CN106672934A - Microwave drying method in process for preparing lithium iron phosphate by wet-process material mixing and lithium iron phosphate preparation process comprising same - Google Patents
Microwave drying method in process for preparing lithium iron phosphate by wet-process material mixing and lithium iron phosphate preparation process comprising same Download PDFInfo
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- CN106672934A CN106672934A CN201610508699.1A CN201610508699A CN106672934A CN 106672934 A CN106672934 A CN 106672934A CN 201610508699 A CN201610508699 A CN 201610508699A CN 106672934 A CN106672934 A CN 106672934A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/265—General methods for obtaining phosphates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
- F26B3/28—Drying solid materials or objects by processes involving the application of heat by radiation, e.g. from the sun
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/58—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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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Abstract
The invention provides a drying method applied to a process for preparing lithium iron phosphate by wet-process material mixing. The method utilizes microwaves to dry. According to the drying method provided by the invention, the drying efficiency of materials in industrial production can be effectively improved, the investment of drying equipment is reduced, and the energy consumption and comprehensive cost are reduced; the practical value is high, and the process is relatively easy to realize; conditions are not strict, and the controllability is relatively high; and inner and outer drying degrees of dried matters are consistent. Furthermore, the invention further provides a lithium iron phosphate preparation process comprising the drying method.
Description
Technical field
The present invention relates to a kind of material by wet type mixing prepares the drying meanss in LiFePO4 technique and the LiFePO4 comprising it
Preparation technology, more particularly, in anode material of lithium battery manufacture field, prepares in LiFePO4 technique in material by wet type mixing
LiFePO4 preparation technology using the method for microwave drying and comprising it.
Background technology
At present, the method for LiFePO4 being prepared in industry has many kinds, for example, solid reaction process, carbothermic method, hydro-thermal
Method, microwave process for synthesizing and liquid-phase coprecipitation etc..Technique is roughly the same in all kinds of method preparation process：Batch mixing, drying, burning
Knot, crushing etc..Although the whole technique through industrially prepared gradual perfection in recent years, in whole technique link is dried
Need to continue to explore, especially in the technique that material by wet type mixing prepares LiFePO4, dry run is even more important.Because being dried
Can not exclusively cause material uneven, more can make to occur condensing shape in sintering, and drying process is relatively inefficient, indirectly
High cost.
It is dried link in all of LiFePO4 preparation technology at present and has been used up spray dryer, vacuum rake style drier
Or the equipment such as hot air circulation drying oven is carried out, such as Chinese patent application CN201310523782.2 and Chinese patent application
Disclosed in CN201310523781.8, it is all that process is dried using spray dryer；Chinese patent application
Conventional drying baker is then used in CN201310150727.3 and is dried process, the method is required at 90 DEG C -150 DEG C
1-5 hours are continued drying out under high temperature；For another example vacuum drying mode is used in Chinese patent application CN201510425066.X,
Requirement is persistently dried 12 hours.
In these drying processes, being dried using hot air circulation drying oven greatly to be lost time so that industry
Efficiency in production is low, and the hot blast energy consumption for constantly producing is higher；It is dried than common using vacuum rake style drier
More than 2 times of the efficiency high of baking oven, and baking temperature is less demanding, energy consumption is controllable, but this process due to itself
Design structure causes internal washing difficult, it is easy to residual materials, is unfavorable for big batch commercial production；Using spray dryer
Drying is the drying process method for currently preparing LiFePO 4 material main flow, and 1-3s can just evaporate more than 95% moisture, is dried
Speed is fast, and by separator collection material after being dried, whole efficiency increases, but this drying process is high using equipment requirements,
Occupation area of equipment is big, and energy consumption is very high, and simple electrical heating can not meet large batch of production, need steam, conduction oil, heat
The external heat sources such as blower fan produce hot blast, so indirect cost is very high.
Here, it is necessary to which it is relatively low to develop a kind of energy consumption, process is simple, industrial suitable serialization implement in wet method
Batch mixing prepares the drying meanss applied in the technique of LiFePO4.
The content of the invention
[technical problem]
The technical problem to be solved is：In overcoming the shortcomings of existing drying process, there is provided a kind of simple steady
It is fixed that the drying meanss applied in the technique of LiFePO4 are prepared in material by wet type mixing, can in the industrial production reduce drying equipment
Input, reducing energy consumption and integrated cost, its practical value is high, and technique is more easy to realize that condition is loose, and controllability is higher, is dried effect
Rate is high, and the inside and outside degree of drying of dried object is consistent.
[technical scheme]
According to an aspect of the invention, there is provided a kind of batch mixing in a wet process prepares apply in the technique of LiFePO4 dry
Drying method, methods described is to carry out the drying using microwave.
In the present invention, term used " LiFePO4 " refers to be typically used as positive pole material in lithium battery manufacture field
The LiFePO4 of material, its available chemical formula " LiFePO4" represent, can also add in the LiFePO4 further according to being actually needed
Plus various additives.
In the present invention, term used " microwave " refers to the microwave that this area routinely understands, i.e., in 300MHz-
Electromagnetic wave in the frequency range of 300GHz.When microwave penetrates medium, because there is certain phase interaction with medium in microwave energy
With, make the molecule vibrations for producing more than one hundred million times per second of medium, the intermolecular mutual generation of medium rub, the medium temperature for causing
Raise, make dielectric material internal, outside almost while heat temperature raising, forms body heat source state, in substantially reducing conventional heating
Heat conduction time.
For example, the hydrone in heated medium material is polar molecule.It is (micro- in fast-changing electromagnetic field of high frequency
Ripple) effect under, its polarity orientation changes the change with external electric field, so as to cause the effect of the spin motion of hydrone,
Now the field energy of microwave field is converted into the heat energy in medium, raises temperature of charge, produce a series of materializing procedures such as transconversion into heat and
Reach the purpose of micro-wave drying.I.e. in the present invention, microwave can produce heat by the moisture absorption in LiFePO4, make
Moisture evaporation is obtained, so as to reach dry purpose.
An embodiment of the invention, the frequency of the microwave can be 2400MHz-2500MHz, preferably
2450-2480MHz.Under this frequency, can efficient drying material by wet type mixing.
Additionally, microwave is instantaneous heat temperature raising to dielectric material, programming rate is fast.On the other hand, the output of microwave
Adjustable at any time, medium temperature rise can change therewith inertialess, there is no residual activity phenomenon, be highly advantageous to and automatically control and serialization
The needs of production.
An embodiment of the invention, the power of the microwave can be 50-90kW, preferred 60-80kW.Here
Under power, can efficient drying material by wet type mixing.
An embodiment of the invention, can by the way of continuous feeding microwave drying material by wet type mixing, for example, can
Material by wet type mixing is carried using conveyer belt continue through microwave radiation area.Preferably, the feeding speed of material by wet type mixing can be 2-
5kg/min, preferred 2.5-4kg/min, the gait of march of conveyer belt can be 0.5-5m/min, preferred 1-3m/min.
Preferably, drying time, (i.e. the time required to microwave radiation area) can be 6-15 minutes, and preferred 9-13 divides
Clock.
By drying meanss of the invention, the water content of dried batch mixing can be down to less than 5%, or even can be down to
Less than 2%.
Further, it is also possible to apply microseismic activity to batch mixing in the microwave drying process, this can help to moisture preferably
Effusion.Alternatively, dehumidifier process can also be simultaneously carried out in the microwave drying process.
According to a further aspect in the invention, there is provided a kind of batch mixing in a wet process prepares the technique of LiFePO4, the technique
Including above-mentioned drying meanss.
According to a further aspect of the invention, there is provided a kind of anode material of lithium battery manufacturing process, the positive electrode
For LiFePO4, the LiFePO4 preparation technology is using above-mentioned drying meanss of the invention.
Still another aspect of the invention, there is provided a kind of lithium battery manufacturing process, the positive electrode of the lithium battery
For LiFePO4, the LiFePO4 preparation technology is using above-mentioned drying meanss of the invention.
[beneficial effect]
Drying meanss of the invention can effectively improve the drying efficiency of material in commercial production, and it does not need fuel,
Boiler is not needed, pollution-free, energy consumption is low, there is no conduction of heat during heating, firing rate is fast, simultaneously because microwave can be in object
Outer to heat simultaneously, the internal-external temperature difference of material is little, and homogeneous heating greatly improves dry mass so that the inside and outside of dried object is dried journey
Degree is consistent.Also, microwave dryer of the invention is simple to operate, controllability is strong, add conveyer belt can directly with subsequently
Technique is connected, time and labour saving sequence so that the integrated artistic of positive electrode is more simple.The method for microwave drying of the present invention is particularly fitted
Close the application at present in industrial a large amount of production LiFePO 4 materials.
Specific embodiment
Hereinafter, the preferred embodiment of the present invention will be described with reference to embodiment.But it should be noted that institute of the present invention
The embodiment of offer is used only as illustrating, and is not intended to be limiting technical spirit and core element and the operation of the present invention.Not
On the premise of departing from the technical spirit and scope of the present invention, the exemplary embodiment of the present invention can change in a variety of manners.
An embodiment of the invention, is obtained LiFePO4 slurry, then by the phosphoric acid using material by wet type mixing
Ferrum lithium slurry is inserted in transmission belt, and with the speed of about 1-3m/min microwave radiation area is entered, and the frequency of the microwave is 2450-
2480MHz, power is 60-80kW, and the feeding speed of the LiFePO4 slurry is 2.5-4kg/min, through microwave exposure area
It it is 9-13 minutes the time required to domain, the water content for measuring dried LiFePO4 is less than 5%.Subsequently, dried phosphoric acid
Ferrum lithium be admitted to after processing procedure in.
Another embodiment of the invention, using the method for comprising the following steps microwave drying is implemented：
(1) water for accounting for material powder weight percent phosphoric acid ferrum and lithium carbonate gross mass 15-20% is placed in ball mill；
(2) lithium carbonate (Li of the additive such as phosphoric acid and 0.5-1% of material powder weight 2-3% will be accounted for2CO3) be added to
Ball milling 5-10 minutes in ball mill；
(3) glucose for accounting for material powder weight 9-12%% is added in ball mill and is stirred for about 10 minutes；
(4) be separately added into again the iron phosphate for sloughing water of crystallization of the water and 75-85% for accounting for material powder weight 25-35% with
The Li of 19-22%%2CO3；
(5) continue to stir more than 6 hours；
(6) discharge after, add slurry into and carry out on the conveyer belt of microwave drying casing microwave drying, microwave drying oven it is defeated
Go out frequency and be adjusted to 2400-2500MHz, preferred 2450-2480MHz, power is adjusted to 50-90kW, preferred 60-80kW, according to 2-
The speed of 5kg/min, preferred 2.5-4kg/min is uniformly put into slurry on conveyer belt, and conveyer belt is excellent according to 0.5-5m/min
Select the speed of 1-3m/min by microwave radiation area, slurry is 6-15 minutes the time required to microwave radiation area, preferably
9-13 minutes, thus it is capable of achieving the microwave drying of slurry.
Further, can follow the steps below to obtain LiFePO4 as needed：
(7) crucible after material is compacted is placed in containing 99.99%N2Protective atmosphere electric furnace in, be at the uniform velocity warming up to
700-800 DEG C of insulation 5-10 hour obtains LiFePO4.
Embodiment
Embodiment 1
1. the water of 20kg is placed in ball mill；
2. by the phosphoric acid of 3.06kg and the Li of 1kg2CO3It is sequentially added stirring 5 minutes in ball mill；
3. the glucose of 13.22kg is added and be stirred 10 minutes；
4. the water of 38.4kg is separately added into again, and 100kg sloughs the iron phosphate of water of crystallization and the Li of 24.6kg2CO3
5. more than 6 hours are stirred；
6. discharge after, add slurry into and carry out on the conveyer belt of microwave drying casing microwave drying, microwave drying oven it is defeated
Go out frequency and be adjusted to 2450MHz, power is adjusted to 60kW, slurry is uniformly put on conveyer belt according to the speed of 3.5kg/min, pass
Send band according to the speed of 2.5m/min by microwave radiation area, slurry is 10 minutes the time required to microwave radiation area,
Thus it is capable of achieving the microwave drying of slurry.Above-mentioned whole slurries can complete drying through about 60 minutes, by dried thing
Material is weighed, and gross mass is 144.33kg, and the gross mass before being dried is 200.28kg, and wherein the quality of water is 58.4kg, is damaged
The quality of mistake is the moisture for evaporating, it follows that can be dried the moisture removed more than 95% through micro-wave drying method；
7. the crucible after material is compacted is placed in containing 99.99%N2Protective atmosphere electric furnace in, be at the uniform velocity warming up to 750
DEG C insulation obtains LiFePO4 in 8 hours.
Embodiment 2
1. the water of 80kg is placed in ball mill；
2. by the phosphoric acid of 12.24kg and the Li of 4kg2CO3It is sequentially added stirring 5 minutes in ball mill；
3. the glucose of 52.88kg is added and be stirred 10 minutes；
4. the water of 153.6kg is separately added into again, and 400kg sloughs the iron phosphate of water of crystallization and the Li of 98.4kg2CO3
5. more than 6 hours are stirred；
6. discharge after, add slurry into and carry out on the conveyer belt of microwave drying casing microwave drying, microwave drying oven it is defeated
Go out frequency and be adjusted to 2480MHz, power is adjusted to 80kw, slurry is uniformly put on conveyer belt according to the speed of 4kg/min, transmit
According to the speed of 1.8m/min by microwave radiation area, slurry is 13 minutes the time required to microwave radiation area to band, by
This is capable of achieving the microwave drying of slurry.Above-mentioned whole slurries can complete drying through about 200 minutes, by dried material
Weighed, gross mass is 577.46kg, the gross mass before being dried is 801.12kg, wherein the quality of water is 233.6kg, is lost
Quality be evaporate moisture, it follows that the moisture more than 95% can be dried through micro-wave drying method；
7. the crucible after material is compacted is placed in containing 99.99%N2Protective atmosphere electric furnace in, be at the uniform velocity warming up to 750
DEG C insulation obtains LiFePO4 in 8 hours.
Claims (10)
1. a kind of batch mixing in a wet process prepares the drying meanss applied in the technique of LiFePO4, it is characterised in that methods described is
It is dried using microwave.
2. drying meanss according to claim 1, wherein, the frequency of the microwave is 2400MHz-2500MHz, preferably
2450-2480MHz。
3. drying meanss according to claim 1, wherein, the power of the microwave is 50-90kW, preferred 60-80kW.
4. drying meanss according to claim 1, wherein, carry the material by wet type mixing using conveyer belt and continue through microwave
Material by wet type mixing described in the mode microwave drying of the continuous feeding of irradiation zone, it is preferable that to mixed in the microwave drying process
Material applies microseismic activity, and dehumidifier process is carried out simultaneously in the microwave drying process.
5. drying meanss according to claim 4, wherein, the feeding speed of the material by wet type mixing is 2-5kg/min, preferably
2.5-4kg/min。
6. drying meanss according to claim 4, wherein, the gait of march of the conveyer belt is 0.5-5m/min, preferably
1-3m/min。
7. drying meanss according to claim 4, wherein, through the required time of microwave radiation area be 6-15 minutes,
It is preferred that 9-13 minutes.
8. drying meanss according to claim 1, wherein, the drying meanss include：
(1) water for accounting for material powder weight percent phosphoric acid ferrum and lithium carbonate gross mass 15-20% is placed in ball mill；
(2) lithium carbonate (Li of the additive such as phosphoric acid and 0.5-1% of material powder weight 2-3% will be accounted for2CO3) it is added to ball milling
Ball milling 5-10 minutes in machine；
(3) glucose for accounting for material powder weight 9-12%% is added in ball mill and is stirred for about 10 minutes；
(4) iron phosphate and 19- of sloughing water of crystallization of the water and 75-85% for accounting for material powder weight 25-35% are separately added into again
22%% Li2CO3；
(5) continue to stir more than 6 hours；
(6) after discharging, add slurry into and carry out on the conveyer belt of microwave drying casing microwave drying, the output frequency of microwave drying oven
Rate is adjusted to 2400-2500MHz, preferred 2450-2480MHz, and power is adjusted to 50-90kW, preferred 60-80kW, according to 2-5kg/
The speed of min, preferred 2.5-4kg/min is uniformly put into slurry on conveyer belt, conveyer belt according to 0.5-5m/min, preferred 1-
By microwave radiation area, slurry is 6-15 minutes the time required to microwave radiation area to the speed of 3m/min, preferred 9-13
Minute, thus it is capable of achieving the microwave drying of slurry.
9. a kind of preparation technology of LiFePO4, the LiFePO4 preparation technology is adopted according to any one of claim 1 to 8 institute
The drying meanss stated.
10. the preparation technology of LiFePO4 according to claim 9, wherein, the technique is further included：(7) by thing
Crucible after material compacting is placed in containing 99.99%N2Protective atmosphere electric furnace in, be at the uniform velocity warming up to 700-800 DEG C insulation 5-10
Hour obtains LiFePO4.
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| CN201610508699.1A CN106672934B (en) | 2016-07-01 | 2016-07-01 | Microwave drying method in process for preparing lithium iron phosphate by wet mixing and lithium iron phosphate preparation process comprising same |
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