CN108675291A - A kind of graphene oxide microwave reduction stripping off device - Google Patents
A kind of graphene oxide microwave reduction stripping off device Download PDFInfo
- Publication number
- CN108675291A CN108675291A CN201810772912.9A CN201810772912A CN108675291A CN 108675291 A CN108675291 A CN 108675291A CN 201810772912 A CN201810772912 A CN 201810772912A CN 108675291 A CN108675291 A CN 108675291A
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- boiler tube
- metal cavity
- gas
- mounting seat
- wall
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 38
- 230000009467 reduction Effects 0.000 title claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 40
- 239000002184 metal Substances 0.000 claims abstract description 40
- 239000007787 solid Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000007599 discharging Methods 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000005672 electromagnetic field Effects 0.000 abstract description 11
- 238000000034 method Methods 0.000 description 10
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000011343 solid material Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000004108 freeze drying Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- -1 oxygen Graphite alkene Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000007799 cork Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
-
- 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
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a kind of graphene oxide microwave reduction stripping off devices, include being made of microwave wave transparent heat-resisting material and vertical boiler tube, metal cavity, gas-solid mixing three-way pipe, inlet suction port, inlet connector, discharge connector, microwave source, wherein boiler tube is set in metal cavity, and the feed end of boiler tube stretches out metal cavity bottom and is connected with gas-solid mixing three-way pipe, the other both ends of gas-solid mixing three-way pipe are connected separately with inlet suction port and inlet connector, and inlet suction port is located at gas-solid mixing threeway bottom of the tube, inlet connector is located at gas-solid mixing three-way pipe side, the discharge end of boiler tube stretches out at the top of metal cavity and is connected with discharging connector, metal cavity outer wall is provided with microwave source.Material enters from inlet connector in boiler tube, gas enters from intake interface and is delivered up material suspended, it is coupled into the material in boiler tube with the electromagnetic field in boiler tube, realizes the stripping and reduction of graphene oxide, complete the graphene of stripping reduction and flowed out from discharging connector.
Description
Technical field
The present invention relates to graphene lift-off technology fields, more specifically, it relates to a kind of graphene oxide microwave reduction
Stripping off device.
Background technology
Graphene (Graphene) be one kind by carbon atom with sp2Hybridized orbit forms the two dimension that hexangle type is in honeycomb lattice
Carbon nanomaterial.
Graphene have excellent optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and
Drug delivery etc. is with important application prospects, it is considered to be a kind of future revolutionary material.
The main mode of production of graphene has mechanical stripping method, oxidation-reduction method, SiC epitaxial growth methods and chemistry at this stage
Vapour deposition process (CVD).
Oxidation-reduction method is by using the oxidants such as the chemical reagent such as sulfuric acid, nitric acid and potassium permanganate, hydrogen peroxide by day
Right graphite oxidation increases the spacing between graphite linings, oxide is inserted between layers in graphite, and graphite oxide is made
(Graphite Oxide).Then reactant is washed, and low temperature drying is carried out to the solid after cleaning, oxidation stone is made
Ink powder body.Graphite oxide powder is removed by the methods of physics stripping, high-temperature expansion, graphene oxide is made.Finally
Graphene oxide is restored by chemical method, obtains graphene (RGO).This method and process is ripe, can obtain single layer or few
Layer graphene.
At this stage after graphite oxide powder is made in oxidizing process, ultrasonic wave stripping is carried out in hydrazine hydrate solution, obtains oxygen
Graphite alkene dispersion liquid is freeze-dried to prevent graphene oxide powder in drying process from reuniting in freeze drier；
The graphene oxide obtained after freeze-drying reduction in reduction furnace (general hydrogen furnace), removes oxygen-containing functional group, generates graphite
Alkene powder.
Presently, there are the problem of：
1, hydrazine hydrate has strong basicity and hygroscopicity, its energy attack glass, rubber, leather, cork etc. decompose at high temperature
At N2, NH3 and H2；Hydrazine hydrate solution has toxicity, harmful, not environmentally.Subsequent treatment cost is high.
2, ultrasonic wave splitting time is long, and efficiency is low.
3, peeling effect is poor, and the content that can reach single layer or few layer graphene is low.
4, the graphene oxide solution after removing is easy to reunite in the drying process, to prevent the group of graphene oxide powder
It is poly-, using freeze-drying.It is freeze-dried under the conditions of tangible cryogenic vacuum, makes the direct lyophilization of solution, drying cost is high, dry
Time is long, low output.
5, the graphene oxide that freeze-drying obtains contains a large amount of oxygen-containing functional group, need to react, remove through high temperature reduction
Oxygen-containing functional group typically now uses high-temperature hydrogen reduction stove.High energy consumption, anti-explosion safety grade are high.
6, entirely long from graphite oxide powder to graphene technological process, control node is more, graphene Manufacture quality control
Ensure that work is complicated.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide a kind of graphene oxide microwave reduction stripping
Device has the characteristics that production process is simple and needs to carry out the chemical substance of follow-up environmental protection treatment without addition addition.
To achieve the above object, the present invention provides following technical solutions：
A kind of graphene oxide microwave reduction stripping off device includes being made of microwave wave transparent heat-resisting material and vertical stove
Pipe, metal cavity, gas-solid mixing three-way pipe, inlet suction port, inlet connector, discharging connector, microwave source, wherein the boiler tube is set to
In the metal cavity, and the feed end of the boiler tube stretches out the metal cavity bottom and is connected with the gas-solid mixing threeway
Pipe, the other both ends of gas-solid mixing three-way pipe are connected separately with the inlet suction port and the inlet connector, and the air inlet
Connector is located at the gas-solid mixing threeway bottom of the tube, and the inlet connector is located at gas-solid mixing three-way pipe side, the stove
The discharge end of pipe stretches out at the top of the metal cavity and is connected with the discharging connector, and the metal cavity outer wall is provided with described
Microwave source.
By using above-mentioned technical proposal, it is located at microwave source outside metal cavity by microwave feed-in metal cavity, and
Electromagnetic field is established in metal cavity, and the boiler tube due to being arranged in metal cavity is made of microwave wave transparent heat-resisting material,
Electromagnetic field in metal cavity passes through furnace wall, electromagnetic field is established in boiler tube, material enters from inlet connector, and passes through gas-solid
Mixing tee pipe enters in boiler tube, and gas enters gas-solid mixing three-way pipe from intake interface, and since inlet suction port is located at gas
Gu mixing tee bottom of the tube, therefore solid material can be suspended and be delivered up, the electricity into the material and boiler tube in boiler tube
Magnetic field is coupled, and realizes the stripping and reduction of graphene oxide, is completed the graphene of stripping reduction and is flowed out from discharging connector.
Further, the boiler tube is hollow tubular structure small in ends, middle part is big.
By using above-mentioned technical proposal, the feed end of boiler tube is small-bore, can improve inlet suction port and enter under boiler tube
The air velocity at end improves the effect that solid material suspension is delivered up, is heavy caliber in the middle part of boiler tube, slows down boiler tube central region
Air velocity, increase solid material in boiler tube with the coupling time of electromagnetic field, the stripping of graphene oxide is better achieved
And reduction, the discharge end of boiler tube is small-bore, improves the air velocity of upper end in boiler tube, makes a concentrated effort to finish the graphene of stripping reduction
Transfer out the speed of boiler tube.
Further, boiler tube upper end outer wall is connected with upper mounting seat, the upper mounting seat and the metal cavity top
Wall connects, and the boiler tube lower end outer wall is connected with lower mounting seat, and the lower mounting seat is connect with the metal cavity bottom wall.
By using above-mentioned technical proposal, boiler tube upper and lower ends pass through upper mounting seat, lower mounting seat realization and metal respectively
At the top of the cavity and connection of bottom, realization boiler tube upper end passes through at the top of metal cavity, and boiler tube lower end passes through the effect of metal cavity.
Further, it is provided with positioning seal ring one between the boiler tube lower end and the lower mounting seat, for sealing
Gap between boiler tube lower end outer wall and the lower mounting seat inner wall is stated, positioning is provided between the boiler tube and the upper mounting seat
Sealing ring two, for sealing gap between boiler tube upper end outer wall and the upper mounting seat inner wall.
By using above-mentioned technical proposal, boiler tube feed end is realized by the way that positioning seal ring one and positioning seal ring two is arranged
The sealed connection of sealed connection and boiler tube discharge end and upper mounting seat with lower mounting seat.
Further, the boiler tube is made of quartz or ceramics.
By using above-mentioned technical proposal, quartz and ceramics all have good microwave wave transparent and heat safe effect.
In conclusion the invention has the advantages that：
1, by the way that boiler tube, metal cavity, gas-solid mixing three-way pipe, inlet suction port, inlet connector, discharging connector, micro- is arranged
Wave source plays the effect of stripping and the reduction of realizing graphene oxide；
2, by the way that boiler tube is arranged to hollow tubular structure small in ends, that middle part is big, the gas improved into boiler tube lower end is played
Flow velocity degree is to suspend the effect that is delivered up solid material.
Description of the drawings
Fig. 1 is that a kind of overall structure of the graphene oxide microwave reduction stripping off device of embodiment provided by the invention is shown
It is intended to.
In figure：1, metal cavity；2, boiler tube；3, lower mounting seat；4, positioning seal ring one；5, gas-solid mixing three-way pipe；6、
Inlet connector；7, inlet suction port；8, upper mounting seat；9, positioning seal ring two；10, discharge connector；11, microwave source.
Specific implementation mode
Embodiment：
Below in conjunction with attached drawing 1, invention is further described in detail.
A kind of graphene oxide microwave reduction stripping off device, as shown in Figure 1, including being made of microwave wave transparent heat-resisting material
And vertical boiler tube 2, metal cavity 1, gas-solid mixing three-way pipe 5, inlet suction port 7, inlet connector 6, discharging connector 10, microwave source
11, in the present embodiment, boiler tube 2 is made of quartz or ceramics.Wherein boiler tube 2 is set in metal cavity 1, and the charging of boiler tube 2
End stretches out 1 bottom of metal cavity and is connected with gas-solid mixing three-way pipe 5, and in the present embodiment, one end of gas-solid mixing three-way pipe 5 is inserted
Enter in boiler tube 2, prevents material from overflowing boiler tube 2.5 other both ends of gas-solid mixing three-way pipe are connected separately with inlet suction port 7 and charging
Connector 6, and inlet suction port 7 is located at 5 bottom of gas-solid mixing three-way pipe, inlet connector 6 is located at 5 side of gas-solid mixing three-way pipe, stove
The discharge end of pipe 2 stretches out 1 top of metal cavity and is connected with discharging connector 10, and 1 outer wall of metal cavity is provided with microwave source 11.This
In embodiment, microwave source 11 is produced using Chengdu water Sai En Electron Technology Co., Ltd and model WSPS-2450-100M
11 module of solid state microwave sources, and in the present embodiment, the frequency of microwave source 11 is 2450Hz.Inlet connector 6 be used for into boiler tube 2 into
Material, inlet suction port 7 are used for the air inlet into boiler tube 2, and the electromagnetic field that microwave source 11 generates is coupled with the material in boiler tube 2, realizes oxygen
The stripping and reduction of graphite alkene.
Wherein boiler tube 2 is hollow tubular structure small in ends, middle part is big.The feed end and discharge end of boiler tube 2 are small-bore, are carried
High solid material, which suspends, is delivered up and completes the effect for the graphene output boiler tube 2 that stripping restores, and 2 middle part of boiler tube is big mouth
Diameter can increase solid material in the interior coupling time with electromagnetic field of boiler tube 2.
2 upper end outer wall of boiler tube is connected with upper mounting seat 8, and upper mounting seat 8 is connect with 1 roof of metal cavity, boiler tube 2 and upper peace
It is provided with positioning seal ring 29 between dress seat 8, for sealing gap between 2 upper end outer wall of boiler tube and 8 inner wall of upper mounting seat, is led to
Cross the sealed connection that positioning seal ring 29 realizes boiler tube 2 discharge end and upper mounting seat 8.
2 lower end outer wall of boiler tube is connected with lower mounting seat 3, and lower mounting seat 3 is connect with 1 bottom wall of metal cavity, 2 lower end of boiler tube with
Positioning seal ring 1 is provided between lower mounting seat 3, between sealing between 3 inner wall of 2 lower end outer wall of boiler tube and lower mounting seat
Gap realizes the sealed connection of boiler tube 2 feed end and lower mounting seat 3 by the way that positioning seal ring 1 is arranged.
Operation principle：
Microwave source 11 outside metal cavity 1 is established in metal cavity 1 by microwave feed-in metal cavity 1
Electromagnetic field, the electromagnetic field in metal cavity 1 pass through 2 wall of boiler tube, establish electromagnetic field in boiler tube 2, material from inlet connector 6 into
Enter, and entered in boiler tube 2 by gas-solid mixing three-way pipe 5, gas enters gas-solid mixing three-way pipe 5 from intake interface, and will consolidate
State is material suspended to be delivered up, and is coupled into the material in boiler tube 2 with the electromagnetic field in boiler tube 2, realizes graphene oxide
Stripping and reduction, complete stripping reduction graphene simultaneously from discharging connector 10 flow out.
It should be noted that all statements for using " first " and " second " are for differentiation two in the embodiment of the present invention
The non-equal entity of a same names or non-equal parameter, it is seen that " first " " second " only for the convenience of statement, does not answer
It is interpreted as the restriction to the embodiment of the present invention, subsequent embodiment no longer illustrates this one by one.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, people in the art
Member can as needed make the present embodiment the modification of not creative contribution after reading this specification, but as long as at this
It is all protected by Patent Law in the right of invention.
Claims (5)
1. a kind of graphene oxide microwave reduction stripping off device, it is characterised in that：Including being made of microwave wave transparent heat-resisting material
And vertical boiler tube (2), metal cavity (1), gas-solid mixing three-way pipe (5), inlet suction port (7), inlet connector (6), discharging connect
Head (10), microwave source (11), wherein the boiler tube (2) is set in the metal cavity (1), and the feed end of the boiler tube (2)
It stretches out the metal cavity (1) bottom and is connected with the gas-solid mixing three-way pipe (5), the gas-solid mixing three-way pipe (5) is another
Outer both ends are connected separately with the inlet suction port (7) and the inlet connector (6), and the inlet suction port (7) is located at the gas
Mixing tee pipe Gu (5) bottom, the inlet connector (6) is located at gas-solid mixing three-way pipe (5) side, the boiler tube (2)
Discharge end stretch out at the top of the metal cavity (1) and be connected with the discharging connector (10), metal cavity (1) outer wall is set
It is equipped with the microwave source (11).
2. graphene oxide microwave reduction stripping off device according to claim 1, it is characterised in that：The boiler tube (2) is
Hollow tubular structure small in ends, middle part is big.
3. graphene oxide microwave reduction stripping off device according to claim 2, it is characterised in that：On the boiler tube (2)
End outer wall is connected with upper mounting seat (8), and the upper mounting seat (8) connect with the metal cavity (1) roof, the boiler tube (2)
Lower end outer wall is connected with lower mounting seat (3), and the lower mounting seat (3) connect with the metal cavity (1) bottom wall.
4. graphene oxide microwave reduction stripping off device according to claim 3, it is characterised in that：Under the boiler tube (2)
It is provided with positioning seal ring one (4) between end and the lower mounting seat (3), for sealing the boiler tube (2) lower end outer wall and institute
Gap between lower mounting seat (3) inner wall is stated, positioning seal ring two is provided between the boiler tube (2) and the upper mounting seat (8)
(9), for sealing gap between the boiler tube (2) upper end outer wall and the upper mounting seat (8) inner wall.
5. graphene oxide microwave reduction stripping off device according to claim 4, it is characterised in that：The boiler tube (2) by
Quartz or ceramics are made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810772912.9A CN108675291A (en) | 2018-07-14 | 2018-07-14 | A kind of graphene oxide microwave reduction stripping off device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810772912.9A CN108675291A (en) | 2018-07-14 | 2018-07-14 | A kind of graphene oxide microwave reduction stripping off device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108675291A true CN108675291A (en) | 2018-10-19 |
Family
ID=63813966
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810772912.9A Pending CN108675291A (en) | 2018-07-14 | 2018-07-14 | A kind of graphene oxide microwave reduction stripping off device |
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| Country | Link |
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| CN (1) | CN108675291A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110482535A (en) * | 2019-09-24 | 2019-11-22 | 大连海事大学 | A kind of method and device of liquid phase microwave plasma redox graphene |
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| CN110482535A (en) * | 2019-09-24 | 2019-11-22 | 大连海事大学 | A kind of method and device of liquid phase microwave plasma redox graphene |
| CN110482535B (en) * | 2019-09-24 | 2024-05-03 | 大连海事大学 | Method and device for reducing graphene oxide by liquid-phase microwave plasma |
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