CN109761232A - A kind of device and method preparing compound between graphite layers - Google Patents
A kind of device and method preparing compound between graphite layers Download PDFInfo
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- CN109761232A CN109761232A CN201910242215.7A CN201910242215A CN109761232A CN 109761232 A CN109761232 A CN 109761232A CN 201910242215 A CN201910242215 A CN 201910242215A CN 109761232 A CN109761232 A CN 109761232A
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- quartz ampoule
- sulfuric acid
- graphite
- porous electrode
- graphite layers
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 80
- 239000010439 graphite Substances 0.000 title claims abstract description 80
- 150000001875 compounds Chemical class 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000003708 ampul Substances 0.000 claims abstract description 54
- 239000010453 quartz Substances 0.000 claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000007789 gas Substances 0.000 claims abstract description 53
- 239000011261 inert gas Substances 0.000 claims abstract description 20
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000003487 electrochemical reaction Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000002687 intercalation Effects 0.000 claims description 18
- 238000009830 intercalation Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000012670 alkaline solution Substances 0.000 claims description 7
- 238000001962 electrophoresis Methods 0.000 claims description 6
- 239000003595 mist Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 230000000505 pernicious effect Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 8
- 229910052717 sulfur Inorganic materials 0.000 description 7
- 239000011593 sulfur Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The invention discloses a kind of device and method for preparing compound between graphite layers, which includes sulfuric acid gas generating unit, electrochemical reaction appts, inert gas feedway and sulfuric acid gas treatment equipment；Electrochemical reaction appts include quartz ampoule, two porous electrode plates and power supply；Two porous electrode plates are arranged in parallel in quartz ampoule, two porous electrode plate in-planes and quartz ampoule it is axially vertical, graphite raw material is fixed on the porous electrode plate connecting with positive pole；The gas outlet of inert gas feedway is connected with the air inlet of quartz ampoule；Sulfuric acid gas generating unit includes sulfur trioxide gas body feeding and water vapor generation device, and the outlet of sulfuric acid gas generating unit is extend among two electrode plates, and the gas outlet of quartz ampoule is connected with the air inlet of sulfuric acid gas treatment equipment.Present invention reduces the consumptions of sulfuric acid in compound between graphite layers preparation process, save the preparation cost, and reduce the pollution level to environment.
Description
Technical field
The present invention relates to machining graphite technical fields, more particularly to a kind of device for preparing compound between graphite layers and side
Method.
Background technique
Graphite is the important strategic resource in China.Expanded graphite is one of the important directions of graphite finely processed product.Graphite
In crystal, between layers apart from larger, about 0.335nm is combined with Van der Waals force.Under felicity condition, natural scale stone
Ink can be by either physically or chemically, in graphite flake Intercalation reaction intercalation agent molecule, forming compound between graphite layers, also referred to as may be used
Expanded graphite.When being placed in high temperature, the compound of Intercalation reaction is heated to be decomposed rapidly, is generated gas, is kept graphite swollen along C axis direction
It is swollen, form expanded graphite.
Expanded graphite has the characteristics such as good absorption, corrosion-resistant, high temperature resistant because of unique network-like microcellular structure.It is swollen
Swollen graphite and its product use temperature range are wide, excellent elasticity and compressibility can be kept under high temperature and cryogenic conditions, extensively
It is general to be used to manufacture flexible graphite article, environmental-protection adsorption material, high-energy battery electrode material, applied fireproofing, biological medicine material
Material and sealing material etc..
The intercalation effect of expansible graphite is the key that influence flexible graphite article and graphite adsorbent material performance, it is existing can
The preparation method of expanded graphite can be divided into chemical oxidization method, electrochemical process, explosion method and vapor phase grafting etc., wherein chemical oxidation
Method is using natural flake graphite as raw material, and hydrogen peroxide etc. is oxidant, and the concentrated sulfuric acid is that main intercalator carries out intercalation.Obtained
Compound between graphite layers are expanded in high temperature furnace or micro-wave oven.Expansion is since compound between graphite layers are met in high temperature furnace
The gas that decomposes immediately of heat instantaneously volatilizees the pressure of generation, overcomes Van der Waals force to push graphite level along C axis direction open, makes graphite
Piece thickness high power expansion, to form expanded graphite.There are prepared expanded graphite sulfur content height, sulfuric acid consumption for this method
Greatly, at high cost, intercalation effect is bad, intercalation order be difficult to control and environmental pollution it is big the problems such as.
Summary of the invention
The object of the present invention is to provide a kind of device and methods for preparing compound between graphite layers, to reduce graphite layers
The consumption of sulfuric acid when closing the sulfur content of object and preparing compound between graphite layers, reduces the dirt to environment while reducing cost
Dye.
To achieve the above object, the present invention provides following schemes:
The invention discloses a kind of devices for preparing compound between graphite layers, including sulfuric acid gas generating unit, electrochemistry
Reaction unit, inert gas feedway and sulfuric acid gas treatment equipment；
The electrochemical reaction appts include quartz ampoule, two porous electrode plates and power supply；Two porous electrode plates
It is arranged in parallel that two porous electrode plate in-planes are axially vertical with the quartz ampoule in the quartz ampoule,
Graphite raw material is fixed on the porous electrode plate connecting with the positive pole；The both ends of the quartz ampoule be respectively air inlet and
The gas outlet of gas outlet, the inert gas feedway is connected with the air inlet of the quartz ampoule；
The sulfuric acid gas generating unit includes sulfur trioxide gas body feeding and water vapor generation device, the sulfuric acid
The outlet of gas generating unit is extend among two porous electrode plates by the air inlet of the quartz ampoule, the quartz ampoule
Gas outlet be connected with the air inlet of the sulfuric acid gas treatment equipment.
Optionally, the device for preparing compound between graphite layers further includes heating device, and the heating device will be described
Quartz ampoule is heated to 105 DEG C~800 DEG C.
Optionally, the power supply is D.C. regulated power supply, and the voltage of the D.C. regulated power supply is adjustable, and the direct current is steady
Voltage source provides operating voltage for two porous electrode plates.
Optionally, the sulfuric acid gas treatment equipment includes alkaline solution, for absorbing the quartz ampoule gas outlet discharge
Sulfuric acid vapor.
Optionally, the graphite raw material is crystalline flake graphite.
The invention also discloses a kind of methods for preparing compound between graphite layers, are applied to above-mentioned preparation graphite layers chemical combination
The device of object, which comprises
Two porous electrode plates axially vertical with the quartz ampoule are set in quartz ampoule, graphite raw material is fixed on and
On the connected porous electrode plate of positive pole；
Two porous electrode plate middle positions are passed through in the quartz ampoule is given birth to by sulfur trioxide gas and vapor
At sulfuric acid mist；
Apply operating voltage on the porous electrode plate；
The sulfuric acid mist occurs ionization and electrophoresis and intercalation occurs under the operating voltage driving effect；It is described
After intercalation, the air inlet of Xiang Suoshu quartz ampoule is passed through inert gas, and the inert gas will be in the quartz ampoule
Remaining pernicious gas carries in alkaline solution.
Optionally, the graphite raw material is crystalline flake graphite.
Optionally, the quartz ampoule is heated, makes 105 DEG C~800 DEG C of temperature of the quartz ampoule.
The summary of the invention provided according to the present invention, the invention discloses following technical effects: the present invention provides a kind of prepare
Sulfuric acid molecule is passed through by the device and method of compound between graphite layers with sulfuric acid vapor state, sulfuric acid gas point in sulfuric acid vapor
Son ionization is that the hydrogen sulfate ion and hydrogen ion of small grain size realize hydrogen sulfate ion by electrostatic attraction and concentration difference
Electrophoresis motion and graphite layers orient be inserted into, and can by the regulation of voltage, realize intercalation order control and insert
The raising of layer effect；Using the in-situ preparation of sulfuric acid vapor, the presence of extra sulfuric acid molecule in the reaction system is reduced as far as possible
With residual, and the sulfur content of product is reduced, so that it is more applicable for certain sulfur content and require lower high-end applications occasion, together
When reduce preparation cost and the pollution level to environment.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is a kind of apparatus structure schematic diagram for preparing compound between graphite layers of the embodiment of the present invention；
Fig. 2 is a kind of method flow schematic diagram for preparing compound between graphite layers of the embodiment of the present invention.
Specific embodiment
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 description, 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.
The object of the present invention is to provide a kind of device and methods for preparing compound between graphite layers, reduce graphite layers chemical combination
The sulfur content of object and when preparing compound between graphite layers sulfuric acid consumption, to reduce cost and reduce environmental pollution.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
Fig. 1 is a kind of apparatus structure schematic diagram for preparing compound between graphite layers of the embodiment of the present invention, as shown in Figure 1, this
Invent a kind of device for preparing compound between graphite layers provided, comprising: sulfuric acid gas generating unit 102, electrochemical reaction dress
Set 101, inert gas feedway 103 and sulfuric acid gas treatment equipment 104；
Electrochemical reaction appts 101 include quartz ampoule, two porous electrode plates and power supply；Two porous electrode plates are mutually flat
Row is arranged in quartz ampoule, axially vertical, the crystalline flake graphite raw material to be reacted of two porous electrode plate in-planes and quartz ampoule
It is fixed on the porous electrode plate being connect with positive pole；The both ends of quartz ampoule are respectively air inlet and air outlet, inert gas
The gas outlet of feedway is connected with the air inlet of quartz ampoule；
Sulfuric acid gas generating unit 102 includes sulfur trioxide gas body feeding and water vapor generation device, sulfuric acid gas
The outlet of generating device 102 is extend among two porous electrode plates by the air inlet of quartz ampoule, the gas outlet of quartz ampoule and sulphur
The air inlet of acid gas processing unit 104 is connected.
The device for preparing compound between graphite layers further includes heating device, heating device by quartz ampoule be heated to 105 DEG C~
800℃。
Power supply is D.C. regulated power supply, and the voltage of D.C. regulated power supply is adjustable, provides work for two porous electrode plates
Voltage provides driving force for the electrophoresis of sulfuric acid vapor and the intercalation of graphite.
Sulfuric acid gas treatment equipment 104 includes alkaline solution, for absorbing the sulfuric acid vapor of quartz ampoule gas outlet discharge.
Inert gas feedway 103 provides stable inert gas for quartz ampoule, after intercalation, to electrochemistry
Reaction unit is passed through stable inert gas, and the exhaust gas that inert gas carries in electrochemical reaction appts is all passed through at sulfuric acid gas
Manage device 104.
The present invention also provides a kind of method for preparing compound between graphite layers, this method is applied to above-mentioned preparation graphite linings
Between compound device, Fig. 2 is a kind of method flow schematic diagram for preparing compound between graphite layers of the present invention, as shown in Fig. 2, should
Method includes:
Step 201: two porous electrode plates axially vertical with quartz ampoule being set in quartz ampoule, graphite raw material is fixed
On the porous electrode plate being connected with positive pole；
Step 202: two porous electrode plate middle positions are passed through in quartz ampoule is given birth to by sulfur trioxide gas and vapor
At sulfuric acid mist；
Step 203: applying operating voltage on porous electrode plate；
Step 204: sulfuric acid mist occurs ionization and electrophoresis and intercalation occurs under operating voltage driving effect；Intercalation
After reaction, it is passed through inert gas to the air inlet of quartz ampoule, inert gas carries the remaining pernicious gas in quartz ampoule
Enter in alkaline solution
Wherein, step 202 further includes heating to quartz ampoule, makes 105 DEG C~800 DEG C of temperature of quartz ampoule.
Wherein, step 204 is specific further include: sulfuric acid vapor occurs ionization and generates hydrogen sulfate ion and hydrogen ion；Sulfuric acid
Hydrogen radical ion and is fixed on porous electrode plate because electrostatic attraction and concentration difference are mobile to the porous electrode plate being connected with positive pole
On graphite raw material contact；Under the driving of operating voltage, hydrogen sulfate ion enters graphite layers and obtains graphite layers chemical combination
Object；
It is passed through inert gas to electrochemical reaction appts after acquisition compound between graphite layers, it will be in electrochemical reaction appts
Exhaust gas, mainly sulfuric acid vapor carry in alkaline solution.
The present invention provides a kind of device and method for preparing compound between graphite layers, and sulfuric acid is led to sulfuric acid vapor state
Enter, the ionization of sulfuric acid gas molecule is the hydrogen sulfate ion and hydrogen ion of small grain size in sulfuric acid vapor, by electrostatic attraction and dense
It is poor to spend, and realizes the electrophoresis motion of hydrogen sulfate ion and is inserted into the orientation of graphite layers, and can pass through the tune of voltage
The control of intercalation order and the raising of intercalation effect are realized in control；Using the in-situ preparation of sulfuric acid vapor, it is extra to reduce as far as possible
The presence of sulfuric acid molecule in the reaction system, and the sulfur content of product is reduced, so that it is more applicable for certain sulfur content requirements
Lower high-end applications occasion, while reducing preparation cost and the pollution level to environment.The present invention is supplied by inert gas
Device and sulfuric acid gas treatment absorption plant realize that the absorption to sulfuric acid gas is handled, relative to the tradition using the liquid concentrated sulfuric acid
The treating capacity of method, this method Waste Sulfuric Acid is smaller and treatment effeciency is high.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.
Used herein a specific example illustrates the principle and implementation of the invention, and above embodiments are said
It is bright to be merely used to help understand method and its core concept of the invention；At the same time, for those skilled in the art, foundation
Thought of the invention, there will be changes in the specific implementation manner and application range.In conclusion the content of the present specification is not
It is interpreted as limitation of the present invention.
Claims (8)
1. a kind of device for preparing compound between graphite layers, which is characterized in that including sulfuric acid gas generating unit, electrochemical reaction
Device, inert gas feedway and sulfuric acid gas treatment equipment；
The electrochemical reaction appts include quartz ampoule, two porous electrode plates and power supply；Two porous electrode plates are mutual
It is arranged in parallel in the quartz ampoule, axially vertical, the graphite of two the porous electrode plate in-planes and the quartz ampoule
Raw material is fixed on the porous electrode plate connecting with the positive pole；The both ends of the quartz ampoule are respectively air inlet and outlet
Mouthful, the gas outlet of the inert gas feedway is connected with the air inlet of the quartz ampoule；
The sulfuric acid gas generating unit includes sulfur trioxide gas body feeding and water vapor generation device, the sulfuric acid gas
The outlet of generating device is extend among two porous electrode plates by the air inlet of the quartz ampoule；The quartz ampoule goes out
Port is connected with the air inlet of the sulfuric acid gas treatment equipment.
2. the device according to claim 1 for preparing compound between graphite layers, which is characterized in that it further include heating device,
The quartz ampoule is heated to 105 DEG C~800 DEG C by the heating device.
3. the device according to claim 1 for preparing compound between graphite layers, which is characterized in that the power supply is that direct current is steady
The voltage of voltage source, the D.C. regulated power supply is adjustable, and the D.C. regulated power supply provides for two porous electrode plates
Operating voltage.
4. the device according to claim 1 for preparing compound between graphite layers, which is characterized in that the sulfuric acid gas treatment
Device includes alkaline solution, for absorbing the sulfuric acid vapor of the quartz ampoule gas outlet discharge.
5. the device according to claim 1 for preparing compound between graphite layers, which is characterized in that the graphite raw material is squama
Piece graphite.
6. a kind of method for preparing compound between graphite layers, which is characterized in that be applied to the described in any item systems of claim 1-5
The device of standby compound between graphite layers, which comprises
Two porous electrode plates axially vertical with the quartz ampoule are set in quartz ampoule, graphite raw material is fixed on and power supply
On the connected porous electrode plate of anode；
Two porous electrode plate middle positions are passed through generated by sulfur trioxide gas and vapor in the quartz ampoule
Sulfuric acid mist；
Apply operating voltage on the porous electrode plate；
The sulfuric acid mist occurs ionization and electrophoresis and intercalation occurs under the operating voltage driving effect；The intercalation
After reaction, the air inlet of Xiang Suoshu quartz ampoule is passed through inert gas, and the inert gas is by the remnants in the quartz ampoule
Pernicious gas carries in alkaline solution.
7. the method according to claim 6 for preparing compound between graphite layers, which is characterized in that the graphite raw material is squama
Piece graphite.
8. the method according to claim 6 for preparing compound between graphite layers, which is characterized in that carried out to the quartz ampoule
Heating, makes 105 DEG C~800 DEG C of temperature of the quartz ampoule.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910242215.7A CN109761232B (en) | 2019-03-28 | 2019-03-28 | Device and method for preparing graphite intercalation compound |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910242215.7A CN109761232B (en) | 2019-03-28 | 2019-03-28 | Device and method for preparing graphite intercalation compound |
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| CN109761232B CN109761232B (en) | 2020-09-25 |
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