CN206316380U - A kind of preparation facilities for preparing high stability lithium metal microsphere powder - Google Patents
A kind of preparation facilities for preparing high stability lithium metal microsphere powder Download PDFInfo
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Abstract
The utility model, which is related to, a kind of prepares the preparation facilities that liquid metal material prepares metal dust, it is atomized indoor location gases at high pressure atomizer, smelting apparatus outlet is connected by the first woven hose and melt guide with the import of gases at high pressure atomizer, the import of reative cell is protected to be connected by powder conduit and powder in the outlet of spray chamber, protection liquid of the powder protection reative cell full of flowing, the outlet of powder protection reative cell is connected by the 3rd woven hose with protection liquid storage tank and separation of solid and liquid room, protect the first outlet of liquid storage tank to be recycled to powder by infusion pump and the second liquid-transport pipe-line and protect reative cell, the second outlet of liquid storage tank is protected to pass through gas pipeline and gas boosting pump circulation to gases at high pressure atomizer.The utility model realizes the serialization of powder production, integration, shortens technological process, improves production efficiency.
Description
[technical field]
The utility model, which is related to, a kind of prepares the preparation facilities that liquid metal material prepares metal dust, and in particular to a kind of
The preparation facilities of high stability lithium metal microsphere powder is prepared, for lithium ion battery electrode material to lift the storehouse first of battery
Human relations efficiency, capacity and cycle performance.
[background technology]
Lithium ion battery is because operating voltage is high, specific energy is big, small volume, light weight, have extended cycle life, self discharge is low, nothing
Memory effect, it is pollution-free the advantages of be widely used.Conventional lithium ion battery negative material is graphite and carbon material, positive electrode
There are the materials such as cobalt acid lithium, LiMn2O4, LiFePO4.But it is due to that graphite type material capacity is relatively low, its endurance is more and more not
The requirement of people can be met.There is a certain amount of active lithium loss, its main body in existing lithium ion battery production technology
Now due to the intercalation potential of graphite cathode is less than electrolyte solvent ethylene carbonate (EC), propene carbonate (PC), carbonic acid two
The reduction potential of ethyl ester (DEC) etc., solvent can be reduced to produce one layer of solid electrolytic in negative terminal surface in charging process
Plasma membrane (SEI), has during this lithium ion to participate in reaction, for example, generates Li2CO3, LiF and alkyl lithium carbonates etc. are in negative material
In be difficult to the irreversible lithium product of deintercalation, so as to result in active lithium about 7-10% loss so that lithium ion battery is first
Coulombic efficiency is reduced.By theoretical and it is demonstrated experimentally that add extra active lithium into lithium ion battery, that is, add lithium metal
Microsphere powder, allows lithium to mix in advance in electrode material, can efficiently solve above mentioned problem.
The preparation method of conventional metals powder typically uses aeroponics or water fog method, is primarily characterized in that by atomization side
Molten metal is ground into metal dust by method.In conventional method, the smelting apparatus of metal is usually using induction heater or resistance
Heating furnace, and separated with atomizer, this metal needs for resulting in after melting wants tundish to carry out keeping temperature, adds energy consumption.
And the fusing point of lithium metal is at 180 DEG C, less than most metal.The present invention utilizes the low-melting characteristic of lithium metal, proposes a kind of
The preparation facilities for preparing lithium metal powder that melting plant and atomizer are directly connected to.
Lithium metal is very active, easily reacts, is prepared into after microsphere powder with oxygen, nitrogen and vapor, compares table
Area is greatly increased, and activity is also greatly improved.The problem of easily being reacted for metallic lithium powder with air and vapor, the present invention
Propose a kind of method for preparing high stability lithium metal microsphere powder.The method operating process is simple, and less energy consumption, product has grain
The controllable and high advantage of stability of degree, can keep obvious lithium metal does not occur within more than 12 hours declining under room temperature and normal humidity
Subtract, it is easy to use in atmosphere, the first effect and cycle performance of battery can be effectively improved by being added in electrode material.Therefore utilize
High stability lithium metal microsphere powder prepared by the process and apparatus of the present invention has boundless application in field of lithium
Prospect.
[content of the invention]
The purpose of this utility model is to provide a kind of preparation facilities of high stability lithium metal microsphere powder, preparation facilities
Make use of the characteristic of lithium metal low melting point makes equipment simpler, environmentally friendly, and preparation method solves lithium microsphere powder in the prior art
The defect easily reacted with empty gas and water, and be applied in lithium ion battery to improve battery head effects, capacity and cycle performance.
To achieve these goals, the technical scheme that the utility model is taken is as follows：
A kind of preparation facilities of high stability lithium metal microsphere powder, it is characterised in that：Including smelting apparatus, spray chamber 8,
Gases at high pressure atomizer 7, powder protection reative cell 10, separation of solid and liquid room 18, infusion pump 12, gas boosting pump 15, powdered pipe
9th, melt liquid-transport pipe-line (the first liquid-transport pipe-line 3), melt guide 6, protection liquid pipe road (the second liquid-transport pipe-line 11 and the 3rd woven hose
Road 17), gas pipeline 14, heater 4 and cooler 5, gases at high pressure atomizer 7 is installed in spray chamber 8, smelting apparatus outlet is logical
Cross the first woven hose 3 and melt guide 6 is connected with the import of gases at high pressure atomizer 7, the outlet of spray chamber 8 passes through powdered pipe
9 protect the import of reative cell 10 to be connected with powder, protection liquid of the powder protection reative cell 10 full of flowing, powder protection reative cell
10 outlet is connected by the 3rd woven hose 17 with protection liquid storage tank 13 and separation of solid and liquid room 18, the protection liquid storage tank 13
First outlet by the liquid-transport pipe-line 11 of infusion pump 12 and second be recycled to powder protect reative cell 10, it is described protection liquid storage tank
13 second outlet is recycled to gases at high pressure atomizer 7 by gas pipeline and gas boosting pump 15.Above arrangement produces
High stability lithium metal microsphere powder preparation facilities, including the ring such as the melting of lithium metal, transfusion, atomization, powder protection, filtering
Section.
Described smelting apparatus includes in smelting furnace 1 and smelting furnace interlayer 2, smelting furnace interlayer admittance deep fat or to install
Induction heating apparatus.Described smelting apparatus be with smelting furnace with dissection, in interlayer can with admittance deep fat or add sensing plus
Hot equipment.
Separation of solid and liquid room 18 is connected built with filter, and with protection liquid storage tank, has cooler on the woven hose
And heater, for feed flow or stopping feed flow；Described spray chamber is provided with cooling device, and the type of cooling is usually water-cooled or gas
It is cold, preferably air cooling.
Described filter is filter screen natural filtration or Buchner funnel suction filtration, and institute can be filtered out by the filtering of screen cloth 19
The lithium powder footpath needed.
Described separation of solid and liquid room 18 can dismantle movement, can timing isolated wet high stability lithium metal is micro-
Ball powder pours out drying.
In summary, the utility model has following features to prior art：
The utility model utilizes the low-melting characteristic of lithium metal, proposes prepared by a kind of atomization powder for lithium metal and fills
Put, the device protects the melting of lithium metal, melt conveying, atomization, powder, sieves grades, and technique has carried out effective integration,
Each process procedure is effectively docked, realize serialization, the integration of powder production, shorten technological process, improve life
Efficiency is produced, while by the recycling and the recycling of protection liquid of gas, discharge being reduced to greatest extent, is realized
The environmental protection of high stability lithium metal microsphere powder production.
[brief description of the drawings]
Fig. 1 is the preparation facilities structural representation of high stability lithium metal microsphere powder.
Description of symbols in figure
1 smelting furnace, 2 smelting furnace interlayers, 3 first woven hoses, 4 heaters, 5 coolers, 6 melt guides, 7 gases at high pressure mists
Change device, 8 spray chambers, 9 powdered pipes, 10 powders protection reative cell, 11 second liquid-transport pipe-lines, 12 infusion pumps, 13 protection liquid storages
Tank, 14 gas pipelines, 15 gas boosting pumps, 16 gas pipelines, 17 the 3rd liquid-transport pipe-lines, 18 separation of solid and liquid rooms, 19 screen clothes.
[embodiment]
The technical solution of the utility model is expanded on further in conjunction with drawings and Examples below, it is believed that to this area skill
It is clear for art personnel, embodiment is only used for explaining without limiting the scope of the invention.
As shown in figure 1, being the preparation facilities structural representation of this high stable lithium metal microsphere powder.It is prepared by this metal dust
Device, including melting furnace 1, melting furnace interlayer 2, gases at high pressure atomizer 7, spray chamber 8, powder protection reative cell 10, protection liquid
Holding vessel 12, separation of solid and liquid room 18, the first woven hose 3, melt guide 6, powdered pipe 9, the second woven hose 11, the 3rd woven hose
17th, gas pipeline 14,16 and infusion pump 12, gas boosting pump 15, screen cloth 19, heater 4, cooler 5 etc. are constituted.
Melting plant is divided into melting furnace 1 and melting furnace interlayer 2, and melting furnace 1 can be opened in addition lithium block, melting furnace interlayer 2
Can admittance deep fat, heat conduction oil temperature is at 200-300 DEG C, or can install induction heating equipment and heated.Melting furnace 1 passes through first
Woven hose 3 is connected with the melt guide 6 of spray chamber 7, and heater 4, cooler 5, heater during feed flow are housed on the first woven hose 3
First woven hose 3 is heated to 200-300 DEG C by 4, and to stop infusing, lithium metal fusing point 50- is cool below by cooler 5
100 DEG C can be such that melt is set in the first woven hose 3, play a part of closing and stop preparation process.
Gases at high pressure atomizer 7 is installed, gases at high pressure atomizer 7 leads to high pressure argon gas in spray chamber 8, mist is carried out to melt
Change.High pressure argon gas is pressurized by gas boosting pump 15 by the argon gas in separation of solid and liquid room 18 and provided by gas conduit 16, and
After the completion of atomization, separation of solid and liquid room 18 is returned to powder, so that argon gas can be recycled.
Spray chamber 8 is provided with cooling device, generally selects air cooling mode.Spray chamber 8 passes through with powder protection reative cell 10
Powdered pipe 9 is connected, and powdered pipe 9 is passed directly into the protection liquid in powder protection reative cell 10.
Protect liquid storage tank 13 by the second woven hose 11 and the 3rd woven hose 17 respectively with powder protection reative cell 10 and
Separation of solid and liquid room 18 is connected, and protection liquid flows into powder from storage tank 13 by the second woven hose 11 using infusion pump 12 and protects anti-
Answer in room 10, protected powder enters separation of solid and liquid room 18 with protection liquid by the 3rd woven hose 17, and protection liquid passes through screen cloth
19 return to protection liquid storage tank 13, and the powder of protected seam parcel is stayed on screen cloth 19.So as to which protection liquid may be reused.
Separation of solid and liquid room 18 is detachable, with the progress of preparation, the powder on screen cloth regularly can be poured out into dry collection.
Apparatus above forms the preparation facilities of high stable lithium metal microsphere powder.
The preparation method of high stability lithium metal microsphere powder of the present invention, including lithium metal melting, transfusion, mist
Change, powder is protected, sieve the link such as dry.All links of the preparation method in addition to drying are entered in argon atmosphere
OK, it is usually to be carried out in the glove box of ar gas environment.Preparation process is as follows：A certain amount of lithium metal block is added into smelting furnace
In, 200-300 DEG C of conduction oil is led in smelting furnace interlayer or by installing induction heating apparatus, melt lithium metal block；Plus
Hot device 4 is heated to 200-300 DEG C, and lithium metal melt reaches gases at high pressure atomizer 7 by the first woven hose 3 and melt guide 6,
Gases at high pressure atomizer 7 leads to high pressure argon gas, and lithium metal melt forms vaporific under high pressure argon gas effect, and vaporific molten drop is in spray chamber
Fly, cool down in 8, being frozen into microsphere powder, powder enters powder by powdered pipe 9 in the presence of gravity and air-flow and protected
In reactor 10, powder protects the protection liquid in reactor 10 fully to contact with powder, and the protection agent molecule in protection liquid is to gold
Belong to lithium microsphere powder surface and carry out Surface coating, the powder being wrapped by enters solid-liquid with protection liquid by the 3rd woven hose 17
Separation chamber 18, carries out separation of solid and liquid, the wet-milling being filtrated to get is poured out from separation of solid and liquid room 18, by true by the filtering of screen cloth 19
Sky can obtain dry high stability lithium metal microsphere powder after drying.
Above method is the basic preparation method of high stability lithium metal microsphere powder.
Embodiment 1：
Under argon atmosphere, 6kg lithium metals block is put into smelting furnace 1,220 DEG C of conduction oil is led in smelting furnace interlayer 2,
At this temperature, lithium metal is slowly melted, and the lithium metal liquid of melting reaches high pressure by the first woven hose 3 and melt guide 6
Gas atomizer 7, gases at high pressure atomizer 7 leads to high pressure argon gas, and argon pressure is 2Mpa, melt quilt in the presence of high pressure argon gas
Atomization, and gradually cooled and solidified is lithium metal microsphere powder in dropping process, powder passes through powder under gravity and airflow function
Body pipeline 9 is delivered into powder protection reative cell 10, and protection liquid is connected with powder protection reative cell 10, and protection liquid composition is
The toluene solution of 0.1% polystyrene (Mn=260000), lithium microsphere powder fills in powder protection reative cell 10 with protection liquid
Tap, which is touched, makes surface be wrapped up by PMA molecule, and is delivered to separation of solid and liquid room 18 with the 3rd woven hose 17 and is filtered
Separation, protection liquid returns to protection liquid storage tank 13, and the wet-milling being filtrated to get is stayed on screen cloth 19, and wet-milling is by vacuum drying
High stability lithium metal powder can be obtained.
Embodiment 2：
Under argon atmosphere, 6kg lithium metals block is put into smelting furnace 1, set in smelting furnace interlayer 2 equipped with sensing heating
It is standby, temperature is risen to 220 DEG C by sensing heating, lithium metal is slowly melted, the lithium metal liquid of melting passes through the first transfusion
Pipe 3 and melt guide 6 reach gases at high pressure atomizer 7, and gases at high pressure atomizer 7 leads to high pressure argon gas, and argon pressure is 2Mpa, melt
Body is atomized in the presence of high pressure argon gas, and gradually cooled and solidified is lithium metal microsphere powder in dropping process, and powder exists
Powder is delivered into by powdered pipe 9 to protect in reative cell 10, lead in powder protection reative cell 10 under gravity and airflow function
There is protection liquid, protection liquid composition is dimethyl carbonate (DMC) solution of 0.1% oleyl amine, and lithium microsphere powder is protected in powder to react
Fully being contacted with protection liquid in room 10 makes surface be wrapped up by oleyl amine molecule, and is delivered to separation of solid and liquid room 18 with the 3rd woven hose 17
It is separated by filtration, protection liquid returns to protection liquid storage tank 13, and the wet-milling being filtrated to get is stayed on screen cloth 19, and wet-milling passes through vacuum
Drying can obtain high stability lithium metal powder.
Embodiment 3：
Under argon atmosphere, 6kg lithium metals block is put into smelting furnace 1,220 DEG C of conduction oil is led in smelting furnace interlayer 2,
At this temperature, lithium metal is slowly melted, and the lithium metal liquid of melting reaches high pressure by the first woven hose 3 and melt guide 6
Gas atomizer 7, gases at high pressure atomizer 7 leads to high pressure argon gas, and argon pressure is 2Mpa, melt quilt in the presence of high pressure argon gas
Atomization, and gradually cooled and solidified is lithium metal microsphere powder in dropping process, powder passes through powder under gravity and airflow function
Body pipeline 9 is delivered into powder protection reative cell 10, and protection liquid is connected with powder protection reative cell 10, protection liquid composition be containing
There is diethyl carbonate (DEC) solution of 0.1% polystyrene (Mn=260000) and 0.05% oleyl amine, lithium microsphere powder is in powder
Fully being contacted with protection liquid in protection reative cell 10 makes surface be wrapped up by PMA molecule, and defeated with the 3rd woven hose 17
Deliver to separation of solid and liquid room 18 to be separated by filtration, protection liquid returns to protection liquid storage tank 13, and the wet-milling being filtrated to get stays in screen cloth
On 19, wet-milling can obtain high stability lithium metal powder by vacuum drying.
Claims (5)
1. a kind of preparation facilities of high stability lithium metal microsphere powder, it is characterised in that：Including smelting apparatus, spray chamber (8),
Gases at high pressure atomizer (7), powder protection reative cell (10), separation of solid and liquid room (18), infusion pump (12), gas boosting pump
(15), powdered pipe (9), woven hose, melt guide (6), protection liquid pipe road, gas pipeline (14), heater (4) and cooler
(5) gases at high pressure atomizer (7), is installed, smelting apparatus outlet passes through the first woven hose (3) and melt guide in spray chamber (8)
Import with gases at high pressure atomizer (7) is connected, and reative cell is protected in the outlet of spray chamber (8) by powdered pipe (9) and powder
(10) import is connected, the outlet of powder protection reative cell (10) by the 3rd woven hose (17) and protection liquid storage tank (13) and
Separation of solid and liquid room (18) is connected, and the first outlet of the protection liquid storage tank (13) passes through infusion pump (12) and the second liquid-transport pipe-line
(11) powder protection reative cell (10) is recycled to, the second outlet of the protection liquid storage tank (13) passes through gas pipeline and gas
Body booster pump (15) is recycled to gases at high pressure atomizer (7).
2. high stability lithium metal microsphere powder preparation facilities according to claim 1, it is characterised in that：Described melting
Device includes in smelting furnace (1) and smelting furnace interlayer (2), smelting furnace interlayer that admittance deep fat or induction heating apparatus can be installed.
3. high stability lithium metal microsphere powder preparation facilities according to claim 1, it is characterised in that：Separation of solid and liquid room
(18) built with filter, and it is connected with protection liquid storage tank, has cooler and heater on the woven hose.
4. high stability lithium metal microsphere powder preparation facilities according to claim 3, it is characterised in that：Described filtering
Device is filter screen natural filtration or Buchner funnel suction filtration, and required lithium powder footpath can be filtered out by being filtered by screen cloth (19).
5. high stability lithium metal microsphere powder preparation facilities according to claim 1, it is characterised in that：Described solid-liquid
Separation chamber (18) can dismantle movement, isolated high stability lithium metal microsphere powder regularly can be poured out into drying.
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| CN109773199A (en) * | 2019-01-15 | 2019-05-21 | 中国科学院合肥物质科学研究院 | A kind of fast preparation method of multiple dimensioned lithium ball |
| CN109773199B (en) * | 2019-01-15 | 2021-05-28 | 中国科学院合肥物质科学研究院 | Rapid preparation method of multi-scale lithium ball |
| CN109967755A (en) * | 2019-05-14 | 2019-07-05 | 湖州恒合科技有限公司 | A kind of spherical shape fine metal powder production system and its method |
| CN109967755B (en) * | 2019-05-14 | 2023-08-18 | 湖州恒合科技有限公司 | Spherical fine metal powder production system and method thereof |
| CN114096346A (en) * | 2019-12-20 | 2022-02-25 | 株式会社Lg化学 | Precursor for positive electrode active material, method for producing same, and apparatus for producing same |
| CN114096346B (en) * | 2019-12-20 | 2024-04-16 | 株式会社Lg化学 | Precursor for positive electrode active material, method for producing same, and apparatus for producing same |
| CN113059167A (en) * | 2021-03-17 | 2021-07-02 | 昆山宝创新能源科技有限公司 | Preparation method of passivated lithium microspheres and device and application thereof |
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Effective date of registration: 20230822 Address after: 202150 No. 825, Xinkaihe Road, Xinhe Town, Chongming District, Shanghai (Shanghai Xinhe economic community) Patentee after: Shanghai Hongchang New Material Technology Co.,Ltd. Address before: Room 2535, No. 5475 Yunchuan Road, Baoshan District, Shanghai, 200942 Patentee before: SHANGHAI AWD NEW ENGERY TECHNOLOGY Co.,Ltd. |