CN208642614U - A kind of production system of fluorinated carbon material - Google Patents
A kind of production system of fluorinated carbon material Download PDFInfo
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- CN208642614U CN208642614U CN201820960030.0U CN201820960030U CN208642614U CN 208642614 U CN208642614 U CN 208642614U CN 201820960030 U CN201820960030 U CN 201820960030U CN 208642614 U CN208642614 U CN 208642614U
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Abstract
The utility model discloses a kind of production system of fluorinated carbon material, including sealable fluidized bed, it is provided with air distribution plate in fluidized bed, is provided with offgas outlet at the top of fluidized bed, offgas outlet is sequentially connected with dust-extraction unit and exhaust gas processing device.Carbon raw material is come into full contact with fluorization agent in fluidized bed and is reacted, the fluorinated carbon material of different fluorine contents is generated；Purification obtains the fluorinated carbon material product that fluorine content is 3% ~ 66% different fluorine contents after drying.Compared with the prior art, the industrial-scale production of fluorinated carbon material may be implemented in this system, and process flow is simple, and reaction efficiency is high, and production cost is low, and product quality is uniform.
Description
Technical field
The utility model relates to a kind of production equipment field of fluorinated carbon material, specially a kind of production of fluorinated carbon material
System.
Background technique
Fluorinated carbon material is a kind of indispensable functional material in the world today, is mainly used in metallurgy, chemical industry, military affairs
Equal fields, it has also become the focus and emphasis of domestic and foreign scholars' research.Since fluorinated carbon material surface can be low, interlamellar spacing is big, chemistry
Property and thermal stability are strong, and degree of fluorination is higher, and lubricity is better, the solid lubrication being widely used under various harsh conditions
Agent or lubricating additive；Active material using fluorinated carbon material as anode can increase the storage life of battery, be formed
The close lithium fluorine cell of high-capacitance, high-output power, high energy；In nuclear reactor, fluorinated carbon material serves as moderator and painting
Compress material prevents fission products to be adsorbed.
Report based on domestic and international related patents and document, the synthetic method of fluorinated carbon material is more, can be in laboratory
Synthesize the higher fluorinated carbon material of fluorine content, for detecting its performance and potential application value, is suitable for small-scale production
Preparation.Currently, the preparation of fluorinated carbon material industrialized production is there are certain difficulty, fluorine content when volume production is not high, and fluorination is uneven
It is even, production is easy to explode etc..
As the demand of fluorinated carbon material increasingly increases, supply falls short of demand, the industrialization large-scale production of fluorinated carbon material
It is extremely urgent.
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.The utility model equipment inventory be 0.1 ~ 100 kg, final products be 0.1 ~
160kg, yield are nearly 100 times of tubular reactor；It has changed simultaneously original fluorization agent and whips carbon material layer surface and be fluorinated
Reactive mode, carbon material come into full contact with reacting under fluidized suspension state with fluorization agent, greatly improves product
It is fluorinated the uniformity.
Summary of the invention
The utility model provides a kind of production system of fluorinated carbon material aiming at above-mentioned defect.This is practical
It is novel to can reduce production cost, product quality is improved, industrialization large-scale production is suitable for.
A kind of production system technical solution of fluorinated carbon material of the utility model is, including sealable fluidized bed, stream
Change bed bottom and be provided with fluorization agent/carrier gas combi inlet port, is internally provided with air distribution plate, is provided with tail gas at the top of fluidized bed and goes out
Mouthful, offgas outlet is sequentially connected with dust-extraction unit and exhaust gas processing device.Fraction solids particle is carried in tail gas in deduster
Bottom is settled down to as product or secondary fluorination material, the gas phase of tail gas is again through subsequent processing.
The conversion zone being divided into above bottom air plenum and gas chamber inside fluidized bed.
For air distribution plate between fluidized-bed bottom gas chamber and conversion zone, carbon raw material entrance is located at fluidized-bed reaction pars infrasegmentalis,
Above air distribution plate.
Product exit is located at the fluidized-bed reaction section side opposite with carbon raw material entrance, and air distribution plate top is highly lower than carbon
Feed(raw material)inlet.
Exhaust gas processing device includes primary adsorption tower, secondary absorption tower.
The primary adsorption tower is provided with charcoal or active carbon, bamboo charcoal or other carbon materials with adsorptivity, absorbs tail
Extra fluorization agent in gas；The secondary absorption tower is provided with one of soda lime, sodium fluoride, alkaline solution, absorbs tail gas
In fluoro-gas.
The material of fluidized bed and air distribution plate is at least one of carbon steel, stainless steel, monel, red copper alloy.
The material of fluidized bed and air distribution plate is monel, red copper alloy is abundant by carbon raw material and fluorization agent in fluidized bed
Haptoreaction generates the fluorinated carbon material of different fluorine contents；Purification, it is 3% ~ 66% different fluorine contents that fluorine content is obtained after drying
Fluorinated carbon material product.
A kind of production method of the fluorinated carbon material, comprising the following steps:
Step 1: carbon raw material investment is included in the fluidized bed of air distribution plate, is sealed to whole system and the leak test that pressurizes；
Step 2: being passed through diluent gas, is to slowly warm up to 200 DEG C, removes moisture and other impurity in carbon raw material.
Step 3: after mixing by fluorization agent and diluent gas, being passed through from the bottom of fluidized bed, top outflow；
Step 4: make the carbon raw material for being in fluidized state in fluidized bed, come into full contact with and react with fluorization agent, generate different fluorine
The fluorinated carbon material of content；
Step 5: system carries out vent gas treatment, and material is purified, and it is that 3% ~ 66% different fluorine contain that fluorine content is obtained after drying
The fluorinated carbon material product of amount.
Carbon raw material in the step 1 is 20 mesh ~ 15000 mesh graphite, carbon fiber, graphene, active carbon, pitch, bamboo
At least one of the carbon materials such as charcoal, fullerene, carbon black, carbon nanotube, coke, bortz powder, inventory are 0.1 ~ 100 kg.
The material of fluidized bed and air distribution plate in the step 1 be carbon steel, stainless steel, monel, red copper alloy and its
At least one of the alloy material that resistance to fluorization agent corrodes under its high temperature.Preferably monel.
Diluent gas in the step 2 is nitrogen, argon gas, helium, carbon tetrafluoride, fluorine-containing alkane and perfluoro alkane etc.
At least one of inert gas.
Fluorization agent in the step 3 is the fluorine-containing objects such as fluorine gas, hydrogen fluoride, oxygen difluoride, Nitrogen trifluoride and antimony pentafluoride
At least one of matter.
Fluorization agent and diluent gas gaseous mixture in the step 3, total gas flow rate are controlled in 0.1 ~ 1000 Nm3/h。
Reaction temperature control in the step 4 is at 150 ~ 600 DEG C, and reaction time control is in 2 ~ 80 h, and fluorization agent is mixed
The volumetric concentration closed in gas is controlled 0.1 ~ 60%.
Material in the step 5 carries out purifying water source used being deionized water or distilled water.
The utility model has the following beneficial effects:
1, the industrial-scale production of fluorinated carbon material is realized, single fluidised bed production capacity is up to 0.1 ~ 50 ton/year.
2, process flow is simple, and reaction efficiency is high, and product quality is uniform, and production cost is low.
3, by parameters such as control reaction temperature, reaction pressure, reaction time and fluorinating agent concentrations, fluorine content, which can be obtained, is
The fluorinated carbon material product of 3% ~ 66% different fluorine contents.
4, carbon raw material is in fluidized state in fluidized bed, and uniform and complete is reacted with fluorization agent, and product quality is uniform, production
Fluorinated carbon material product out is mainly as the positive electrode of new type lithium ion battery and high-end solid lubricant material and height
Hold the filler of anticorrosive paint.
Detailed description of the invention
Fig. 1 show the schematic device of the utility model fluorinated carbon material industrialized production；
In figure, 1- fluidized bed, 2- air distribution plate, 3- dust-extraction unit, 4- exhaust gas processing device.
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
A kind of production system of fluorinated carbon material of the utility model, including sealable fluidized bed 1 are set in fluidized bed 1
It is equipped with air distribution plate 2, offgas outlet, offgas outlet and dust-extraction unit 3 and exhaust gas processing device 4 are provided at the top of fluidized bed 1 successively
Connection.Fraction solids particle is carried in tail gas bottom is settled down in deduster as product or secondary fluorination material, tail gas
Gas phase is again through subsequent processing.The conversion zone being divided into above bottom air plenum and gas chamber inside fluidized bed 1.
Air distribution plate 2 is located between 1 bottom air plenum of fluidized bed and conversion zone, and carbon raw material entrance is located under 1 conversion zone of fluidized bed
Portion, 2 top of air distribution plate.
Product exit is located at 1 conversion zone of the fluidized bed side opposite with carbon raw material entrance, and 2 top of air distribution plate is highly lower than
Carbon raw material entrance.
Exhaust gas processing device 4 include primary adsorption tower, secondary absorption tower processing, the primary adsorption tower be provided with charcoal or
Active carbon absorbs fluoro-gas extra in tail gas；The secondary absorption tower is provided with soda lime, sodium fluoride, in alkaline solution
One kind, absorb tail gas in fluoro-gas.
The material of fluidized bed 1 and air distribution plate 2 is at least one of carbon steel, stainless steel, monel, red copper alloy.
Embodiment 2
By taking aquadag raw material as an example, the side of fluidized-bed reactor large-scale production fluorinated carbon material is used using the present invention
Method production fluorination aquadag, comprises the following steps that
It takes in fluidized bed 1 of 15 kg of the aquadag raw material investment containing air distribution plate 2, whole system is sealed and is pressurizeed
Leak test is passed through nitrogen removal volatile impurity, and to 1 heat temperature raising of fluidized bed；Reach 250 DEG C after 2 h, at this time from fluidized bed 1
Bottom is passed through oxygen difluoride/nitrogen mixture, and flow velocity is 7.5 Nm3/h；Pressure is normal pressure, reaction temperature 400 in fluidized bed 1
~ 450 DEG C, oxygen difluoride concentration is 4%, and the reaction time is 38 h, stops heating, nitrogen displacement, Temperature fall；To fluidized bed 1
Internal temperature is cooled to room temperature feeding, obtains the bed body material of 29.8 kg grey blacks, after the elution of multiple deionized water is pure, obtains
To the fluorinated carbon material product of 28.2 kg grey blacks.
It is 51% by test characterization fluorine content, purification rate 94.63%.
Embodiment 3
By taking nano-graphite raw material as an example, the side of fluidized-bed reactor large-scale production fluorinated carbon material is used using the present invention
Method produces fluorinated nano graphite, comprises the following steps that
It takes in fluidized bed 1 of 5 kg of the nano-graphite raw material investment containing air distribution plate, whole system is sealed and examination of pressurizeing
Leakage is passed through helium removal volatile impurity, and to 1 heat temperature raising of fluidized bed；Reach 280 DEG C after 1 h, at this time from 1 bottom of fluidized bed
Portion is passed through fluorine gas/helium mix gas, and flow velocity is 3.5 Nm3/h；Pressure is normal pressure in fluidized bed 1, and reaction temperature is 450 ~ 500
DEG C, concentration of fluorine 3%, the reaction time is 42 h, stops heating, helium replacement, Temperature fall；It is dropped to 1 internal temperature of fluidized bed
Feeding after to room temperature obtains the bed body material of 10.8 kg grey, after the elution of multiple deionized water is pure, obtains 10.2 kg grey
Fluorinated carbon material product.
It is 54% by test characterization fluorine content, purification rate 94.44%.
Embodiment 4
By taking expanded graphite raw material as an example, the side of fluidized-bed reactor large-scale production fluorinated carbon material is used using the present invention
Method production fluorination expanded graphite, comprises the following steps that
It takes in fluidized bed of 100 kg of the expanded graphite raw material investment containing air distribution plate, whole system is sealed and examination of pressurizeing
Leakage is passed through carbon tetrafluoride removal volatile impurity, and to fluidized bed heat temperature raising；Reach 320 DEG C after 5 h, at this time from fluidized bed
Bottom is passed through Nitrogen trifluoride/carbon tetrafluoride gaseous mixture, and flow velocity is 12 Nm3/h；Pressure is normal pressure in fluidized bed, and reaction temperature is
460 ~ 510 DEG C, Nitrogen trifluoride concentration is 17%, and the reaction time is 30 h, stops heating, and carbon tetrafluoride gas displacement is dropped naturally
Temperature；It is cooled to room temperature feeding to fluidized bed internal temperature, the linen bed body material of 224kg is obtained, is washed through multiple deionization
After purification, the linen fluorinated carbon material product of 208 kg is obtained.
It is 58% by test characterization fluorine content, purification rate 92.86%.
Embodiment 5
By taking spherical graphite raw material as an example, the side of fluidized-bed reactor large-scale production fluorinated carbon material is used using the present invention
Method production fluorination spherical graphite, comprises the following steps that
It takes in fluidized bed 1 of 40 kg of the spherical graphite raw material investment containing air distribution plate, whole system is sealed and examination of pressurizeing
Leakage is passed through argon gas removal volatile impurity, and to 1 heat temperature raising of fluidized bed；Reach 350 DEG C after 3 h, at this time from 1 bottom of fluidized bed
Portion is passed through antimony pentafluoride/argon gas gaseous mixture, and flow velocity is 10 Nm3/h；Pressure is normal pressure in fluidized bed, and reaction temperature is 480 ~ 530
DEG C, antimony pentafluoride concentration is 6%, and the reaction time is 23 h, stops heating, argon gas displacement, Temperature fall；To 1 inside temperature of fluidized bed
Degree is cooled to room temperature feeding, obtains the linen bed body material of 86.7 kg, after the elution of multiple deionized water is pure, obtains 80.6
The linen fluorinated carbon material product of kg.
It is 55% by test characterization fluorine content, purification rate 92.96%.
Embodiment 6
By taking crystalline flake graphite raw material as an example, the side of fluidized-bed reactor large-scale production fluorinated carbon material is used using the present invention
Method production fluorination crystalline flake graphite, comprises the following steps that
It takes in fluidized bed 1 of 80 kg of the crystalline flake graphite raw material investment containing air distribution plate, whole system is sealed and examination of pressurizeing
Leakage is passed through carrier gas removal volatile impurity, and to 1 heat temperature raising of fluidized bed；Reach 500 DEG C after 5 h, at this time from fluidized bed
Bottom is passed through fluorine gas/helium, and flow velocity is 26 Nm3/h；Pressure is 0.3MPag in fluidized bed 1, and reaction temperature is 500 ~ 560 DEG C,
Concentration of fluorine is 42%, and the reaction time is 6.5 h, stops heating, helium replacement, Temperature fall；It is dropped to 1 internal temperature of fluidized bed
Feeding after to room temperature obtains the linen bed body material of 173.5 kg, after the elution of multiple deionized water is pure, obtains 162 kg ash
The fluorinated carbon material product of white.
It is characterized by test: fluorine content 56%, purification rate 93.37%.
Claims (6)
1. a kind of production system of fluorinated carbon material, which is characterized in that including sealable fluidized bed, fluidized-bed bottom is provided with
Fluorization agent/carrier gas combi inlet port, is internally provided with air distribution plate, is provided with offgas outlet at the top of fluidized bed, offgas outlet with
Dust-extraction unit and exhaust gas processing device are sequentially connected.
2. a kind of production system of fluorinated carbon material according to claim 1, which is characterized in that
The conversion zone being divided into above bottom air plenum and gas chamber inside fluidized bed.
3. a kind of production system of fluorinated carbon material according to claim 2, which is characterized in that air distribution plate is located at fluidized bed
Between bottom air plenum and conversion zone, carbon raw material entrance is located at fluidized-bed reaction pars infrasegmentalis, air distribution plate top.
4. a kind of production system of fluorinated carbon material according to claim 3, which is characterized in that product exit is located at fluidisation
The bed conversion zone side opposite with carbon raw material entrance, air distribution plate top, is highly lower than carbon raw material entrance.
5. a kind of production system of fluorinated carbon material according to claim 1, which is characterized in that exhaust gas processing device includes
Primary adsorption tower, secondary absorption tower.
6. a kind of production system of fluorinated carbon material according to claim 5, which is characterized in that in the primary adsorption tower
Equipped with charcoal, bamboo charcoal or active carbon, fluoro-gas extra in tail gas is absorbed；The secondary absorption tower is provided with soda lime, fluorine
Change one of sodium, alkaline solution, further absorbs the fluoro-gas in tail gas.
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| CN201820960030.0U CN208642614U (en) | 2018-06-21 | 2018-06-21 | A kind of production system of fluorinated carbon material |
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| CN201820960030.0U CN208642614U (en) | 2018-06-21 | 2018-06-21 | A kind of production system of fluorinated carbon material |
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| CN208642614U true CN208642614U (en) | 2019-03-26 |
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