CN209034318U - A kind of fluidized-bed reactor producing fluorinated carbon material - Google Patents
A kind of fluidized-bed reactor producing fluorinated carbon material Download PDFInfo
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- CN209034318U CN209034318U CN201821401135.9U CN201821401135U CN209034318U CN 209034318 U CN209034318 U CN 209034318U CN 201821401135 U CN201821401135 U CN 201821401135U CN 209034318 U CN209034318 U CN 209034318U
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Abstract
The utility model discloses a kind of fluidized-bed reactor for producing fluorinated carbon material, the fluidized-bed reactor successively includes gas chamber, conversion zone, material settling section from bottom to top；Gas distribution grid is provided between gas chamber and conversion zone, gas chamber bottom is equipped with fluorization agent/carrier gas combi inlet port, and conversion zone lower sides are equipped with discharge port and recycle stock import, and side is equipped with feed opening in the middle part of conversion zone；Tail gas interface and pumped vacuum systems interface are additionally provided at the top of material settling section；The tail gas interface of the fluidized-bed reactor is connected with gas-solid separator, and gas-solid separator is connect by Pneumatic conveyer with recycle stock import, and gas-solid separator also passes through recyclegas and removes high fluorine carbon alkane equipment to be connect with fluorization agent/carrier gas combi inlet port.Compared with traditional fluorination reactor, it is able to ascend fluorization agent utilization rate, improves the working efficiency of reactor, realize the scale of mass production of fluorinated carbon material and effectively reduces the production cost of fluorinated carbon material.
Description
Technical field
The utility model belongs to technical field of fluorine chemical industry, specially a kind of fluidized-bed reactor for producing fluorinated carbon material.
Background technique
Fluorinated carbon material is a kind of indispensable functional material in the world today, and fluorinated carbon material has excellent lubrication
Performance, greasy property are better than general graphite and molybdenum disulfide, and in dry or moist high temperature, coefficient of friction is smaller, use the longevity
It orders longer；Fluorinated carbon material has extremely low surface energy simultaneously, and the presence of C-F key makes it have stronger hydrophobic oleophobic ability,
Its excellent performance has become the focus and emphasis of domestic and foreign scholars' research.
The synthetic method of existing fluorinated carbon material is more, and tube furnace can be used in laboratory, and to synthesize fluorine content higher
Fluorinated carbon material for detecting its performance and potential application value, but needs interval blowing and feeding, and there is volume productions not
High, the problems such as fluorization agent utilization rate is low, energy consumption is high, it is suitable for small-scale production and prepares, currently, fluorinated carbon material industrialized production
That there are certain difficulty, when volume production, there is fluorine contents is not high for preparation, and fluorination is uneven, produces many difficult points such as easily decomposes.
Fluorinated carbon material process units industrial at present generally uses horizontal pipe furnace reactor, and it is anti-that there is intervals
Answer, manually into discharging, to be difficult to disadvantages, fluorinated carbon material field related patents and the documents such as volume production, fluorization agent utilization rate be low current
It being capable of not the other reactor of volume production feather weight.
Summary of the invention
The utility model provides a kind of fluidized-bed reaction for producing fluorinated carbon material aiming at above-mentioned defect
Device.The utility model fluidized-bed reactor inventory is big, and yield is big, and change original fluorization agent whip carbon material layer surface into
The fluorinated reactive mode of row, carbon material come into full contact with reacting, greatly be improved under fluidized suspension state with fluorization agent
The fluorination uniformity of product.
A kind of fluidized-bed reactor technical solution producing fluorinated carbon material of the utility model is a kind of production fluorocarbons
The fluidized-bed reactor of material, the fluidized-bed reactor successively include gas chamber, conversion zone, material settling section from bottom to top；
Gas distribution grid is provided between gas chamber and conversion zone, gas chamber bottom is equipped with fluorization agent/carrier gas combi inlet port；
Conversion zone lower sides are equipped with discharge port and recycle stock import, and side is equipped with feed opening in the middle part of conversion zone；
Tail gas interface and pumped vacuum systems interface are additionally provided at the top of material settling section；
The tail gas interface of the fluidized-bed reactor is connected with gas-solid separator, and gas-solid separator passes through Pneumatic conveyer
It is connect with recycle stock import, gas-solid separator also passes through recyclegas and removes high fluorine carbon alkane equipment and fluorization agent/carrier gas
Combi inlet port connection.
External heating device is equipped on the outside of the conversion zone.
Insulating is provided on the outside of the external heating device.
The recycle stock import of reaction pars infrasegmentalis is located above discharge port, and recycle stock import and discharge port be not in the same side
Face.
Bleed-off system is connected by rupture disk at the top of material settling section.
Gas chamber is provided with pressure detecting point, and the temperature detecting point of 3-4 group is uniformly distributed in conversion zone, is set in material settling section
There is pressure detecting point.
The gas chamber, conversion zone, material settling section, gas distribution grid material are carbon steel, stainless steel, monel, purple
At least one of copper alloy.
Recyclegas removes high fluorine carbon alkane equipment and condenses and separates high fluorine carbon alkane in such a way that refrigerant heat exchange is cooling
Method removes high fluorine carbon alkane using the method for cobalt trifluoride, the catalytic decomposition conversion of borontrifluoride iron.
The utility model has the following beneficial effects: the utility model fluidized-bed reactor structure is simple, reactor production maintenance
It is convenient and efficient；Equipment inventory is 0.1 ~ 100 kg, and final products are 0.1 ~ 160kg, and yield is nearly the 200 of tubular reactor
Times；It has changed simultaneously original fluorization agent and has whipped the fluorinated reactive mode of carbon material layer surface progress, carbon material is in fluidized suspension shape
Come into full contact with reacting with fluorization agent under state, greatly improves the fluorination uniformity of product.With traditional fluorination reactor phase
Than, be able to ascend fluorization agent utilization rate, improve the working efficiency of reactor, realize fluorinated carbon material scale of mass production and effectively
Reduction fluorinated carbon material production cost.
Carbon material is partially or fully fluorinated in even fluidizing state and fluorization agent generation in reactor in the utility model
Reaction, product homogeneity is good, while improving the production of reactor into discharge way using vacuum feed and pressurising discharging
The setting of efficiency, recycle stock improves the utilization rate of fluorization agent and the yield of product, and the setting of recyclegas improves fluorine
The safety of utilization rate and the device operation of agent, compared to the method that conventional tubular furnace reactor prepares fluorinated carbon material, more
Add and is suitable for industrial scale production.
Detailed description of the invention:
Fig. 1 show the basic structure schematic diagram of the utility model；
Fig. 2 show the grain size distribution that the utility model embodiment 4 prepares product
Fig. 3 show the SEM figure that the utility model embodiment 4 prepares product.
In figure, 1- fluorization agent/carrier gas combi inlet port, 2- gas chamber, 3- gas distribution grid, 4- conversion zone, 5- material is heavy
Drop section, 6- rupture disk, 7- tail gas interface, 8- pumped vacuum systems interface, 9- discharge port, 10- feed opening, 11- recycle stock import,
12- external heating device, 13- gas-solid separator, 14- Pneumatic conveyer, 15- recyclegas remove high fluorine carbon alkane equipment.
Specific embodiment:
The technical side of the utility model is described in detail in the utility model in order to better understand with specific example below
Case, but the utility model is not limited thereto.
Embodiment 1
As shown in Figure of description Fig. 1, a kind of fluidized-bed reactor producing fluorinated carbon material, the fluidized-bed reaction
Device successively includes gas chamber 2, conversion zone 4, material settling section 5 from bottom to top；
Gas distribution grid 3 is provided between gas chamber 2 and conversion zone 4,2 bottom of gas chamber is equipped with fluorization agent/carrier gas gaseous mixture
Import 1；
4 lower sides of conversion zone are equipped with discharge port 9 and recycle stock import 11, and 4 middle part side of conversion zone is equipped with charging
Mouth 10；
Tail gas interface 7 and pumped vacuum systems interface 8 are additionally provided at the top of material settling section 5；
The tail gas interface 7 of the fluidized-bed reactor is connected with gas-solid separator 13, and gas-solid separator 13 passes through pneumatic transporting
Send device 14 to connect with recycle stock import 11, gas-solid separator 13 also by recyclegas remove high fluorine carbon alkane equipment 15 with
Fluorization agent/carrier gas combi inlet port 1 connects.
External heating device 12 is equipped on the outside of the conversion zone 4.
The gas chamber 2, conversion zone 4, material settling section 5,3 material of gas distribution grid are that carbon steel, stainless steel, ambrose alloy close
At least one of gold, red copper alloy.
Embodiment 2
As shown in Figure of description Fig. 1, a kind of fluidized-bed reactor producing fluorinated carbon material, the fluidized-bed reaction
Device successively includes gas chamber 2, conversion zone 4, material settling section 5 from bottom to top；
Gas distribution grid 3 is provided between gas chamber 2 and conversion zone 4,2 bottom of gas chamber is equipped with fluorization agent/carrier gas gaseous mixture
Import 1；
4 lower sides of conversion zone are equipped with discharge port 9 and recycle stock import 11, and 4 middle part side of conversion zone is equipped with charging
Mouth 10；
Tail gas interface 7 and pumped vacuum systems interface 8 are additionally provided at the top of material settling section 5；
The tail gas interface 7 of the fluidized-bed reactor is connected with gas-solid separator 13, and gas-solid separator 13 passes through pneumatic transporting
Send device 14 to connect with recycle stock import 11, gas-solid separator 13 also by recyclegas remove high fluorine carbon alkane equipment 15 with
Fluorization agent/carrier gas combi inlet port 1 connects.
External heating device 12 is equipped on the outside of the conversion zone 4.
Insulating is provided on the outside of the external heating device 12.
The recycle stock import 11 of 4 lower part of conversion zone is located at 9 top of discharge port, and recycle stock import 11 and discharge port 9 are not
In same side.
Bleed-off system is connected by rupture disk 6 at the top of material settling section 5.
Gas chamber 2 is provided with pressure detecting point, and the temperature detecting point of 3-4 group, material settling section 5 are uniformly distributed in conversion zone 4
It is interior to be equipped with pressure detecting point.
The gas chamber 2, conversion zone 4, material settling section 5,3 material of gas distribution grid are that carbon steel, stainless steel, ambrose alloy close
At least one of gold, red copper alloy.
Embodiment 3
A method of fluorinated carbon material is prepared using the fluidized-bed reactor, comprising the following steps:
(1) fluidized-bed reactor is evacuated to negative pressure state using vacuum pump, stream is added in carbon raw material in a manner of vacuum feed
In fluidized bed reactor；
(2) be passed through carrier gas, fluidized-bed reactor is to slowly warm up to 100-600 DEG C, remove moisture in carbon raw material and its
Its impurity；
(3) after mixing by fluorization agent and carrier gas, it is passed through from the bottom of fluidized-bed reactor, top outflow；
(4) make the carbon raw material for being in fluidized state in fluidized-bed reactor, come into full contact with and react with fluorization agent, generate different
The fluorinated carbon material of fluorine content；
(5) material is purified, and the fluorinated carbon material product that fluorine content is 3% ~ 70% different fluorine contents is obtained after drying.
Negative pressure is -10 ~ -90Pa in fluidized-bed reactor in step (1)；Carbon raw material is 20 mesh ~ 15000 mesh graphite, carbon fiber
At least one of dimension, graphene, active carbon, pitch, bamboo charcoal, fullerene, carbon black, carbon nanotube, coke, inventory be 0.1 ~
100 kg；
(2) in step (2) carrier gas be nitrogen, argon gas, helium, carbon tetrafluoride, fluorine-containing alkane and perfluoro alkane in extremely
Few one kind；
Fluorization agent is at least one of fluorine gas, hydrogen fluoride, oxygen difluoride, Nitrogen trifluoride and antimony pentafluoride in step (3)；
150 ~ 600 DEG C of reaction temperature；2 ~ 80 h of reaction time；Volumetric concentration 0.1 ~ 60% of the fluorization agent in gaseous mixture；Gaseous mixture always flows
Measure 0.1 ~ 1000 Nm3/h。
Material in step (5) carries out purifying water used being deionized water or distilled water.
Recyclegas removes high fluorine carbon alkane equipment and condenses and separates high fluorine carbon alkane in such a way that refrigerant heat exchange is cooling
Method removes high fluorine carbon alkane using the method for cobalt trifluoride, the catalytic decomposition conversion of borontrifluoride iron.
Embodiment 4
Using fluidized-bed reactor as described in example 2,5 kg of graphite raw material is taken to put into the fluidized bed containing gas distribution grid 2
In reactor, whole system is sealed and the leak test that pressurizes, is passed through carrier gas removal volatile impurity, and to fluidized-bed reaction
Device heat temperature raising；Reach 250 DEG C after 3 h, fluorization agent/carrier gas combi inlet port 1 is passed through fluorization agent/carrier gas mixing at this time
Gas, flow velocity are 3 Nm3/h；Pressure is normal pressure in fluidized-bed reactor, and reaction temperature is 400 ~ 450 DEG C, and fluorinating agent concentration is
4%, the reaction time is 20 h, stops heating, carrier gas displacement, Temperature fall；To the near room temperature of fluidized-bed reactor internal temperature
Feeding afterwards obtains the bed body material of 7 kg grey blacks, after the elution of multiple deionized water is pure, obtains the fluorocarbons of 5 kg grey blacks
Material product.
It is 51% by test characterization fluorine content, purification rate 71%, fluorization agent mass flowmenter integrated flow is 1.72Nm
3, fluorine element content is 2.55kg in fluorographite, and fluorization agent utilization rate is 95.6%.The detection of fluorographite product index is as follows:
1 fluorographite product testing result of table
Claims (6)
1. a kind of fluidized-bed reactor for producing fluorinated carbon material, which is characterized in that the fluidized-bed reactor is from bottom to top
It successively include gas chamber (2), conversion zone (4), material settling section (5)；
It is provided between gas chamber (2) and conversion zone (4) gas distribution grid (3), gas chamber (2) bottom is mixed equipped with fluorization agent/carrier gas
It closes gas import (1)；
Conversion zone (4) lower sides are equipped with discharge port (9) and recycle stock import (11), and side is equipped in the middle part of conversion zone (4)
Feed opening (10)；
Tail gas interface (7) and pumped vacuum systems interface (8) are additionally provided at the top of material settling section (5)；
The tail gas interface (7) of the fluidized-bed reactor is connected with gas-solid separator (13), and gas-solid separator (13) passes through strength
Conveying device (14) is connect with recycle stock import (11), and gas-solid separator (13) also removes high fluorine carbon alkane by recyclegas
Equipment (15) is connect with fluorization agent/carrier gas combi inlet port (1).
2. a kind of fluidized-bed reactor for producing fluorinated carbon material according to claim 1, which is characterized in that described is anti-
It answers and is equipped with external heating device (12) on the outside of section (4).
3. a kind of fluidized-bed reactor for producing fluorinated carbon material according to claim 2, which is characterized in that described is outer
Insulating is provided on the outside of portion's heating device (12).
4. a kind of fluidized-bed reactor for producing fluorinated carbon material according to claim 1, which is characterized in that conversion zone
(4) the recycle stock import (11) of lower part is located above discharge port (9), and recycle stock import (11) is with discharge port (9) not same
One side.
5. a kind of fluidized-bed reactor for producing fluorinated carbon material according to claim 1, which is characterized in that material sedimentation
Bleed-off system is connected by rupture disk (6) at the top of section (5).
6. a kind of fluidized-bed reactor for producing fluorinated carbon material according to claim 1, which is characterized in that gas chamber (2)
It is provided with pressure detecting point, the temperature detecting point of 3-4 group is uniformly distributed in conversion zone (4), is equipped with pressure in material settling section (5)
Test point.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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