CN107128896A - A kind of fluorographite pipe reaction stove - Google Patents
A kind of fluorographite pipe reaction stove Download PDFInfo
- Publication number
- CN107128896A CN107128896A CN201710582071.0A CN201710582071A CN107128896A CN 107128896 A CN107128896 A CN 107128896A CN 201710582071 A CN201710582071 A CN 201710582071A CN 107128896 A CN107128896 A CN 107128896A
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- heater
- fluorographite
- filter layer
- reaction
- reaction chamber
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The present invention is related to a kind of fluorographite pipe reaction stove, and it includes body of heater, is followed successively by gas mixer chamber, lower filter layer, reaction chamber and upper filter layer in the body of heater from down to up;The gas mixer chamber bottom is respectively equipped with nitrogen inlet and fluorine gas import;The lower filter layer and upper filter layer are sintering sieves;Heater is provided with the outside of the reaction chamber;Atmospheric valve is provided with the top of the body of heater.Graphite of the present invention and fluorine gas are more abundant, and fluorination efficiency is high.Graphite is arbitrarily stacked in reacting furnace, adds graphite linings thickness, and reaction chamber utilization rate is high, is improved per furnace output.In production process, after per stove, fluorination is finished, discharging and replacing virgin material feed supplement process, body of heater need not stop heating.Realize that not blowing out is continuously produced, improve operating efficiency.
Description
Technical field
The invention belongs to technical field of fluorine chemical industry, and in particular to a kind of in production fluorographite technique, for converting
Produce the fluorographite pipe reaction stove of fluorographite.
Background technology
In current industrial production, the preparation method of fluorographite is mainly fluorine gas and fluorine is carried out in high temperature reaction stove with graphite
Change reaction.Existing Graphite fluorination reacting furnace is horizontal chamber furnace (oven), and raw graphite is to spread out to be placed in pipe, and reactor has heater,
Raw material is heated to require temperature.Fluorine gas enters from one end, reacts generation fluorographite at high temperature with graphite.The reacting furnace is deposited
In problems with:1) fluorine gas conversion ratio is not high, is placed due to horizontal, fluorine gas passes through from graphite linings upper space, only with graphite table
Layer contact, occurs fluorination reaction.Quite a few fluorine gas is not reached with raw material, is just removed from gas-phase space, is reduced fluorine gas
Conversion ratio.2) reacting furnace utilization rate is not high, terminates from fluorination reaction in terms of rear reaction effect, is deposited in the generation fluorographite on upper strata
Color is whiter, because lower floor does not reach, or contact fluorine gas is less, and the fluorographite color of generation is more grey or even black.Therefore,
In order to ensure product quality, reacting furnace is in placing graphite, it is desirable to which the graphite linings thickness of laying is as relatively thin as possible, causes reaction
Space availability ratio is not high in chamber, and reaction furnace output is difficult to be lifted.3) it is cumbersome to be required due to feed product graphite in stove
Thin layer is placed, therefore the form reacting furnace can only carry out gap operating., it is necessary to first stop heating when changing raw material per stove,
Take charge door flange apart, reaction boat is taken out, product is laid down, meticulous by raw graphite, very thin is laid in reaction boat, then
Reaction boat is reentered into fluorination stove, fluorine gas carries out fluorination reaction with graphite in reaction boat.It is cumbersome, inefficiency.
The content of the invention
The purpose of the present invention is that there is provided a kind of fluorographite tubular type of new structure for existing Graphite fluorination stove not enough
Reacting furnace, makes it compared with legacy equipment, it is possible to increase the conversion ratio of raw material, improves utilization rate of equipment and installations, while improving graphite
The operating efficiency of fluorination reaction stove, so as to be effectively reduced the production cost of fluorographite.
The object of the invention to solve the technical problems is also realized using following technical scheme.According to proposed by the present invention
A kind of fluorographite pipe reaction stove, it includes body of heater, is followed successively by gas mixer chamber 16, lower filter layer in the body of heater from down to up
15th, reaction chamber 6 and upper filter layer 7;The bottom of gas mixer chamber 16 is respectively equipped with nitrogen inlet 2 and fluorine gas import 1;Institute
It is sintering sieves to state lower filter layer 15 and upper filter layer 7;The outside of reaction chamber 6 is provided with heater 5;The body of heater top
Portion is provided with atmospheric valve 10.
The purpose of the present invention and solve its technical problem and can also be further achieved by the following technical measures.
Foregoing fluorographite pipe reaction stove, wherein mouth 12 is added in the described top of reaction chamber 6 provided with raw material, the original
Material, which is added, is provided with control valve at mouth 12.
Foregoing fluorographite pipe reaction stove, wherein described raw material, which is added between the mouth of pipe and body of heater of mouth 12, inclination angle,
45 ° of inclination angle best angle.
Foregoing fluorographite pipe reaction stove, wherein being arranged with heat-insulation layer 4 outside described heater 5.
Foregoing fluorographite pipe reaction stove, wherein being fixed with outside described heater 5 for measuring the chamber of reaction chamber 6
The outer wall detecting temperature meter 14 of the inner chamber thermo detector 13 of interior temperature and the measurement outside wall temperature of reaction chamber 6, the inner chamber thermo detector 13 and outer
Wall thermo detector 14 is connected with temperature control device 8, and the temperature control device 8 is also connected with heater 5.
Foregoing fluorographite pipe reaction stove, wherein being additionally provided with discharge port on the body of heater of the described upside of lower filter layer 15
3, discharge valve is provided with the discharge port 3.
Foregoing fluorographite pipe reaction stove, wherein being additionally provided with safety valve 9 at the top of described body of heater.
Foregoing fluorographite pipe reaction stove, wherein being additionally provided with the pressure for detecting furnace pressure on the outside of described body of heater
Power table 11.
The object of the invention to solve the technical problems is also realized using following technical scheme.According to proposed by the present invention
A kind of method that use fluorographite pipe reaction stove prepares fluorographite, comprises the following steps:1) mouth 12 is added by raw material
Add 4-10g into reaction chamber 6, the crystalline graphite powder of 200-600 mesh, these graphite powders fall and then be stacked on lower filter layer
On 15;2) closing raw material adds the valve at mouth 12, opens heater 5, reaction chamber 6 is heated, temperature control device 8 passes through inner chamber
Thermo detector 13 and outer wall detecting temperature meter 14 monitor the temperature of reaction chamber 6, and adjust heater 5 with this;3) when reaction chamber temperature
When reaching that 300-600 spends, fluorine gas and nitrogen are passed through into gas mixer chamber 16 from fluorine gas import 1 and nitrogen inlet 2 respectively, wherein
Nitrogen flow rate is 0.1~20m/s;Fluorine gas flow velocity is 0.01~2m/s;Through mixed gas in gas mixer chamber 16 by descending
Filtering layer 15 enters reaction chamber 6, and the gas being mixed with the graphite powder stacked on filter layer 15 at present in device takes up, and is suspended in anti-
Answer in chamber 6, in fluid boiling state, when the mol ratio for being passed through fluorine gas and graphite powder in reaction chamber reaches 1:When (0.5~3),
Stop ventilation, reaction product fluorographite is fallen on lower filter layer again;4) valve at discharge port 3 is opened, makes reaction product
Discharged from discharge port 13.
The method that foregoing use fluorographite pipe reaction stove prepares fluorographite, be wherein passed through in step 3 fluorine gas and
The volume ratio of nitrogen is:1:(10~50).
The present invention has clear advantage and beneficial effect compared with prior art.By above-mentioned technical proposal, the present invention
Fluorographite pipe reaction can reach suitable technological progress and practicality, and with the extensive value in industry, its
At least there are following advantages:Sintered screen is divided into chamber, gas can be passed through, and solid powder is in chamber,
It can not downwards miss, can not be blown.Fluorine gas inlet needs because of technique, it is impossible to too fast, to ensure gas in fluorination furnace chamber
Body flow, is aided in nitrogen, accelerates into gas flow rate in chamber.After two kinds of gases are mixed in a mixer, it is ensured that enter
The gas flow for being fluorinated chamber enough, blows afloat powder raw material graphite in suspension, heated device heating is in fluid boiling state, is made
Reaction is more abundant.Temperature control device ensure that fluorination temperature automatic control.Original is respectively provided with reaction chamber upper and lower part
Material adds mouth, and product discharge port after completion of the reaction, it is not necessary to cooling operation, direct blowing, then feeds, realizes continuous metaplasia
Production.
To sum up:Graphite of the present invention and fluorine gas are more abundant, and fluorination efficiency is high.Graphite is arbitrarily stacked in reacting furnace, increases
Graphite linings thickness is added, reaction chamber utilization rate is high, is improved per furnace output.In production process, per stove fluorination finish after, discharging and
Virgin material feed supplement process is changed, body of heater need not stop heating.Realize that not blowing out is continuously produced, improve operating efficiency.
Brief description of the drawings
Fig. 1 is the structural representation of fluorographite pipe reaction stove of the present invention.
【Main element symbol description】
1:Fluorine gas import
2:Nitrogen inlet
3:Discharge port
4:Heat-insulation layer
5:Heater
6:Reaction chamber
7:Upper filter layer
8:Temperature control device
9:Safety valve
10:Atmospheric valve
11:Pressure gauge
12:Raw material adds mouth
13:Inner chamber thermometric
14:Outer wall detecting temperature
15:Lower filter layer
16:Gas mixer chamber
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Accompanying drawing and preferred embodiment, to according to fluorographite pipe reaction stove proposed by the present invention its embodiment, structure, feature
And its effect, describe in detail as after.
Referring to Fig. 1, it is a kind of structural representation of fluorographite pipe reaction stove of the invention, the reacting furnace includes:
Gas mixer chamber 16, lower filter layer 15, reaction chamber 16 and upper filter layer 7 are followed successively by body of heater, the body of heater from down to up.
Nitrogen inlet 2 and fluorine gas import 1 are respectively equipped with the bottom wall body of gas mixer chamber 16, passes through nitrogen inlet 2
The nitrogen and fluorine gas entered with fluorine gas import 1 buffering and mixing in gas mixer chamber 16.
The lower filter layer 15 is a sintering sieves, and gas can pass through the micro-mesh, and raw material solid stone
Ink powder will not be spilt on the filter layer, adhered to or be deposited on filter layer.Enter fluorine nitrogen from fluorine gas import 1 and nitrogen inlet 2
The fluorine nitrogen of blender 16 blows afloat graphite powder after lower filter layer 15, it is in suspended state in reaction chamber 6.
Mouth 12 is added in the top of reaction chamber 6 provided with raw material, for the addition of graphite raw material, the raw material add mouthful at set
There is valve.The raw material, which is added between the mouth of pipe and body of heater of mouth 12, inclination angle, is easy to material to supplement in time into furnace chamber.Preferably
, the inclination angle is 45 °.
The outside of reaction chamber 6 is provided with heater 5.Reaction chamber 6 is heated to needing after temperature by heater 5, fluorine
Fluorination reaction occurs in the chamber for gas and the graphite powder of suspended state.Preferably, heat-insulation layer 4 is arranged with outside the heater 5, but simultaneously
It is not limited to this.For the temperature inside and outside monitoring and controlling reaction chamber 6, it is fixed with respectively outside heater 5 for measuring reaction chamber
The inner chamber thermo detector 13 of the cavity temperature of room 6 and the outer wall detecting temperature meter 14 of the measurement outside wall temperature of reaction chamber 6;The inner chamber thermo detector
13 and outer wall detecting temperature meter 14 be connected with temperature control device 8, the temperature control device 8 is also connected with heater 5, and temperature control device 8 is by interior
Temperature inside and outside chamber thermo detector 13 and the measurement reaction chamber of outer wall detecting temperature meter 14, then by controlling heater 5, reaches automatic tune
Whole, control reaction chamber temperature purpose, makes the temperature of reaction chamber be constantly in suitable state.
The upper filter layer 7 is equally a sintering sieves.Filter layer 7 to ensure the solids in fluorination stove on this
Material is in chamber 6, tail gas after completion of the reaction, and logical upper filter layer 7 is escaped.
Atmospheric valve 10 and safety valve 9 are provided with the top of the body of heater, atmospheric valve 10 is used for the discharge of tail gas, and safety valve 9 is used to protect
Demonstrate,prove the safety of reacting furnace.
Preferably, the outside of body of heater 1 is additionally provided with the pressure gauge 11 for detecting furnace pressure.
Fluorographite pipe reaction stove of the present invention is additionally provided with discharge port 3, the discharge for reacting rear material.The discharge port
3 are located on the upside of lower filter layer, and are additionally provided with discharge valve at the discharge port 3.
The present invention be directed to the equipment of Graphite fluorination, designed for the physicochemical properties feature of graphite and fluorine gas.
Graphite of the present invention is the sieves for having filtration above and below fluid boiling state, reaction chamber in reacting furnace, it is ensured that graphite
Chamber conversion zone repeatedly with fluorine gas, carry out fluorination reaction, make reaction more thoroughly, it is quick.Reacting furnace of the present invention
Material be high temperature resistant, corrosion resistant special material.
Reacting furnace of the present invention is tubular form, and it can stand up when in use, can also tiltedly be put, or bending placement etc..
Below by way of specific embodiment to using a kind of fluorographite pipe reaction stove of the invention
The concrete technology flow process for preparing fluorographite is illustrated.
In a body of heater Φ 57 × 2500 tubular type fluorination stove, the reaction chamber that mouth is fluorinated stove to tubular type is added by raw material
Interior addition 6g, the crystalline graphite powder of 400 mesh, these graphite powders fall and then are stacked on lower filter layer.It is then shut off raw material benefit
Plus the valve at mouth, heater is opened, reaction chamber is heated, temperature control device is monitored by inner chamber thermo detector and outer wall detecting temperature meter
The temperature of reaction chamber, and heater is adjusted with this.When furnace temperature rises to 300 degree, it is passed through fluorine gas, nitrogen and enters reaction chamber,
Wherein nitrogen flow rate is 2.5m/s;Fluorine gas flow velocity is 0.1m/s, is entered through mixed gas in gas mixing room by lower filter layer 1
Enter reaction chamber, blown afloat the graphite powder in reaction chamber on lower filter layer, in suspended state, fluorine gas, nitrogen are from bottom to up
In uphill process, fully contacted with the graphite powder of suspension, fluorination reaction occurs at high temperature.Reacted tail gas is through upper level filter
It is vented after layer by the atmospheric valve of furnace roof.When the mol ratio of the graphite powder in the fluorine gas and reaction chamber being passed through reaches 1:1.25 when,
Fluorine gas, nitrogen valve are closed, the fluorographite powder in the valve at discharge port 3, discharge reaction chamber is opened and obtains 10.2g fluorination stones
Ink, detection fluorographite performance indications are as follows:
Table 1:Pipe reaction stove fluorographite testing result
The above described is only a preferred embodiment of the present invention, any formal limitation not is done to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit according to the present invention
To any simple modification made for any of the above embodiments, equivalent variations and modification, in the range of still falling within technical solution of the present invention.
Claims (7)
1. a kind of fluorographite pipe reaction stove, it includes body of heater, it is characterised in that:
Gas mixer chamber (16), lower filter layer (15), reaction chamber (6) and upper filter layer are followed successively by the body of heater from down to up
(7);
Gas mixer chamber (16) bottom is respectively equipped with nitrogen inlet (2) and fluorine gas import (1);
The lower filter layer (15) and upper filter layer (7) are sintering sieves;
Heater (5) is provided with the outside of the reaction chamber (6);
Mouth (12) is added provided with raw material in reaction chamber (6) top;
Discharge port (3) is additionally provided with body of heater on the upside of the lower filter layer (15);
Atmospheric valve (10) is provided with the top of the body of heater;
The inner chamber thermo detector (13) for measuring reaction chamber (6) cavity temperature is fixed with outside the heater (5) and measures anti-
The outer wall detecting temperature meter (14) of chamber (6) outside wall temperature is answered, the inner chamber thermo detector (13) and outer wall detecting temperature meter (14) are filled with temperature control
(8) connection is put, the temperature control device (8) is also connected with heater (5).
2. fluorographite pipe reaction stove according to claim 1, it is characterised in that wherein described raw material adds mouth (12)
The mouth of pipe and body of heater between have inclination angle.
3. fluorographite pipe reaction stove according to claim 1, it is characterised in that on the outside of wherein described heater (5)
Provided with heat-insulation layer (4).
4. fluorographite pipe reaction stove according to claim 1, it is characterised in that also set at the top of wherein described body of heater
There is safety valve (9).
5. fluorographite pipe reaction stove according to claim 1, it is characterised in that be additionally provided with outside wherein described body of heater
Pressure gauge (11) for detecting furnace pressure.
6. a kind of usage right requires that the fluorographite pipe reaction stove described in 1 to 5 any claim prepares fluorographite
Method, it is characterised in that comprise the following steps:
1) mouth (12) is added by raw material and 4-10g, the crystalline graphite powder of 200-600 mesh, these stones is added into reaction chamber (6)
Ink powder falls and then is stacked on lower filter layer (15);
2) valve that raw material adds mouth (12) place is closed, opens heater (5), reaction chamber (6) is heated, temperature control device (8)
The temperature of reaction chamber (6) is monitored by inner chamber thermo detector (13) and outer wall detecting temperature meter (14), and heater (5) is adjusted with this;
3) when reaction chamber temperature reaches that 300-600 spends, respectively from fluorine gas import (1) and nitrogen inlet (2) to gas mixing
Fluorine gas and nitrogen are passed through in room (16), wherein nitrogen flow rate is 0.1~20m/s;Fluorine gas flow velocity is 0.01~2m/s;It is mixed through gas
Close mixed gas in room (16) and reaction chamber (6) is entered by lower filter layer (15), with what is stacked on filter layer (15) at present
The gas that graphite powder is mixed in device takes up, be suspended in reaction chamber (6), is rubbed when being passed through fluorine gas with graphite powder in reaction chamber
You reach 1 by ratio:When (0.5~3), stop ventilation, reaction product fluorographite is fallen on lower filter layer again;
4) valve at discharge port (3) place is opened, reaction product is discharged from discharge port (3).
7. the method that a kind of use fluorographite pipe reaction stove according to claim 6 prepares fluorographite, its feature
It is, fluorine gas is wherein passed through in step 3 and the volume ratio of nitrogen is:1:(10~50).
Priority Applications (1)
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CN201710582071.0A CN107128896B (en) | 2017-07-17 | 2017-07-17 | Graphite fluoride tubular reaction furnace |
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CN201710582071.0A CN107128896B (en) | 2017-07-17 | 2017-07-17 | Graphite fluoride tubular reaction furnace |
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CN107128896B CN107128896B (en) | 2023-03-10 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108940129A (en) * | 2018-08-29 | 2018-12-07 | 山东重山光电材料股份有限公司 | A kind of system and production method of Multi-class propagation fluorization agent production fluorinated carbon material |
CN109158057A (en) * | 2018-08-29 | 2019-01-08 | 山东重山光电材料股份有限公司 | A kind of fluidized-bed reactor and the method for preparing fluorinated carbon material with it |
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EP0236882A2 (en) * | 1986-03-08 | 1987-09-16 | Hoechst Aktiengesellschaft | Process for the preparation of graphite fluoride |
CN201473319U (en) * | 2009-07-30 | 2010-05-19 | 株洲红亚电热设备有限公司 | Vertical graphitizing furnace for carbon dust high temperature graphitization |
CN102863312A (en) * | 2012-09-07 | 2013-01-09 | 黎明化工研究设计院有限责任公司 | Preparation process of carbon tetrafluoride and device implementing same |
CN203540491U (en) * | 2013-11-18 | 2014-04-16 | 福建省邵武市永晶化工有限公司 | Reactor for preparing antimony pentafluoride |
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CN204324896U (en) * | 2014-12-25 | 2015-05-13 | 江西新卡奔科技有限公司 | A kind of high purity graphite high temperature graphitization stove |
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US4593132A (en) * | 1981-07-22 | 1986-06-03 | Central Glass Co., Ltd. | Process for producing a graphite fluoride |
EP0236882A2 (en) * | 1986-03-08 | 1987-09-16 | Hoechst Aktiengesellschaft | Process for the preparation of graphite fluoride |
CN201473319U (en) * | 2009-07-30 | 2010-05-19 | 株洲红亚电热设备有限公司 | Vertical graphitizing furnace for carbon dust high temperature graphitization |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108940129A (en) * | 2018-08-29 | 2018-12-07 | 山东重山光电材料股份有限公司 | A kind of system and production method of Multi-class propagation fluorization agent production fluorinated carbon material |
CN109158057A (en) * | 2018-08-29 | 2019-01-08 | 山东重山光电材料股份有限公司 | A kind of fluidized-bed reactor and the method for preparing fluorinated carbon material with it |
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