CN107601448A - A kind of lithium iron phosphate positive material preparation technology and device - Google Patents
A kind of lithium iron phosphate positive material preparation technology and device Download PDFInfo
- Publication number
- CN107601448A CN107601448A CN201710767835.3A CN201710767835A CN107601448A CN 107601448 A CN107601448 A CN 107601448A CN 201710767835 A CN201710767835 A CN 201710767835A CN 107601448 A CN107601448 A CN 107601448A
- Authority
- CN
- China
- Prior art keywords
- raw material
- homogenizing
- tower
- product
- nanosizing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A kind of lithium iron phosphate positive material preparation technology and device, technique include：The step of LiFePO4 raw material nanoization is homogenized；The step of material that nanosizing raw material pyroreaction is generated is through cooling down tower cooler；The step of material particles after cooling are homogenized；Wherein, nanosizing homogenizing refers to the particle that raw material is ground into 0.1 100nm sizes, and nanosizing raw material pyroreaction is continuous reaction.1）This technique is using continuous high temperature solid phase method production LiFePO4, and the material continuously conveyed in screw reactor improves heat utilization rate, and compares traditional approach, and raw material mixing uniformity is good, and material reaction is uniform；2）The raw material of nanosizing homogenizing improves the efficiency for charge-discharge and stability 3 of positive electrode）The present apparatus replaces traditional batch (-type) firing equipment using screw reactor（Such as kiln）, power consumption is reduced, and reaction stability is good.
Description
Technical field
The present invention relates to lithium iron phosphate positive material preparing technical field, more particularly, to a kind of lithium iron phosphate positive material
Preparation facilities, further relate to the preparation technology of the material.
Background technology
In recent years, as progressively attention of the people to environmental issue, requirement of the country to environmental protection improve constantly, new energy vapour
Car and energy storage market develop rapidly, and the high security, high uniformity, high qualification rate and low manufacturing cost to battery propose higher
Requirement.As the positive electrode of lithium ion battery, cobalt acid lithium, LiMn2O4 and its derivative are own to have obtained business through different degrees of
Industry.Certainly, for conventional lithium ion battery positive electrode the defects of, people are endeavouring to study continuous improved performance always, but
It is, for electric automobile and high capacity battery, the utilization rate of battery, the price of positive electrode and the energy of rupture to environment
Power is all very important factor.Therefore, as most promising anode material for lithium-ion batteries, LiFePO4 is due to tool
There is the features such as height ratio capacity, cycle performance are good, security is good, cost is cheap, pollution-free, attracted a large amount of scholars and industry circle
Concern, and the important kind of anode material for lithium-ion batteries of new generation.
LiFePO4It is rhombic system for olivine-type structure, belongs to Pbmn space groups, Fe and Li forms FeO6And LiO6Octahedral
Body, p-shaped is into PO4Tetrahedron.The Li+ parallel with c-axis for continuous linear chain, two-dimensional diffusion can be formed along c-axis and be moved, from
Deviate from by ground or embedded.Theoretical capacity is 170mAh/g, and actual capacity only has 81% of theoretical capacity or so.It is low with price
Honest and clean, the advantages that chemical property is good, environmentally friendly pollution-free.
And research of most of researchers to LiFePO4 is concentrated mainly on three aspects：
1. in order to improve the measure that the electric conductivity of LiFePO4 is taken：Mainly there are carbon coating and metal ion mixing.
2. in order to improve the diffusion velocity of lithium ion, so as to change the measure that charging rate is taken：Need to control particle
Particle diameter.
3. for the measure for controlling purity to be done：Need to add inert gas shielding during the course of the reaction, controlling reaction temperature,
Relatively low reaction temperature not only makes that finished product grain size is small, and ferric iron content is low, and avoidable formation.
The preparation method of lithium iron phosphate positive material generally has two kinds of solid phase method and liquid phase method, because liquid phase method can cause greatly
The industrial wastewater of amount, so solid phase method is most common industrialized method.Solid phase method can be divided into high temperature solid-state method, carbon heat also again
A variety of different methods such as former method and iron oxide red method, because high temperature solid-state method has, cost of material is low, and the advantage such as easy to operation, is very
The selection of more factories.Traditional high temperature solid-state method technics comparing falls behind, including：Mixing raw materials --- raw mill --- roast
Burn --- middle product grinding --- screening --- carbon coating --- roasting --- finished product grinding --- finished product screening --- product etc.
Technological process.
In above-mentioned technique, mixing raw materials and homogenizing typically be high-speed mixer, high-speed mixer has its advantage, but
It is that the operation of batch (-type) easily causes unstable between batch and with a batch of non-uniformity.Raw material mixing is uneven to be caused
React uneven, product mix is uneven to cause product chemical property poor.And chemical property is to weigh positive electrode quality
A critically important index.
The roasting various forms of resistance furnaces such as equipment such as roller kilns, pushed bat kiln, rotary furnace.Roaster：1) hot blast is passed through
Heat transfer, heat transfer are washed one's face and rinsed one's mouth only 20 kilocalories/m3.h. DEG C, and the thermal efficiency is extremely low, and generally only 50%, therefore high energy consumption；2) invest
Greatly, producing 5000 tons of LiFePO4s per year at least needs 4 heating furnace production lines, invests more than 30,000,000 yuan；3) protect gas dosage big,
Positive electrode does not have immixture on pallet in stove, the uniformity of material is produced a very large impact, so as to have influence on its electrification
Learn performance and the specific capacity of final products；4) because gas production is big, the compacted density of material can not ensure, have influence on making for product
With performance, substantial amounts of gas can not be reclaimed, is directly discharged in air, cause the pollution of air.
Grinding is typically using equipment such as airflow milling, ball mill, nanometer sand mills；And abradant equipment crushing knife will be used
Zirconium or zirconium oxide, will also use zirconium pearl during crushing, overall price is high.Particle diameter after ball milling is 2 μm or so.And phosphorus
The sour elongated 6.63nm of iron lithium average grain diameter, and particle diameter 2000nm raw material is difficult uniformly to mix, so using solid phase method, raw material grain
Footpath is bigger, and the actual capacity of the LiFePO 4 material of synthesis is lower.The problem of ball mill processing product brings maximum is exactly product
Particle diameter distribution is wide, and a big chunk product causes that the yield rate of product is low, and cost enters one because particle diameter is improper just goes out of use
Step increase.
Screening is general to use vibratory sieve, and the product of the last batch remained on vibratory sieve is another that cause product uneven
Defect.
It is varied in terms of the species of LiFePO4 raw material.Liu Xu is identical to use FeC2O4·2H2O、Fe2O3、FeCl3Etc. original
Expect to synthesize LiFePO for source of iron4/ C specific discharge capacity is 152.2mAh/g, 133.8mAh/g and 122.5mAh/g respectively.At present
The country generally uses ferric phosphate synthesizing iron lithium phosphate, and must be added to excessive carbon source with ferric phosphate reaction, using ferric phosphate
One of reason is because ferric phosphate can accomplish nanoscale, so that the specific capacity increase of product.Cong Changjie etc. is sunk using liquid phase
Shallow lake method synthesis nano ferric phosphate, and as source of iron, pass through the nanometer spherical iron phosphate lithium of carbothermic method preparation uniform particle sizes
Positive electrode.Material first discharge specific capacity reaches 161.8mAh/g, coulombic efficiency 98.3%.Liu etc. is by CH3COOLi·
2H2O、Fe2O3、Fe、NH4H2PO4With 3：1：1：3 ratio and the mixing of appropriate citric acid, are consolidated under hydrogen atmosphere by traditional
Phase synthesi has synthesized 50-70nm LiFePO4/ C, first charge-discharge capacity have reached 162.4mAh/g.Huang etc. is by carbon
Gel mixes with lithium acetate, ferrous acetate, ammonium dihydrogen phosphate, is mixed through molecular level, by two-step thermal processing, finally gives
LiFePO4/ C composite, specific discharge capacity 163mAh/g under 0.1C multiplying powers, and capacity attenuation only has 8% after circulating 800 times.
Jiang Zhengfu etc. is using sol method synthesis nano LiMn0.9Fe0.1PO4, its charge specific capacity 174mAh/g, specific discharge capacity
160mAh/g, average grain diameter 95nm.Research gorgeous Chen Hong shows：Raw material particle size is smaller, and charging and discharging capacity is higher, discharge and recharge effect
Rate is also higher.But her research is limited to micron order raw material.
Above example shows：Positive electrode raw material nano, homogenization can effectively improve the charge and discharge electric capacity of positive electrode
Amount and stability.Because raw material particle size is smaller, electrical property is better.Nano-scale particle has special property, specific surface area
Higher, interparticle contact is more preferable, mixes to each other evenly.
The content of the invention
It is an object of the invention to overcome shortcoming present in prior art, there is provided prepared by a kind of lithium iron phosphate positive material
Technique, the technique is using nanometer homogenizing raw material and realizes continuous high-temperature solid phase reaction, and present invention also offers one kind to realize
The device of above-mentioned preparation technology, the technical scheme of use are：A kind of lithium iron phosphate positive material preparation technology, it is characterised in that：
The preparation technology includes：The step of LiFePO4 raw material nanoization is homogenized；The thing that nanosizing raw material pyroreaction is generated
The step of material is through cooling down tower cooler；The step of material particles after cooling are homogenized；Wherein, nanosizing homogenizing refers to crush raw material
Into the particle of 0.1-100nm sizes, nanosizing raw material pyroreaction is continuous reaction.
The technical characteristic of the present invention also has：The continuous reaction is carried out in screw reactor, screw reactor
Reaction temperature be 600-750 DEG C.
The technical characteristic of the present invention also has：Raw material source of iron is FeC2O4·2H2O,FeC2O4Or (CH3COO)2Fe, raw material phosphor
Source is NH4H2PO4Or (NH4)2HPO4, raw material lithium source is Li2CO3, LiOH or Li3PO4。
The technical characteristic of the present invention also has：The LiFePO4 raw material nanoization homogenizing refers to raw material being well mixed, and
All mixed raw materials are processed into particle diameter 0.1-100nm particle.
Technical scheme also has：A kind of device for above-mentioned preparation technology, described device include material homogenizer
Partly, pyroreaction cooling segment and product homogenizing part, it is characterised in that：The pyroreaction cooling segment includes screw
Reactor, the screw reactor connect cooling tower.
The technical characteristic of the present invention also has：The screw reactor is what more than two screw reactors were in series
Multi-stage screw formula reactor.
The technical characteristic of the present invention also has：The material homogenizer part includes nanometer homogenizing tower, nanometer homogenizing tower with
Raw material measuring tank is connected, and the nanometer homogenizing tower is also connected with cyclone, is stored up among the output end connection of the nanometer homogenizing tower
Tank, the outlet connection plate and frame filter press of the intermediate storage tank, the hopper of the plate and frame filter press connection feeding spiro rod, the conveying
Screw rod is also connected with desolventizing machine, the desolventizing machine connection mixed material storehouse.
The technical characteristic of the present invention also has：The desolventizing machine is also connected with condenser, and the condenser connection solvent receives
Tank, the solvent receiving tank connect solvent recovery tank, and the solvent recovery tank also pipeline connects the plate and frame filter press, described molten
Agent receiving tank is also connected with trapping heat exchanger.
The technical characteristic of the present invention also has：The product homogenizing part includes product homogenizing tower, and the product homogenizing tower connects
Connect separator, the overfall connection product pans of the separator, the heavy burder discharging opening connection product homogenizing of the separator
Tower.
The technical characteristic of the present invention also has：The product homogenizing part also includes solvent measuring tank, and the measuring tank goes out
Mouth end connects the product homogenizing tower, is homogenized in the product on the connecting line between tower and measuring tank and sets displacement pump.
The beneficial effects of the present invention are：1) this technique is using continuous high temperature solid phase method production LiFePO4, continuously in spiral shell
The material conveyed in rod-type reactor improves heat utilization rate, and compares traditional approach, and raw material mixing uniformity is good, and material is anti-
Should be uniform；2) raw material of nanosizing homogenizing improves the efficiency for charge-discharge and stability 3 of positive electrode) present apparatus uses screw
Reactor replaces traditional batch (-type) firing equipment (such as kiln), reduces power consumption, and reaction stability is good.
Brief description of the drawings
Accompanying drawing 1 is raw material nanoization homogenizing schematic flow sheet of the present invention, and accompanying drawing 2 is pyroreaction technique of the present invention and product
Homogenizing process schematic flow sheet, 11 be raw material measuring tank, and 12 be nanometer homogenizing tower, and 13 be intermediate storage tank, and 14 be cyclone, and 15 are
Nanometer pulverization pump, 16 be product pump, and 17 be plate and frame filter press, and 18 be hopper, and 19 be feeding spiro rod, and 110 be desolventizing machine, 111
It is cooling screw, 112 be mixed material storehouse, and 113 be condenser, and 114 be solvent receiving tank, and 115 be solvent recovery tank, and 116 are
Heat exchanger is trapped, 117 be solvent receiving tank, and 118 be water sealed tank, and 119 be vacuum tank, and 120 be liquid seal can, and 121 be solvent pump；21
It is head tank, 22 be multi-stage screw formula reactor, and 23 be cooling tower；31 be solvent measuring tank, and 33 be cooling screw, and 34 be feeding
Screw rod, 35 be product homogenizing tower, and 36 be separator, and 37 be circulating pump, and 38 be gas separator, and 39 be multiple-stage separator, and 310 are
Cooling screw, 311 be demister, and 312 be product pans, and 313 be displacement pump.
Embodiment
Below in conjunction with the accompanying drawings, the embodiment of the present invention is illustrated.
The invention provides a kind of lithium iron phosphate positive material preparation technology, the preparation technology includes：LiFePO4 is former
The step of expecting nanosizing homogenizing；The step of material that nanosizing raw material pyroreaction is generated is through cooling down tower cooler；After cooling
The step of material particles are homogenized；Wherein, nanosizing homogenizing refers to the particle that raw material is ground into 0.1-100nm sizes, nanosizing
Raw material pyroreaction is continuous reaction.Continuous reaction is carried out in screw reactor, the reaction temperature of screw reactor
Spend for 600-750 DEG C.
In the present invention, raw material source of iron is FeC2O4·2H2O,FeC2O4Or (CH3COO)2Fe, raw material phosphorus source are NH4H2PO4Or
(NH4)2HPO4, raw material lithium source is Li2CO3, LiOH or Li3PO4, LiFePO4 raw material nanoization homogenizing refers to raw material mixing is equal
It is even, and all mixed raw materials are processed into particle diameter 0.1-100nm particle.
Present invention also offers a kind of device for realizing above-mentioned lithium iron phosphate positive material preparation technology, the device includes original
Material homogenizing part, pyroreaction cooling segment and product homogenizing part, pyroreaction cooling segment include screw reactor, spiral shell
Rod-type reactor connects cooling tower.The screw reactor at this place is the multistage spiral shell that more than two screw reactors are in series
Rod-type reactor 22.
Material homogenizer part includes nanometer homogenizing tower 12, and nanometer homogenizing tower 12 is connected with raw material measuring tank 11, nanometer homogenizing
Tower 12 also includes the cyclone 14 being attached thereto, and the overflow pipe connection intermediate storage tank 13 of cyclone 14, it is equal that sand sediment pipe connects nanometer
Change the capable homogenizing processing again of tower 12.The output end connection intermediate storage tank 13 of nanometer homogenizing tower 12, the outlet connecting plate of intermediate storage tank 13
Frame filter press 17, plate and frame filter press 17 connect the hopper 18 of feeding spiro rod 19, and feeding spiro rod 19 is also connected with desolventizing machine 110, take off
Solvent machine 110 connects mixed material storehouse.Desolventizing machine 110 is also connected with condenser 113, and condenser 113 connects solvent receiving tank
114, solvent receiving tank 114 connects solvent recovery tank 115, and solvent recovery tank 115 goes back pipe connecting frame filter press 17, and solvent connects
Closed cans 114 is also connected with trapping heat exchanger 116.
Product homogenizing part includes product homogenizing tower 35, and product homogenizing tower 35 connects separator 36, the overflow of separator 36
Mouth connection product pans 312, the heavy burder discharging opening connection product homogenizing tower 35 of separator 36.Product homogenizing part also includes molten
Agent measuring tank 31, the port of export connection product homogenizing tower 35 of measuring tank 31, the company between tower 35 and measuring tank 31 is homogenized in product
Adapter Lu Shangshe displacement pumps 313.
Raw material nano homogenizing process flow is：By required raw material input raw material measuring tank 11, while nanometer is homogenized
Solvent is full of in tower 12, raw material is put into nanometer homogenizing tower 12 afterwards, material flows into intermediate storage tank 13 after nanosizing is homogenized,
Plate and frame filter press 17 is pumped to afterwards, and material is after press filtration, and filter cake is through screw rod transmission to desolventizing machine 110, and homogenizing raw material is from de-
Solvent machine 110 is standby to mixed material storehouse 112 through screw rod transmission after coming out.Filtrate is reclaimed into solution recovery system.Raw material passes through
Turn into the particle of 0-100nm particle diameters after the processing of nanosizing homogenizing process.Concrete technology flow process is shown in accompanying drawing 1.
Pyroreaction technological process is：Multi-stage screw formula is delivered to after the preheated device preheating of raw material that upper step is prepared
Reactor 22, the transmission speed of screw rod is mixed up, ensure that material is completely reacted during screw reactor is passed in and out.It is reacted
Material cools down into cooling tower 23, product homogenizing tower 35 is delivered to after being cooled to normal temperature, into product homogenizing process.Pyroreaction
Waste gas caused by process is delivered to recovery system recovery after the separation of gas separator 38.
Product homogenizing process flow is：The product of cooling tower 23 is delivered to the product homogenizing tower 35 full of solvent, product
Product pans 312 are flowed into after product homogenizing tower 35 is homogenized, are pumped to plate and frame filter press afterwards, material is after press filtration, filter cake
Through screw rod transmission to desolventizer, obtain finally being homogenized product after desolvation, be delivered to automatic packaging line packaging therewith.Filtrate
Reclaimed into solvent recovering system.Product homogenizing flow of the present invention causes the yield rate of product to increase substantially, and is nearly free from
Waste material.
The multi-stage screw formula reaction utensil used in the present apparatus has the advantage that：
1) reactor is using sensing electrical heating, and the thermal efficiency is up to more than 90%.
2) with screw rod wall direct heat transfer in screw channel of the material in screw rod, heat transfer coefficient is up to 50 kilocalories/m3.h. DEG C；
3) material continuous dynamic Hybrid Heating in screw rod, has good immixture, makes material reaction uniform；
4) material can complete carbon coating or doping simultaneously during reaction；
5) reactor excludes gas caused by reaction with lower negative pressure；
6) reactor apparatus small volume, the filling rate of material is 30%, and the dosage of the protective gas such as nitrogen is greatly lowered；
7) due to the decline of nitrogen amount used, caused ammonia can prepare biphosphate with phosphoric acid recovery in course of reaction
Ammonium, the raw material as secondary response again.
8) screw rod has self clean-up action, can not only constantly clear up wall material, also the material constantly in cleaning screw slot,
Ensure the stability, uniformity of lithium anode material quality；
9) reactor realizes continuous production, and investment is greatly lowered, and produces 5000 tons of lithium anode materials, Multi-stage heating spiral shell per year
40-50 tons of bar gross weight, 50-100KW of total installed capacity, gross investment are less than 5,000,000 yuan.
Embodiment 1
On a kind of LiFePO4/ C preparation.By anhydrous oxalic acid ferrous iron 1453kg, ammonium dihydrogen phosphate 1150kg, lithium carbonate
370kg, sucrose 140kg raw materials are put into measuring tank, while nanometer homogenizing tower is full of into solvent, afterwards under nitrogen protection by original
Material is put into nanometer and is homogenized tower, and material flows into intermediate storage tank after nanosizing is homogenized, is pumped to plate and frame filter press, material afterwards
After press filtration, filter cake is homogenized after raw material comes out from desolventizer through screw rod transmission to raw material cabin through screw rod transmission to desolventizer
It is standby.Filtrate is reclaimed into solution recovery system.Pyroreaction screw rod will be delivered to after the preheated device preheating of the raw material prepared,
The transmission speed of screw rod is mixed up, ensures to react 10 hours at 700 DEG C in material pyroreaction screw rod.Reacted material enters cold
But tower cooler, product homogenizing tower is delivered to after being cooled to normal temperature, into product homogenizing process.Ammonia caused by high-temperature reaction process
After gas separator separates, ammonia is delivered to ammonia for the industrial waste gases such as gas, carbon monoxide, carbon dioxide and protective gas nitrogen
Gas recovery system is reclaimed, and the industrial waste gas such as carbon monoxide, carbon dioxide is directly discharged into air with nitrogen after treatment.Cooling
The product that tower comes is delivered to the particle diameter homogenizing tower full of solvent, flows into intermediate storage tank after the homogenized tower homogenizing of product, pumps afterwards
To plate and frame filter press, for material after press filtration, filter cake obtains final homogenizing production through screw rod transmission to desolventizer after desolvation
Product, automatic packaging line packaging is delivered to therewith.Filtrate is reclaimed into solvent recovering system.Final products 1600kg is obtained, it is average
Particle diameter is 70nm, compacted density 2.6g/ml, first discharge specific capacity 166mAh/g.
Embodiment 2
On a kind of LiFePO4/ C preparation.By anhydrous oxalic acid ferrous iron 1453kg, anhydrous phosphoric acid lithium 386kg, glucose
220kg raw materials are put into measuring tank, while nanometer homogenizing tower is full of into solvent, and raw material is put into receiving under nitrogen protection afterwards
Meter Jun Hua towers, material flow into intermediate storage tank after nanosizing is homogenized, and are pumped to plate and frame filter press afterwards, material after press filtration,
Filter cake is standby to raw material cabin through screw rod transmission after being come out from desolventizer through screw rod transmission to desolventizer, homogenizing raw material.Filtrate
Reclaimed into solution recovery system.Pyroreaction screw rod will be delivered to after the preheated device preheating of the raw material prepared, mixes up screw rod
Transmission speed, ensure to react 15 hours at 650 DEG C in material pyroreaction screw rod.It is cold that reacted material enters cooling tower
But, product homogenizing tower is delivered to after being cooled to normal temperature, into product homogenizing process.Ammonia, an oxygen caused by high-temperature reaction process
Change the industrial waste gases such as carbon, carbon dioxide and protective gas nitrogen after gas separator separates, ammonia is delivered to Ammonia recovery
System is reclaimed, and the industrial waste gas such as carbon monoxide, carbon dioxide is directly discharged into air with nitrogen after treatment.What cooling tower came
Product is delivered to the particle diameter homogenizing tower full of solvent, flows into intermediate storage tank after the homogenized tower homogenizing of product, is pumped to sheet frame afterwards
Filter press, after press filtration, filter cake obtains finally being homogenized product, therewith through screw rod transmission to desolventizer material after desolvation
It is delivered to automatic packaging line packaging.Filtrate is reclaimed into solvent recovering system.Final products 1590kg is obtained, average grain diameter is
50nm, compacted density 2.85g/ml, first discharge specific capacity 157mAh/g.
Embodiment 3
On a kind of LiFePO4/ C preparation.By anhydrous acetic acid ferrous iron 1739kg, anhydrous phosphoric acid lithium 400kg, glucose
200kg raw materials are put into measuring tank, while nanometer homogenizing tower is full of into solvent, and raw material is put into receiving under nitrogen protection afterwards
Meter Jun Hua towers, material flow into intermediate storage tank after nanosizing is homogenized, and are pumped to plate and frame filter press afterwards, material after press filtration,
Filter cake is standby to raw material cabin through screw rod transmission after being come out from desolventizer through screw rod transmission to desolventizer, homogenizing raw material.Filtrate
Reclaimed into solution recovery system.Pyroreaction screw rod will be delivered to after the preheated device preheating of the raw material prepared, mixes up screw rod
Transmission speed, ensure to react 8 hours at 760 DEG C in material pyroreaction screw rod.Reacted material enters cooling tower cooler,
Product homogenizing tower is delivered to after being cooled to normal temperature, into product homogenizing process.Ammonia, an oxidation caused by high-temperature reaction process
After gas separator separates, ammonia is delivered to Ammonia recovery system for the industrial waste gases such as carbon, carbon dioxide and protective gas nitrogen
The industrial waste gases such as system recovery, carbon monoxide, carbon dioxide are directly discharged into air with nitrogen after treatment.The production that cooling tower comes
Product are delivered to the particle diameter homogenizing tower full of solvent, flow into intermediate storage tank after the homogenized tower homogenizing of product, are pumped to sheet frame pressure afterwards
Filter, after press filtration, filter cake obtains finally being homogenized product through screw rod transmission to desolventizer material after desolvation, defeated therewith
Deliver to automatic packaging line packaging.Filtrate is reclaimed into solvent recovering system.Final products 1620kg is obtained, average grain diameter is
85nm, compacted density 2.92g/ml, first discharge specific capacity 155mAh/g.
Claims (10)
- A kind of 1. lithium iron phosphate positive material preparation technology, it is characterised in that：The preparation technology includes：By LiFePO4 raw material The step of nanosizing is homogenized；The step of material that nanosizing raw material pyroreaction is generated is through cooling down tower cooler；Thing after cooling The step of expecting particle homogenizing；Wherein, nanosizing homogenizing refers to the particle that raw material is ground into 0.1-100nm sizes, nanosizing original Material pyroreaction is continuous reaction.
- 2. according to the preparation technology described in claim 1, it is characterised in that：The continuous reaction enters in screw reactor OK, the reaction temperature of screw reactor is 600-750 DEG C.
- 3. according to the preparation technology described in claim 1, it is characterised in that：Raw material source of iron is FeC2O4·2H2O,FeC2O4Or (CH3COO)2Fe, raw material phosphorus source are NH4H2PO4Or (NH4)2HPO4, raw material lithium source is Li2CO3, LiOH or Li3PO4。
- 4. the Preparation equipment for preparation technology described in claim 1, it is characterised in that：The LiFePO4 raw material nanoization is equal Change refers to raw material being well mixed, and all mixed raw materials are processed into particle diameter 0.1-100nm particle.
- 5. a kind of device for preparation technology described in claim 1, described device is cold including material homogenizer part, pyroreaction But part and product homogenizing part, it is characterised in that：The pyroreaction cooling segment includes screw reactor, the screw rod Formula reactor connects cooling tower.
- 6. according to the device described in claim 5, it is characterised in that：The screw reactor is that more than two screws react The multi-stage screw formula reactor that device is in series.
- 7. according to the device described in claim 5, it is characterised in that：The material homogenizer part includes nanometer homogenizing tower, described Nanometer homogenizing tower is connected with raw material measuring tank, and the nanometer homogenizing tower is also connected with cyclone, the output of the nanometer homogenizing tower End connection intermediate storage tank, the outlet connection plate and frame filter press of the intermediate storage tank, the plate and frame filter press connection feeding spiro rod Hopper, the feeding spiro rod are also connected with desolventizing machine, the desolventizing machine connection mixed material storehouse.
- 8. according to the device described in claim 7, it is characterised in that：The desolventizing machine is also connected with condenser, the condenser Solvent receiving tank is connected, the solvent receiving tank connects solvent recovery tank, and the solvent recovery tank also pipeline connects the sheet frame Filter press, the solvent receiving tank are also connected with trapping heat exchanger.
- 9. according to the device described in claim 5, it is characterised in that：The product homogenizing part includes product homogenizing tower, described Product homogenizing tower connection separator, the overfall connection product pans of the separator, the heavy burder discharging opening of the separator Connect product homogenizing tower.
- 10. according to the device described in claim 9, it is characterised in that：The product homogenizing part also includes solvent measuring tank, institute The port of export for stating measuring tank connects the product homogenizing tower, is homogenized on the connecting line between tower and measuring tank and sets in the product Displacement pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710767835.3A CN107601448A (en) | 2017-08-30 | 2017-08-30 | A kind of lithium iron phosphate positive material preparation technology and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710767835.3A CN107601448A (en) | 2017-08-30 | 2017-08-30 | A kind of lithium iron phosphate positive material preparation technology and device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107601448A true CN107601448A (en) | 2018-01-19 |
Family
ID=61056286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710767835.3A Withdrawn CN107601448A (en) | 2017-08-30 | 2017-08-30 | A kind of lithium iron phosphate positive material preparation technology and device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107601448A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113381005A (en) * | 2021-05-27 | 2021-09-10 | 厦门大学 | Single-crystal ternary cathode material, continuous preparation method and device and application |
-
2017
- 2017-08-30 CN CN201710767835.3A patent/CN107601448A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113381005A (en) * | 2021-05-27 | 2021-09-10 | 厦门大学 | Single-crystal ternary cathode material, continuous preparation method and device and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101106194B (en) | Cathode material Li3V2(PO4)3 of lithium ion battery and its making method | |
| CN101693532B (en) | Method for preparing lithium ferrous phosphate | |
| CN101145611B (en) | Lithium ion cell anode material lithium vanadium phosphate preparation method | |
| CN110323434B (en) | Method for preparing lithium iron manganese phosphate-carbon composite material and lithium iron manganese phosphate-carbon composite material | |
| CN104752718B (en) | A kind of LiMnxFe1‑xPO4Positive electrode active materials and preparation method thereof | |
| CN107814372A (en) | A kind of preparation method and application of lithium iron phosphate positive material | |
| EP3909912A1 (en) | Method for preparing multi-stage pore-forming lithium iron phosphate | |
| CN100491239C (en) | Preparation method of lithium ion battery positive pole material lithium iron phosphate and its product | |
| CN107565132B (en) | The preparation method of the ferric phosphate and its ferric phosphate of preparation, the LiFePO4 and lithium battery of the preparation method of LiFePO4 and its preparation | |
| CN105390693B (en) | A kind of nanocrystalline positive electrode LiNi of high power capacity0.8Co0.1Mn0.1O2And its high pressure synthesis method | |
| CN101764226B (en) | Oxygen vacancy-contained and Fe site-doped lithium ferric phosphate and rapid solid-phase sintering method thereof | |
| CN102311109B (en) | Method for preparing LiFePO4/C composite cathode material by continuous reaction | |
| CN102623705B (en) | Lithium ion battery cathode material LiFePO4/C, and preparation method and application thereof | |
| CN100564250C (en) | The microwave fast solid phase sintering method of lithium ion battery anode material lithium iron phosphate | |
| CN109167028B (en) | Regeneration preparation method of lithium iron phosphate/carbon composite material | |
| CN101920952B (en) | Technique and device for producing iron phosphate lithium positive pole material through one-step process | |
| CN102185136B (en) | Preparation method of lithium ion battery cathode material nano lithium iron phosphate | |
| CN103391897B (en) | The manufacture method of double oxide and manufacturing installation | |
| CN113659133A (en) | Preparation method of high-compaction lithium ferric manganese phosphate cathode material | |
| US20150030517A1 (en) | Preparation method of battery composite material and precursor thereof | |
| CN102942167A (en) | Anhydrous ferric phosphate, lithium iron phosphate prepared from the anhydrous ferric phosphate and use of the lithium iron phosphate | |
| CN207361793U (en) | A kind of lithium iron phosphate positive material preparation facilities | |
| CN111540901B (en) | Method for preparing lithium iron phosphate (LEP) by using lithium iron phosphate (III) | |
| CN103367722B (en) | A kind of preparation method of charcoal coated LiFePO 4 for lithium ion batteries nanocomposite | |
| CN107601448A (en) | A kind of lithium iron phosphate positive material preparation technology and device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180119 |
|
| WW01 | Invention patent application withdrawn after publication |