CN108807884A - A kind of system and method for lithium ion battery negative material carbon coating modification - Google Patents
A kind of system and method for lithium ion battery negative material carbon coating modification Download PDFInfo
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- CN108807884A CN108807884A CN201810549196.8A CN201810549196A CN108807884A CN 108807884 A CN108807884 A CN 108807884A CN 201810549196 A CN201810549196 A CN 201810549196A CN 108807884 A CN108807884 A CN 108807884A
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of system and methods of lithium ion battery negative material carbon coating modification, the system includes mainly feed bin, feeding screw, preheater inlet valve, fluidized bed powder preheater, reactor feed valve, fluidized-bed reactor, reactor outlet valve, reactor product cooler, product collector, cold mixture heater, first order reaction tail gas cyclone separator, second order reaction tail gas cyclone separator, reaction end gas bagroom, reaction end gas burner, the pre- hot exhaust gas cyclone separator of level-one, the pre- hot exhaust gas cyclone separator of two level, pre- hot exhaust gas bagroom and preheating exhaust gas cooler are formed according to given combinations；The method is the carbon coating method based on the system, and carbon coating cathode composite granule is obtained by fluidization chemical vapor deposition.The present invention has many advantages, such as that coating efficiency is high, simple for process controllable, at low cost, is suitble to the scale industrial production of lithium ion battery coated modified carbon negative material, with good economic efficiency and social benefit.
Description
Technical field
The invention belongs to lithium ion battery materials and chemical field, and in particular to a kind of lithium ion battery negative material carbon packet
Cover modified system and method.
Background technology
Lithium ion battery with the features such as its high-energy density, long circulation life, memory-less effect and safety and environmental protection very much
Field is widely used.In recent years, with the fast development of electric vehicle, people propose the performance of lithium ion battery
Higher requirement.Core component of the electrode material as lithium ion battery, decides the performance of lithium ion battery.In reality
During the use of border, traditional lithium ion battery negative material, such as carbon-based, silicon substrate and lithium titanate, it there are problems that.Carbon
The lithium ion mobility rate of base graphite is relatively low, is not suitable for high current charge-discharge, and there are solvents to be embedded in phenomenon altogether；Silica-base material fills
Due to Volumetric expansion in discharge process, easily leads to material disintegrating and form new exposed surface, cause the solid electrolyte on surface
It the lasting rupture of interfacial film (SEI films) and re-forms, causes circulation volume to decline, coulombic efficiency is low, while the intrinsic conduction of silicon
Poor performance；The electronic conduction ability of lithium titanate itself is general, limits battery performance under the conditions of high current charge-discharge.These
Problem seriously limits the development and application of negative material.
Coated modified carbon is a kind of highly effective feasible method for solving the problems, such as this, and electricity can be reduced by coated modified carbon
Charge transfer resistance of the pond in charge and discharge process improves electron conduction and ionic conductivity, improves the multiplying power of transition material
On the other hand performance can prevent being in direct contact for material and electrolyte, inhibit erosion of the hydrofluoric acid to material in cyclic process,
Reduce the side reaction of material and electrolyte.For carbon-based material, coated modified carbon can stablize the material structure stability of graphite,
Prevent graphite from failing because solvent is embedded altogether.For silica-base material, it is de- in lithium ion insertion that coated modified carbon can also buffer silicon
Volume change during going out improves the structural stability of material.Therefore, coated modified carbon is to lithium ion battery electrode material
Performance improvement is significant.
Currently, the carbon coating method of lithium ion battery negative material includes mainly：
(1) mechanical-physical mixes：The patent CN1252846C of Wuhan University disclose it is a kind of using mechanical ball mill directly will
The method that silicon alloy and carbon-based material are mixed with Si-C composite material.Although this method preparation process is simple, at low cost,
Operating time is long, mixing is uneven, and carbon is insufficient contact with silicon alloy, and material property improves extremely limited.
(2) solid phase mixing is pyrolyzed：Solid phase mixing method for pyrolysis refers to passing through solid phase machine by negative material and containing carbon matrix precursor
Tool mixes, then prepares carbon encapsulated material by pyrolysis.The patent CN103311522B of Chinese Academy Of Sciences Process Engineering Research Institute is straight
It connects and mixes silica flour, graphite and carbon containing organic binder, then carbon coating silica-base material is obtained by high temperature pyrolysis.Shenzhen Bei Te
The patent CN1913200B of auspicious Electron Material Co., Ltd discloses a kind of silica flour and pitch mechanical mixture, then mixing material is set
It is thermally treated resulting in carbon coating silica-base material in 1200 DEG C.The patent CN103474635B of Foshan Advanced Electronics Energy Co., Ltd. by silicon,
Titanium and other metal and nonmetal elements are smelted into the alloy of uniform component, and ball milling is at amorphous alloy powder in agitating ball mill
End, then be uniformly mixed with carbon source, it is heat-treated in protective atmosphere or vacuum, carbon coating silicotitanium negative material is prepared.
The patent CN103647056B of Shenzhen City Beiterui New Energy Materials Co., Ltd discloses a kind of carbon coating oxidation silicon substrate
The preparation method of composite negative pole material is that micron-sized silica material is passed through to mechanical fusion, solid phase cladding, high temperature successively to burn
Knot obtains carbon-coated composite material.The uniformity effects of this kind of carbon coating method depend primarily on negative material and carbon matrix precursor
Mixing uniformity, and the solid phase mixing used, based on mechanical mixture, uniformity is poor.Carbon matrix precursor is easy when high temperature pyrolysis
Idiomorphism karyogenesis causes performance improvement effect limited from the carbon reunited.
(3) liquid phase mixed pyrolysis：Liquid phase mixed pyrolysis refers to mixing negative material and carbon containing precursor solution, warp
It crosses pyrolysis and prepares carbon encapsulated material.The patent CN1199300C of Shanghai Inst. of Microsystem and Information Technology, Chinese Academy of Sci will be dripped
Blueness is used as carbon source presoma, is dissolved in organic solvent, silica flour or silica powder is added in solution, evenly dispersed processing, drying
It carries out protective atmosphere high-temperature heat treatment again afterwards, prepares carbon coating silica-base material.Tianjin Kimwan Special Carbon Material Technology Development Co., Ltd.
Disclose similar patent (CN102593426A).The patent CN104617291A of Fudan University with specific organic compound from
Sub- liquid is carbon source, is sufficiently mixed with electrode material, and the carbon coating electricity of high conductivity and high power capacity is pyrolyzed to obtain after dry
Pole material.The patent CN105958036A of Tianjin Pulan Energy Science Co., Ltd is mixed with carbonaceous organic material dispersion liquid using silica flour
It closes, drying pyrolysis, obtained primary carbon coating silicium cathode material second mix with carbonaceous organic material dispersion liquid, dries and hot
Solution, obtains secondary carbon coating silica-base material.Common carbon source presoma has ionic liquid (CN104282896A), pitch
(CN106684360A), phenolic resin (CN101859893A), epoxy resin (CN100413127C), polyacrylonitrile
(CN105529466A) and organic or inorganics carbonaceous material, the heat treatment temperature section such as benzene naphthalene copolymer (CN1144304C) are
400~1300 DEG C, processing time is 6~48h.Compared with solid phase mixing is pyrolyzed, liquid phase mixes negative material and carbon matrix precursor
Uniformity can greatly improve, but liquid phase mixed pyrolysis process bands come complex process and processing time length can increase it is carbon-coated
Cost, while carbon matrix precursor is easy idiomorphism karyogenesis from the carbon reunited when high temperature pyrolysis, also influences carbon coating to chemical property
Improvement.
(4) chemical vapor deposition：Realize that carbon coating can effectively improve carbon coating by the pyrolytic deposition of gas phase carbon matrix precursor
Uniformity.Catalyst is mixed with silicon particle or is made alloy by the patent CN1903793A of Inst. of Physics, CAS
Afterwards, chemical vapor deposition carbon nanotube or carbon nano-fiber are reused.The patent CN106784732A of Tsinghua University
Using nano-silicon particle as content, using carbon as the preparation method of the powder of the nucleocapsid of shell, there is into the micro- of oxide layer on surface
Meter level silica flour carries out oxygen diffusion, then carries out chemical vapor deposition method and coats one layer of carbon, then is impregnated and removed with hydrofluoric acid solution
Silica ingredient obtains carbon coating silicon nano material.The patent CN102324501B of Chinese Academy Of Sciences Process Engineering Research Institute is then
It is, by the chemical vapor deposition of gaseous state carbon matrix precursor, to be prepared with porous using the porous silicon embedded with copper oxide particle as matrix
The carbon coating silicon based composite material of structure.Patent CN102569804B passes through chemical vapor deposition using organic amine as gaseous precursor
Product technique deposits carbon nitrogen composite layer on graphite material surface, improves graphite material properties.It is vapor-deposited in the carbon packet of particle surface
The method of carbon matrix precursor and negative material mixed pyrolysis is had apparent advantage by coating method compared to solid phase or liquid phase mode, is obtained
Carbon coating there is better uniformity, treatment process also relatively easy economy.But current vapor deposition is carbon-coated
Technology is carried out by the way of powder tiling in the fixed reaction bed of tradition, and the shortcoming of which mainly has at 2 points,
First, the powder of tiling only has exposed surface portion Carbon deposition efficient, and it is low without exposed part deposition efficiency, to powder
For body, when carbon coating amount is larger, deposition uniformity will be deteriorated；Second is that the mode of fixed reaction bed tiling powder leads to list
The material powder of secondary cladding process processing is less, and yield is relatively low, and can not continuous production, seriously hinder vapor deposition carbon coating
The application of technology.
Fluidized-bed chemical vapor deposition technology combines chemical vapor deposition and fluidization technique, is a kind of novel material system
Standby technology.In a fluidized bed, particle is in fluidization under airflow function, and gas reactant enters fluidisation by the form of carrier band
Bed, chemically reacts in high-temperature region, forms superfines or is deposited on particle surface.The initial application of the technology is core combustion
Material field, be mainly used to application and preparation in high temperature gas cooled reactor coated fuel particles (CN204865735U,
CN105139897A, CN103357869B and CN102231291A etc.), subsequently gradually expand to carbon nanotube preparation, polysilicon
It prepares, catalytic carrier and the fields such as powder-modified.United States Patent (USP) US9279181 is by hydrocarbon gas, high warm in a fluidized bed
It decomposes, is deposited on matrix, forms the clad of pyrolytic carbon.The patent only provides the principle stream that fluid bed forms pyrolytic carbon
Journey does not illustrate and specifically how to implement.United States Patent (USP) US6410087 discloses the technique of fluidized bed pyrolysis Carbon deposition and sets
It is standby, detailed setting and constraint carried out for fluidized bed type structure and gas distribution grid, but also without illustrate it is specific such as
What is implemented.
Carbon-coated effect directly affects the chemical property of negative material, summarizes existing negative material carbon coating technology,
Either mechanical-physical mixing, carbon matrix precursor mixed pyrolysis or conventional chemical vapor deposition, cannot achieve efficiently controllable
Carbon coating continuous production.Therefore, there is an urgent need for a kind of high-efficiency and economic, the carbon coating technologies of suitable large-scale production for this field.Fluid bed
Chemical vapour deposition technique embodies advantage in powder body material carbon coating, and fluid bed chemistry gas is based on however, still lacking at present
Phase deposition technique, the specific enforceable the relevant technologies for lithium ion battery negative material carbon cladding.
Invention content
It is negative that carbon coating is generated the purpose of the present invention is to provide a kind of easy to operate, good economy performance, suitable for continuous scale
The system and method for pole material is based on fluidized-bed chemical vapor deposition technology.
To reach this purpose, the specific technical solution of the present invention is as follows：
The present invention's provides a kind of system of lithium ion battery negative material carbon coating modification, and the system comprises feed bins
1, feeding screw 2, preheater inlet valve 3, fluidized bed powder preheater 4, reactor feed valve 5, fluidized-bed reactor 6, anti-
Answer device outlet valve 7, reactor product cooler 8, product collector 9, cold mixture heater 10, first order reaction tail gas cyclone separator 11,
The pre- hot exhaust gas rotation of second order reaction tail gas cyclone separator 12, reaction end gas bagroom 13, reaction end gas burner 14, level-one
The pre- hot exhaust gas cyclone separator 16 of wind separator 15, two level, pre- hot exhaust gas bagroom 17 and preheating exhaust gas cooler 18；
The discharge port of the feed bin 1 is connected with the feed inlet of feeding screw 2, the discharge port of the feeding screw 2
It is connected with the feed inlet of preheater inlet valve 3, discharge port and the fluidized bed powder preheater 4 of the preheater inlet valve 3
Feed inlet is connected, and the air inlet of the fluidized bed powder preheater 4 is connected with the gas outlet of reaction end gas burner 14, stream
The air inlet for changing the pre- hot exhaust gas cyclone separator of the gas outlet of bed Powder Preheater 4 and level-one 15 is connected, the pre- hot exhaust gas of level-one
The air inlet of the pre- hot exhaust gas cyclone separator of the gas outlet of cyclone separator 15 and two level 16 is connected, the pre- hot exhaust gas whirlwind of level-one
The discharge port of separator 15 and the pre- hot exhaust gas cyclone separator of two level 16 is connected with the feed inlet of fluidized bed powder preheater 4,
The gas outlet of the pre- hot exhaust gas cyclone separator of two level 16 is connected with the air inlet of pre- hot exhaust gas bagroom 17, pre- hot exhaust gas
The discharge port of bagroom 17 is connected with the feed inlet of reactor feed valve 5, the outlet of pre- hot exhaust gas bagroom 17
Mouth is connected with the air inlet of preheating exhaust gas cooler 18, discharge port and the reactor feed valve 5 of fluidized bed powder preheater 4
Feed inlet is connected；
The feed inlet of fluidized-bed reactor 6 is connected with the discharge port of reactor feed valve 5, fluidized-bed reactor 6 into
Gas port is connected with the gas outlet of cold mixture heater 10, gas outlet and the first order reaction tail gas whirlwind point of fluidized-bed reactor 6
Air inlet from device 11 is connected, gas outlet and the second order reaction tail gas cyclone separator of first order reaction tail gas cyclone separator 11
12 air inlet is connected, the discharge port of first order reaction tail gas cyclone separator 11 and second order reaction tail gas cyclone separator 12 with
The feed inlet of fluidized-bed reactor 6 is connected, and gas outlet and the reaction end gas cloth bag of second order reaction tail gas cyclone separator 12 are received
The air inlet of dirt device 13 is connected, and the discharge port of reaction end gas bagroom 13 is connected with the feed inlet of fluidized-bed reactor 6
It connects, the gas outlet of reaction end gas bagroom 13 is connected with the air inlet of reaction end gas burner 14, fluidized-bed reactor
(6) discharge port is connected with the feed inlet of reactor outlet valve 7, discharge port and the reactor product cooler 8 of reactor outlet valve 7
Feed inlet is connected, and the discharge port of reactor product cooler 8 is connected with the feed inlet of product collector 9.
A kind of method of lithium ion battery negative material carbon coating modification of the present invention, includes the following steps：
(1) negative electrode material powder enters fluidized bed powder through feeding screw 2 and preheater inlet valve 3 by feed bin 1 and preheats
Device 4 stops certain time, through the pre- hot exhaust gas cyclone separator 15 of level-one, the pre- hot exhaust gas cyclone separator 16 of two level and pre- hot exhaust gas
Bagroom 17 returns to fluidized bed powder preheater 4 after collecting；After the discharge of the discharge port of fluidized bed powder preheater 4, warp
Reactor feed valve 5 enters fluidized-bed reactor 6 and stops certain time, anti-through first order reaction tail gas cyclone separator 11, two level
Fluidized-bed reactor 6 is returned to after answering tail gas cyclone separator 12 and reaction end gas bagroom 13 to collect；From fluidized-bed reaction
After the discharge port discharge of device 6, reacted device outlet valve 7 is cooled down into reactor product cooler 8, enters product collector after cooling
9。
(2) gaseous mixture is anti-into fluidized bed from the air inlet of fluidized-bed reactor 6 after the preheating of cold mixture heater 10
Device 6 is answered, vapor deposition reaction is carried out in fluidized-bed reactor 6 so that carbon coating is in powder surface, then from fluidized-bed reactor
6 gas outlet discharge, sequentially enters first order reaction tail gas cyclone separator 11 and second order reaction tail gas cyclone separator 12, through dividing
It is discharged from the gas outlet of second order reaction tail gas cyclone separator 12 from after, reacted tail gas bagroom 13 enters reaction end gas
Burner 14, in right amount with addition of air and coal gas after burning is handled, the gas being discharged from 14 gas outlet of reaction end gas burner, one
Air inlet of the part through fluidized bed powder preheater 4 enters fluidized bed powder preheater 4, preheated material powder, then from fluid bed
The gas outlet of Powder Preheater 4 is discharged, and sequentially enters the pre- hot exhaust gas cyclone separator 15 of level-one and the pre- hot exhaust gas whirlwind of two level point
From device 16, it is discharged from the gas outlet of the pre- hot exhaust gas cyclone separator of two level 16 after separation, preheated tail gas bagroom 17
It into preheating exhaust gas cooler 18, is discharged after cooling, the gas being discharged from 14 gas outlet of reaction end gas burner, another part is logical
It crosses cold mixture heater 10 to exchange heat, preheats gaseous mixture, the gas of discharge is directly entered preheating exhaust gas cooler 18, after cooling
Discharge.
Preferably, the negative material is one kind in carbon-based graphite, silicon substrate and lithium titanate base negative material.
Preferably, the mass percent of the carbon coated is 1~10%, is preferably further 2~5%.
Preferably, the preheating temperature in the fluidized bed powder preheater 4 is 250~900 DEG C, and the material powder is flowing
It is 10~30min to change the residence time in bed Powder Preheater 4.
Preferably, the reaction temperature in the fluidized-bed reactor 6 is 400~1200 DEG C.Further, the fluid bed is anti-
It is 500~800 DEG C to answer the reaction temperature in device 6 preferably.Residence time of the material powder in fluidized-bed reactor 6 be
3~120min, further, residence time of the material powder in fluidized-bed reactor 6 are preferably 5~30min.
Preferably, the gaseous mixture is the mixed gas of carbon-source gas and inert gas, and the volume of wherein carbon-source gas is dense
Degree is 5~30%.The carbon-source gas can be one kind or at least two in methane, ethane, ethylene, propylene, acetylene, propine
Combination.The inert gas can be the combination of one kind or at least two in nitrogen, helium, argon gas, neon.
Preferably, the discharge of reaction end gas burner 14 gas enters fluidized bed powder preheater 4 and charge heating
The volume ratio of device 10 is 1:1~1:4.
Carbon coating negative material prepared by the present invention has carbon coating pattern controllable, and carbon coating amount is controllable, electrochemistry
The advantages that haveing excellent performance.The carbon-coated method of negative material provided by the invention, it is of the invention compared to existing carbon coating technology
Advantage is：
(1) fluidized bed plant and method can make negative electrode material powder uniformly quick particulate fluidization, and fine powder difficulty is overcome to fluidize
The shortcomings that；
(2) fluidized-bed reactor bed-type it is simple, it is easily controllable and amplification.Each device of system belongs to chemical industry routine model
Specification, is not necessarily to specific customization, and system economy is good；
(3) vapor deposition reaction carries out in a fluidized bed, and gas-solid contact is abundant, and reaction efficiency is high, and the reaction time is short；
(4) the controllable cladding of negative material surface carbon may be implemented in carbon coating method, you can be adjusted by experiment parameter
The performance regulation and control for realizing carbon coating layer, include the covered effect and covering amount of carbon.
Description of the drawings
Fig. 1 is negative material carbon coating process flow diagram provided by the invention；
Fig. 2 is the carbon coating silicon materials particle photo of embodiment 3 provided by the invention；
Fig. 3 is the sub- silicon materials particle photo of carbon coating oxidation of embodiment 4 provided by the invention；
Fig. 4 is the sub- silicon materials particle photo of carbon coating oxidation of embodiment 6 provided by the invention；
Fig. 5 is the carbon coating graphite material particle photo of embodiment 7 provided by the invention.
Reference numeral：
1, feed bin；2, feeding screw；3, preheater inlet valve；4, fluidized bed powder preheater；5, reactor feed valve；
6, fluidized-bed reactor；7, reactor outlet valve；8, reactor product cooler；9, product collector；10, cold mixture heater；11, one
Order reaction tail gas cyclone separator；12, second order reaction tail gas cyclone separator；13, reaction end gas bagroom；14, it reacts
Tail gas burner；15, the pre- hot exhaust gas cyclone separator of level-one；16, the pre- hot exhaust gas cyclone separator of two level；17, pre- hot exhaust gas cloth
Bag collector；18, exhaust gas cooler is preheated.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the attached drawing of the present invention, to this hair
Technical solution in bright embodiment carries out clear and complete description, but is not limited to protection scope of the present invention：
Embodiment 1
A kind of system of lithium ion battery negative material carbon coating modification
As shown in Figure 1, described device system include sequentially connected feed bin 1, feeding screw 2, preheater inlet valve 3,
Fluidized bed powder preheater 4, reactor feed valve 5, fluidized-bed reactor 6, reactor outlet valve 7, reactor product cooler 8, product
Collector 9, cold mixture heater 10, first order reaction tail gas cyclone separator 11, second order reaction tail gas cyclone separator 12, reaction
The pre- hot exhaust gas cyclone separator 15 of tail gas bagroom 13, reaction end gas burner 14, level-one, the pre- hot exhaust gas whirlwind of two level point
From device 16, pre- hot exhaust gas bagroom 17 and preheating exhaust gas cooler 18；
The discharge port of the feed bin 1 is connected with the feed inlet of feeding screw 2, the discharge port of the feeding screw 2
It is connected with the feed inlet of preheater inlet valve 3, discharge port and the fluidized bed powder preheater 4 of the preheater inlet valve 3
Feed inlet is connected, and the air inlet of the fluidized bed powder preheater 4 is connected with the gas outlet of reaction end gas burner 14, stream
The air inlet for changing the pre- hot exhaust gas cyclone separator of the gas outlet of bed Powder Preheater 4 and level-one 15 is connected, the pre- hot exhaust gas of level-one
The air inlet of the pre- hot exhaust gas cyclone separator of the gas outlet of cyclone separator 15 and two level 16 is connected, the pre- hot exhaust gas whirlwind of level-one
The discharge port of separator 15 and the pre- hot exhaust gas cyclone separator of two level 16 is connected with the feed inlet of fluidized bed powder preheater 4,
The gas outlet of the pre- hot exhaust gas cyclone separator of two level 16 is connected with the air inlet of pre- hot exhaust gas bagroom 17, pre- hot exhaust gas
The discharge port of bagroom 17 is connected with the feed inlet of reactor feed valve 5, the outlet of pre- hot exhaust gas bagroom 17
Mouth is connected with the air inlet of preheating exhaust gas cooler 18, discharge port and the reactor feed valve 5 of fluidized bed powder preheater 4
Feed inlet is connected；
The feed inlet of fluidized-bed reactor 6 is connected with the discharge port of reactor feed valve 5, fluidized-bed reactor 6 into
Gas port is connected with the gas outlet of cold mixture heater 10, gas outlet and the first order reaction tail gas whirlwind point of fluidized-bed reactor 6
Air inlet from device 11 is connected, gas outlet and the second order reaction tail gas cyclone separator of first order reaction tail gas cyclone separator 11
12 air inlet is connected, the discharge port of first order reaction tail gas cyclone separator 11 and second order reaction tail gas cyclone separator 12 with
The feed inlet of fluidized-bed reactor 6 is connected, and gas outlet and the reaction end gas cloth bag of second order reaction tail gas cyclone separator 12 are received
The air inlet of dirt device 13 is connected, and the discharge port of reaction end gas bagroom 13 is connected with the feed inlet of fluidized-bed reactor 6
It connects, the gas outlet of reaction end gas bagroom 13 is connected with the air inlet of reaction end gas burner 14, fluidized-bed reactor 6
Discharge port be connected with the feed inlet of reactor outlet valve 7, the discharge port of reactor outlet valve 7 and reactor product cooler 8 into
Material mouth is connected, and the discharge port of reactor product cooler 8 is connected with the feed inlet of product collector 9.
Embodiment 2
A kind of method of lithium ion battery negative material carbon coating modification
The method of the coated modified carbon, includes the following steps：Negative electrode material powder is by feed bin 1 through 2 He of feeding screw
Preheater inlet valve 3 enters fluidized bed powder preheater 4 and stops certain time, through the pre- hot exhaust gas cyclone separator of level-one 15, two
The pre- hot exhaust gas cyclone separator 16 of grade and pre- hot exhaust gas bagroom 17 return to fluidized bed powder preheater 4 after collecting；From stream
After the discharge port discharge for changing bed Powder Preheater 4, reacted device inlet valve 5 enters fluidized-bed reactor 6 and stops certain time, warp
After first order reaction tail gas cyclone separator 11, second order reaction tail gas cyclone separator 12 and reaction end gas bagroom 13 are collected
Return to fluidized-bed reactor 6；After the discharge of the discharge port of fluidized-bed reactor 6, reacted device outlet valve 7 enters reactor product cooler
8 are cooled down, and enter product collector 9 after cooling.
Gaseous mixture enters fluidized-bed reactor after the preheating of cold mixture heater 10 from the air inlet of fluidized-bed reactor 6
6, vapor deposition reaction is carried out in fluidized-bed reactor 6 so that carbon coating is in powder surface, then from fluidized-bed reactor 6
Gas outlet is discharged, and sequentially enters first order reaction tail gas cyclone separator 11 and second order reaction tail gas cyclone separator 12, through separation
It is discharged afterwards from the gas outlet of second order reaction tail gas cyclone separator 12, reacted tail gas bagroom 13 enters reaction end gas and fires
Burner 14, in right amount with addition of air and coal gas after burning is handled, the gas being discharged from 14 gas outlet of reaction end gas burner, one
The air inlet of lease making fluidized bed powder preheater 4 enters fluidized bed powder preheater 4, preheated material powder, then from fluid bed powder
The gas outlet of body preheater 4 is discharged, and sequentially enters the pre- hot exhaust gas cyclone separator 15 of level-one and the pre- hot exhaust gas cyclonic separation of two level
Device 16 is discharged after separation from the gas outlet of the pre- hot exhaust gas cyclone separator of two level 16, preheated tail gas bagroom 17 into
Enter to preheat exhaust gas cooler 18, discharged after cooling, the gas being discharged from 14 gas outlet of reaction end gas burner, another part passes through
Cold mixture heater 10 exchanges heat, and preheats gaseous mixture, and the gas of discharge is directly entered preheating exhaust gas cooler 18, cooling heel row
It puts.
Embodiment 3
Using the modified technique described in embodiment 2, by silicon materials by feed bin 1 through feeding screw 2 and preheater inlet valve 3
Into being preheated in fluidized bed powder preheater 4, preheating temperature is 900 DEG C, preheating time 10min, the material after preheating
The reacted device inlet valve 5 of powder enters fluidized-bed reactor 6, and the gaseous mixture of methane/argon gas (volume percent methane 25%) is logical
Cross cold mixture heater 10, it is preheated after gaseous mixture be uniformly passed through by 6 bottom inlet of fluidized-bed reactor, make fluidized-bed reaction
Silicon powder in device 6 is in fluidized state.Gaseous mixture comes into full contact with silicon powder in a fluidized bed, the behaviour of fluidized-bed reactor 6
Make temperature control at 1200 DEG C, the residence time of silicon powder in a fluidized bed is 10min.Silicon powder after reaction is by fluid bed bottom
Portion is flowed out, and is discharged into cooling in reactor product cooler 8 by reactor outlet valve 7, is entered product collector 9 after cooling, prepare carbon
Coated Si negative material, wherein carbon coating amount are 3%.
Embodiment 4
Using the modified technique described in embodiment 2, the sub- silicon of oxidation is fed by feed bin 1 through feeding screw 2 and preheater
Valve 3, which enters in fluidized bed powder preheater 4, to be preheated, and preheating temperature is 250 DEG C, preheating time 30min, the material after preheating
The reacted device inlet valve 5 of feed powder body enters fluidized-bed reactor 6, and the gaseous mixture of acetylene/nitrogen (acetylene volumetric concentration is 5%) is logical
Cross cold mixture heater 10, it is preheated after gaseous mixture be uniformly passed through by 6 bottom inlet of fluidized-bed reactor, make fluidized-bed reaction
Oxidation Asia silicon in device 6 is in fluidized state.Gaseous mixture comes into full contact with the sub- silicon of oxidation in a fluidized bed, fluidized-bed reactor 6
Operation temperature control at 400 DEG C, it is 3min to aoxidize the residence time of sub- silicon in a fluidized bed.Oxidation Asia silicon after reaction is by flowing
Change the outflow of bed bottom, cooling in reactor product cooler 8 is discharged by reactor outlet valve 7, product collector 9, system are entered after cooling
For the sub- silicium cathode material of carbon coating oxidation is gone out, wherein carbon coating amount is 1%.
Embodiment 5
Using the modified technique described in embodiment 2, by lithium titanate by feed bin 1 through feeding screw 2 and preheater inlet valve 3
Into being preheated in fluidized bed powder preheater 4, preheating temperature is 400 DEG C, preheating time 20min, the material after preheating
The reacted device inlet valve 5 of powder enters fluidized-bed reactor 6, and (gaseous mixture of a concentration of 15%) of volume of ethylene is logical for ethylene/helium
Cross cold mixture heater 10, it is preheated after gaseous mixture be uniformly passed through by 6 bottom inlet of fluidized-bed reactor, make fluidized-bed reaction
Lithium titanate in device 6 is in fluidized state.Gaseous mixture comes into full contact with lithium titanate in a fluidized bed, the behaviour of fluidized-bed reactor 6
Make temperature control at 550 DEG C, the residence time of lithium titanate in a fluidized bed is 10min.Lithium titanate after reaction is by fluid bed bottom
Portion is flowed out, and is discharged into cooling in reactor product cooler 8 by reactor outlet valve 7, is entered product collector 9 after cooling, prepare carbon
Lithium titanate anode material is coated, wherein carbon coating amount is 3%.
Embodiment 6
Using the modified technique described in embodiment 2, the sub- silicon of oxidation is fed by feed bin 1 through feeding screw 2 and preheater
Valve 3, which enters in fluidized bed powder preheater 4, to be preheated, and preheating temperature is 600 DEG C, preheating time 13min, the material after preheating
The reacted device inlet valve 5 of feed powder body enters fluidized-bed reactor 6, the gaseous mixture of ethane/neon (ethane volumetric concentration is 30%)
By cold mixture heater 10, it is preheated after gaseous mixture be uniformly passed through by 6 bottom inlet of fluidized-bed reactor, keep fluid bed anti-
The oxidation Asia silicon in device 6 is answered to be in fluidized state.Gaseous mixture comes into full contact with the sub- silicon of oxidation in a fluidized bed, fluidized-bed reactor
6 operation temperature is controlled at 800 DEG C, and the residence time of the sub- silicon of oxidation in a fluidized bed is 60min.Oxidation Asia silicon after reaction by
Fluidized-bed bottom flows out, and is discharged into cooling in reactor product cooler 8 by reactor outlet valve 7, enters product collector 9 after cooling,
The sub- silicium cathode material of carbon coating oxidation is prepared, wherein carbon coating amount is 8%.
Embodiment 7
Using the modified technique described in embodiment 2, by graphite by feed bin 1 through feeding screw 2 and preheater inlet valve 3 into
It is preheated in fluidized bed Powder Preheater 4, preheating temperature is 680 DEG C, preheating time 11min, the material powder after preheating
The reacted device inlet valve 5 of body enters fluidized-bed reactor 6, and the gaseous mixture of propylene/nitrogen (propylene volumetric concentration is 20%) passes through
Cold mixture heater 10, it is preheated after gaseous mixture be uniformly passed through by 6 bottom inlet of fluidized-bed reactor, make fluidized-bed reactor
Graphite in 6 is in fluidized state.Gaseous mixture comes into full contact with graphite in a fluidized bed, the operation temperature of fluidized-bed reactor 6
At 850 DEG C, the residence time of graphite in a fluidized bed is 25min for control.Graphite after reaction is flowed out by fluidized-bed bottom, is passed through
Reactor outlet valve 7 is discharged into cooling in reactor product cooler 8, enters product collector 9 after cooling, prepares carbon coating graphite cathode
Material, wherein carbon coating amount are 4%.
Embodiment 8
Using the modified technique described in embodiment 2, by silicon materials by feed bin 1 through feeding screw 2 and preheater inlet valve 3
Into being preheated in fluidized bed powder preheater 4, preheating temperature is 700 DEG C, preheating time 10min, the material after preheating
The reacted device inlet valve 5 of powder enters fluidized-bed reactor 6, and the gaseous mixture of propine/argon gas (propine volumetric concentration is 10%) is logical
Cross cold mixture heater 10, it is preheated after gaseous mixture be uniformly passed through by 6 bottom inlet of fluidized-bed reactor, make fluidized-bed reaction
Silicon powder in device 6 is in fluidized state.Gaseous mixture comes into full contact with silicon powder in a fluidized bed, the behaviour of fluidized-bed reactor 6
Make temperature control at 900 DEG C, the residence time of silicon powder in a fluidized bed is 120min.Silicon powder after reaction is by fluid bed bottom
Portion is flowed out, and is discharged into cooling in reactor product cooler 8 by reactor outlet valve 7, is entered product collector 9 after cooling, prepare carbon
Coated Si negative material, wherein carbon coating amount are 10%.
It should be noted last that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting.Although ginseng
It is described the invention in detail according to embodiment, it will be understood by those of ordinary skill in the art that, to the technical side of the present invention
Case is modified or replaced equivalently, and without departure from the spirit and scope of technical solution of the present invention, should all be covered in the present invention
Right in.
Claims (9)
1. a kind of system of lithium ion battery negative material carbon coating modification, which is characterized in that the system comprises feed bin (1),
Feeding screw (2), preheater inlet valve (3), fluidized bed powder preheater (4), reactor feed valve (5), fluidized-bed reaction
Device (6), reactor outlet valve (7), reactor product cooler (8), product collector (9), cold mixture heater (10), first order reaction tail
Cyclonic wind separator (11), second order reaction tail gas cyclone separator (12), reaction end gas bagroom (13), reaction end gas combustion
The pre- hot exhaust gas cyclone separator (15) of burner (14), level-one, the pre- hot exhaust gas cyclone separator (16) of two level, pre- hot exhaust gas cloth bag are received
Dirt device (17) and preheating exhaust gas cooler (18)；
The discharge port of the feed bin (1) is connected with the feed inlet of feeding screw (2), the discharging of the feeding screw (2)
Mouth is connected with the feed inlet of preheater inlet valve (3), and discharge port and the fluidized bed powder of the preheater inlet valve (3) preheat
The feed inlet of device (4) is connected, the outlet of the air inlet and reaction end gas burner (14) of the fluidized bed powder preheater (4)
Mouth is connected, and the gas outlet of fluidized bed powder preheater (4) is connected with the air inlet of the pre- hot exhaust gas cyclone separator (15) of level-one
It connects, the gas outlet of the pre- hot exhaust gas cyclone separator (15) of level-one is connected with the air inlet of the pre- hot exhaust gas cyclone separator (16) of two level
It connects, the discharge port and fluidized bed powder of the pre- hot exhaust gas cyclone separator (15) of level-one and the pre- hot exhaust gas cyclone separator (16) of two level
The feed inlet of preheater (4) is connected, gas outlet and the pre- hot exhaust gas bag collection of the pre- hot exhaust gas cyclone separator (16) of two level
The air inlet of device (17) is connected, the feed inlet of the discharge port and reactor feed valve (5) of pre- hot exhaust gas bagroom (17)
It is connected, the gas outlet of pre- hot exhaust gas bagroom (17) is connected with the air inlet of preheating exhaust gas cooler (18), fluidizes
The discharge port of bed Powder Preheater (4) is connected with the feed inlet of reactor feed valve (5)；
The feed inlet of fluidized-bed reactor (6) is connected with the discharge port of reactor feed valve (5), fluidized-bed reactor (6)
Air inlet is connected with the gas outlet of cold mixture heater (10), gas outlet and the first order reaction tail gas of fluidized-bed reactor (6)
The air inlet of cyclone separator (11) is connected, gas outlet and the second order reaction tail gas of first order reaction tail gas cyclone separator (11)
The air inlet of cyclone separator (12) is connected, first order reaction tail gas cyclone separator (11) and second order reaction tail gas cyclonic separation
The discharge port of device (12) is connected with the feed inlet of fluidized-bed reactor (6), and second order reaction tail gas cyclone separator (12) go out
Gas port is connected with the air inlet of reaction end gas bagroom (13), the discharge port and stream of reaction end gas bagroom (13)
The feed inlet of fluidized bed reactor (6) is connected, gas outlet and the reaction end gas burner of reaction end gas bagroom (13)
(14) air inlet is connected, and the discharge port of fluidized-bed reactor (6) is connected with the feed inlet of reactor outlet valve (7), instead
The discharge port of device outlet valve (7) is answered to be connected with the feed inlet of reactor product cooler (8), the discharge port of reactor product cooler (8) and production
The feed inlet of product collector (9) is connected.
2. a kind of method of lithium ion battery negative material carbon coating modification, includes the following steps：
(1) negative electrode material powder is pre- into fluidized bed powder through feeding screw (2) and preheater inlet valve (3) by feed bin (1)
Hot device (4) stops certain time, through the pre- hot exhaust gas cyclone separator (15) of level-one, the pre- hot exhaust gas cyclone separator (16) of two level and
Pre- hot exhaust gas bagroom (17) returns to fluidized bed powder preheater (4) after collecting；From going out for fluidized bed powder preheater (4)
After material mouth discharge, reacted device inlet valve (5) enters fluidized-bed reactor (6) and stops certain time, is revolved through first order reaction tail gas
Wind separator (11), second order reaction tail gas cyclone separator (12) and reaction end gas bagroom (13) return to fluidisation after collecting
Bed reactor (6)；After the discharge of the discharge port of fluidized-bed reactor (6), reacted device outlet valve (7) enters reactor product cooler
(8) it is cooled down, enters product collector (9) after cooling；
(2) gaseous mixture is anti-into fluidized bed from the air inlet of fluidized-bed reactor (6) after cold mixture heater (10) preheating
Device (6) is answered, vapor deposition reaction is carried out in fluidized-bed reactor (6) so that carbon coating is anti-in powder surface, then from fluid bed
It answers the gas outlet of device (6) to be discharged, sequentially enters first order reaction tail gas cyclone separator (11) and second order reaction tail gas cyclonic separation
Device (12) is discharged after separation from the gas outlet of second order reaction tail gas cyclone separator (12), reacted tail gas bagroom
(13) go out into reaction end gas burner (14) from reaction end gas burner (14) with addition of air and coal gas after burning is handled
The gas of gas port discharge, a part of air inlet through fluidized bed powder preheater (4) enter fluidized bed powder preheater (4), in advance
Hot material powder, then be discharged from the gas outlet of fluidized bed powder preheater (4), sequentially enter the pre- hot exhaust gas cyclone separator of level-one
(15) and the pre- hot exhaust gas cyclone separator (16) of two level, from the gas outlet of the pre- hot exhaust gas cyclone separator (16) of two level after separation
Discharge, preheated tail gas bagroom (17) enter preheating exhaust gas cooler (18), are discharged after cooling, burnt from reaction end gas
The gas of device (14) gas outlet discharge, another part are exchanged heat by cold mixture heater (10), preheat gaseous mixture, discharge
Gas is directly entered preheating exhaust gas cooler (18), is discharged after cooling.
3. the method for lithium ion battery negative material carbon coating modification according to claim 2, which is characterized in that described negative
Pole material is one kind in carbon-based graphite, silicon substrate and lithium titanate base negative material.
4. the method for lithium ion battery negative material carbon coating modification according to claim 2, which is characterized in that the packet
The mass percent for covering carbon is 1~10%.
5. the method for lithium ion battery negative material carbon coating modification according to claim 2, which is characterized in that the stream
The preheating temperature changed in bed Powder Preheater (4) is 250~900 DEG C, and the material powder is in fluidized bed powder preheater (4)
Residence time be 10~30min.
6. the method for lithium ion battery negative material carbon coating modification according to claim 2, which is characterized in that the stream
Reaction temperature in fluidized bed reactor (6) is 400~1200 DEG C, stop of the material powder in fluidized-bed reactor (6)
Time is 3~120min.
7. the method for lithium ion battery negative material carbon coating modification according to claim 2, which is characterized in that described mixed
The mixed gas that gas is carbon-source gas and inert gas is closed, the wherein volumetric concentration of carbon-source gas is 5~30%.
8. the method for lithium ion battery negative material carbon coating modification according to claim 7, which is characterized in that the carbon
Source gas can be the combination of one kind or at least two in methane, ethane, ethylene, propylene, acetylene, propine, the indifferent gas
Body can be the combination of one kind or at least two in nitrogen, helium, argon gas, neon.
9. the method for lithium ion battery negative material carbon coating modification according to claim 2, which is characterized in that described anti-
It is 1 to answer tail gas burner (14) discharge gas to enter fluidized bed powder preheater (4) and the volume ratio of cold mixture heater (10):
1~1:4.
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