass concentration of water is 1.5-5%.
Preferably, the mass ratio of potassium permanganate and natural graphite powder is 6 in the step 1:1.
Preferably, drying temperature is 60-110 DEG C in the step 1.
Preferably, the mass concentration of ethyl alcohol is 5% in the step 2.
Preferably, the surfactant used in the step 3 is stearic acid or lecithin, and its a concentration of 0.01mg/
ML, meanwhile, the time that natural stone inker impregnates is 10-50min.
The technique effect and advantage of the present invention：
1, by separately preparing natural stone inker and graphene oxide, and natural electrode table is made using infusion method
Bread covers one layer of graphene oxide membrane, enormously simplifies technique, enhances the electronic conductivity energy of graphite electrode；
2, by using existing simple production equipment, manufacturing process is simple, convenient for controlling, and also it is of low cost, it carries significantly
Its high economic feasibility.
Description of the drawings
Fig. 1 is the overall structure diagram of the present invention；
Fig. 2 is the regulating mechanism structural schematic diagram of the present invention；
Fig. 3 is the locating slot sectional view of the present invention；
Fig. 4 be in embodiment 2-4 drying temperature and soaking time to adhering to the influence tables of data of thickness；
In figure：1 base station, 2 water-baths, 3 supporting rods, 4 regulating mechanisms, 41 left adjusting blocks, 42 right adjusting blocks, 43 shafts, 44 convex blocks,
45 nuts, 46 regulation studs, 5 brackets, 6 magnetic stirring bars, 7 beakers, 8 closed cavities, 9 motors, 10 cylinders, 11 locating slots, 12
Sand paper, 13 geometrical clamps, 14 lids, 15 viewing windows, 16 straight slots, 17 disposal boxes.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1：
The present invention provides a kind of preparation facilities of graphene oxide graphite electrode as shown in Figs. 1-3, including base station 1 and water-bath
Pot 2,1 top of the base station are provided with water-bath 2, and 2 top of the water-bath is vertically equipped with supporting rod 3, is covered on the supporting rod 3
Equipped with regulating mechanism 4, there are two the regulating mechanism 4 is set, two 4 one end of the regulating mechanism are respectively connected with bracket 5, top institute
It states to be provided on bracket 5 on bracket 5 described in magnetic stirring bar 6 and bottom and is provided with beaker 7, the setting of 2 side of the water-bath
There are closed cavity 8,8 side of the closed cavity to be provided with motor 9,8 inner cavity top of the closed cavity is provided with cylinder 10, institute
It states 10 end of cylinder and is connected with locating slot 11,8 madial wall of the closed cavity is provided with geometrical clamp 13,9 output shaft of the motor
End and geometrical clamp 13 are sequentially connected, and 8 front of the closed cavity is provided with lid 14, the lid 14 and closed cavity 8 it
Between be connected by leaf hinge, 8 bottom of the closed cavity run through be equipped with straight slot 16,16 bottom of the straight slot cooperation be equipped with collection
Dirt case 17.
Further, in the above-mentioned technical solutions, the regulating mechanism 4 is made of left adjusting block 41 and right adjusting block 42,
The left adjusting block 41 and 42 one end junction of right adjusting block are provided with shaft 43 and the other end is both provided with convex block 44, described
It is flexibly connected by shaft 43 between left adjusting block 41 and right adjusting block 42,44 side of the convex block weldering of 41 end of left adjusting block
It is connected to nut 45, regulation stud 46 is provided through on the convex block 44 of 42 end of the left adjusting block 41 and right adjusting block, is convenient for
The height of bracket 5 is adjusted, to obtain best water-bath effect.
Further, in the above-mentioned technical solutions, the locating slot 11 is shaped to arc, 11 inside of the locating slot
It is coated with sand paper 12, it is possible to increase the contact area between sand paper and natural stone inker improves grinding efficiency.
Further, in the above-mentioned technical solutions, it is provided with viewing window 15 on the lid 14, it is internal natural convenient for observation
The polishing situation of graphite rod.
Embodiment 2：
The present invention also provides a kind of preparation method of graphene oxide graphite electrode, specific preparation process is as follows：
Step 1：The preparation of graphene oxide：
（1）It is respectively 98% and 85% concentrated sulfuric acid and concentrated phosphoric acid by mass concentration, by the concentrated sulfuric acid：Concentrated phosphoric acid=9:1 proportioning is matched
Mixed acid solution processed, and be put into totally dry beaker for use, meanwhile, it is for use that electronic scale weighs suitable potassium permanganate；
（2）Electronic scale, which weighs a certain amount of natural graphite powder and is placed in, to be washed repeatedly in dry large beaker, and will be above-mentioned
Nitration mixture is slowly poured into along wall of cup in the beaker for filling natural graphite powder；
（3）Above-mentioned mixed reactant is placed in water-bath, and starts to be slowly added to potassium permanganate, in the mistake that potassium permanganate is added
Cheng Zhong is always stirred the mixture in beaker with magnetic stirring bar；
（4）After potassium permanganate adds, beaker mouth is covered with one big filter paper, avoids impurity etc. from falling in beaker, and will be anti-
System is answered to be heated 6 hours under conditions of 50 DEG C；
（5）Continue that the hydrogen peroxide after dilution is added into mixture under conditions of 50 DEG C of heating stirrings, mass concentration is
1.5-5% eventually becomes glassy yellow, and no longer until generation bubble, in order to make until solution colour becomes purplish by black
System temperature is unlikely to become too high because hydrogen peroxide is added, and can first be inhaled a bit with syringe, then syringe needle is inserted into instead
It answers the bottom of system slowly to inject emitter, so that its temperature is unlikely to variation too many；
（6）It after above-mentioned reaction system is continued under conditions of being placed in 50 DEG C heating stirring 3 hours, is cooled to room temperature, waits for that centrifugation is washed
Wash processing；
（7）The product of above-mentioned reaction system is placed in beaker plus water is diluted, and by the reaction product after dilution with
9000rpm centrifuges 3-5min, is filtered after carrying out five centrifuge washings, and water need to be slowly added when being diluted, is avoided in reaction system
The unreacted concentrated sulfuric acid meets water and generates a large amount of heat, makes to obtain liquid boiling in reaction system and cause the accident；
（8）Above-mentioned filtration product is placed in drying in the baking oven that drying temperature is 60 DEG C and obtains graphene oxide powder, it is spare；
Step 2：The preparation of graphite electrode：
（1）Natural stone inker is subjected to polishing 3-5 times using the sand paper of 200 mesh；
（2）First the natural stone inker after polishing is rinsed with clear water immediately, then the second for being 5% with the mass concentration after dilution
Alcohol is cleaned by ultrasonic natural stone inker；
（3）Cleaned natural stone inker is air-dried spare；
Step 3：The coating film treatment of graphite electrode：
（1）The graphene oxide powder in step 1 is taken to prepare graphene oxide solution in right amount, and to graphene oxide solution
Middle addition stearic acid or lecithin, and the surfactant of its a concentration of 0.01mg/mL, to reduce the surface of graphene oxide
Power and surface free energy；
（2）Natural stone inker in step 2 is placed in graphene oxide solution after impregnating 10min, takes out naturally dry
Graphene oxide graphite electrode is made.
Embodiment 3：
As different from Example 2, in step 1（8）Drying temperature be 90 DEG C, and in step 3（2）Soaking time be
30min。
Embodiment 4：
Unlike equal from embodiment 2 and 3, in step 1（8）Drying temperature be 110 DEG C, and in step 3（2）Immersion when
Between be 50min.
Comparison according to embodiment 2-4 can obtain following data, be specifically shown in Figure of description 4.
From the data in the table, when drying temperature is 90 DEG C, the drying time of graphene oxide is relatively short, and when leaching
When the bubble time is 30min, the film thickness on natural stone inker surface reaches maximum.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (10)
1. a kind of preparation facilities of graphene oxide graphite electrode, including base station（1）And water-bath（2）, it is characterised in that：It is described
Base station（1）Top is provided with water-bath（2）, the water-bath（2）Top is vertically equipped with supporting rod（3）, the supporting rod（3）On
It is arranged with regulating mechanism（4）, the regulating mechanism（4）There are two if, two regulating mechanisms（4）One end is respectively connected with bracket
（5）, the top bracket（5）On be provided with magnetic stirring bar（6）And bracket described in bottom（5）On be provided with beaker（7）, institute
State water-bath（2）Side is provided with closed cavity（8）, the closed cavity（8）Side is provided with motor（9）, the closing chamber
Body（8）Inner cavity top is provided with cylinder（10）, the cylinder（10）End is connected with locating slot（11）, the closed cavity（8）
Madial wall is provided with geometrical clamp（13）, the motor（9）Output shaft end and geometrical clamp（13）It is sequentially connected, the closed cavity
（8）Front is provided with lid（14）, the lid（14）With closed cavity（8）Between be connected by leaf hinge, the envelope
Closed chamber body（8）Bottom, which is run through, is equipped with straight slot（16）, the straight slot（16）Bottom cooperation is equipped with disposal box（17）.
2. a kind of preparation facilities of graphene oxide graphite electrode according to claim 1, it is characterised in that：The adjusting
Mechanism（4）By left adjusting block（41）With right adjusting block（42）Composition, the left adjusting block（41）With right adjusting block（42）One end connects
The place of connecing is provided with shaft（43）And the other end is both provided with convex block（44）, the left adjusting block（41）With right adjusting block（42）It
Between pass through shaft（43）Flexible connection, the left adjusting block（41）The convex block of end（44）Side is welded with nut（45）, described
Left adjusting block（41）With right adjusting block（42）The convex block of end（44）On be provided through regulation stud（46）.
3. a kind of preparation facilities of graphene oxide graphite electrode according to claim 1, it is characterised in that：The positioning
Slot（11）It is shaped to arc, the locating slot（11）Inside is coated with sand paper（12）.
4. a kind of preparation facilities of graphene oxide graphite electrode according to claim 1, it is characterised in that：The lid
（14）On be provided with viewing window（15）.
5. a kind of preparation method of graphene oxide graphite electrode according to any one of claim 1-4, specific to make
It is standby that steps are as follows：
Step 1：The preparation of graphene oxide：
By the concentrated sulfuric acid：Concentrated phosphoric acid=9:1 proportioning prepares mixed acid solution, and be put into it is for use in totally dry beaker, together
When, it is for use that electronic scale weighs suitable potassium permanganate；
Electronic scale, which weighs a certain amount of natural graphite powder and is placed in, to be washed repeatedly in dry large beaker, and by above-mentioned nitration mixture
It is slowly poured into along wall of cup in the beaker for filling natural graphite powder；
Above-mentioned mixed reactant is placed in water-bath, and starts to be slowly added to potassium permanganate, in the process that potassium permanganate is added
In, the mixture in beaker is stirred with magnetic stirring bar always；
After potassium permanganate adds, beaker mouth is covered with one big filter paper, and it is small that reaction system is heated under conditions of 50 DEG C to 6
When；
Continue that the hydrogen peroxide after dilution is added into mixture under conditions of 50 DEG C of heating stirrings, until solution colour is become by black
At purplish, glassy yellow is eventually become, and no longer until generation bubble；
After above-mentioned reaction system is continued under conditions of being placed in 50 DEG C heating stirring 3 hours, it is cooled to room temperature, waits at centrifuge washing
Reason；
The product of above-mentioned reaction system is placed in beaker plus water is diluted, and by the reaction product after dilution with 9000rpm
3-5min is centrifuged, is filtered after carrying out five centrifuge washings；
Above-mentioned filtration product is placed in drying in baking oven and obtains graphene oxide powder, it is spare；
Step 2：The preparation of graphite electrode：
Natural stone inker is subjected to polishing 3-5 times using the sand paper of 200 mesh；
First the natural stone inker after polishing is rinsed with clear water immediately, then natural stone inker is carried out with the ethyl alcohol after dilution
It is cleaned by ultrasonic；
Cleaned natural stone inker is air-dried spare；
Step 3：The coating film treatment of graphite electrode：
It takes the graphene oxide powder in step 1 to prepare graphene oxide solution in right amount, and adds into graphene oxide solution
Enter surfactant, to reduce the surface tension and surface free energy of graphene oxide；
Natural stone inker in step 2 is placed in graphene oxide solution after being soaked for a period of time, takes out naturally dry
Graphene oxide graphite electrode is made.
6. a kind of preparation method of graphene oxide graphite electrode according to claim 5, it is characterised in that：The step
The mass concentration of the concentrated sulfuric acid and concentrated phosphoric acid in one is respectively 98% and 85%, and the mass concentration of the hydrogen peroxide is 1.5-5%.
7. a kind of preparation method of graphene oxide graphite electrode according to claim 5, it is characterised in that：The step
The mass ratio of potassium permanganate and natural graphite powder is 6 in one:1.
8. a kind of preparation method of graphene oxide graphite electrode according to claim 5, it is characterised in that：The step
Drying temperature is 60-110 DEG C in one.
9. a kind of preparation method of graphene oxide graphite electrode according to claim 5, it is characterised in that：The step
The mass concentration of ethyl alcohol is 5% in two.
10. a kind of preparation method of graphene oxide graphite electrode according to claim 5, it is characterised in that：The step
The surfactant used in rapid three is stearic acid or lecithin, and its a concentration of 0.01mg/mL, meanwhile, the leaching of natural stone inker
The time of bubble is 10-50min.
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