CN107225251A - A kind of passivation of lithium microsphere production device - Google Patents
A kind of passivation of lithium microsphere production device Download PDFInfo
- Publication number
- CN107225251A CN107225251A CN201710613184.2A CN201710613184A CN107225251A CN 107225251 A CN107225251 A CN 107225251A CN 201710613184 A CN201710613184 A CN 201710613184A CN 107225251 A CN107225251 A CN 107225251A
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- Prior art keywords
- tank
- lithium
- passivation
- air
- atomizer
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Links
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 131
- 238000002161 passivation Methods 0.000 title claims abstract description 107
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000004005 microsphere Substances 0.000 title claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 239000002184 metal Substances 0.000 claims abstract description 29
- 238000007599 discharging Methods 0.000 claims abstract description 27
- 238000012216 screening Methods 0.000 claims abstract description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 46
- 239000007789 gas Substances 0.000 claims description 36
- 229910052786 argon Inorganic materials 0.000 claims description 23
- 230000007704 transition Effects 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 6
- 238000000889 atomisation Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000003306 harvesting Methods 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 4
- 239000003990 capacitor Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 16
- 239000007788 liquid Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 229910001338 liquidmetal Inorganic materials 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 230000003137 locomotive effect Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000521 B alloy Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 1
- HXAKWVCRTCUPKH-UHFFFAOYSA-N [Li].[Mg].[B] Chemical compound [Li].[Mg].[B] HXAKWVCRTCUPKH-UHFFFAOYSA-N 0.000 description 1
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- HRKQOINLCJTGBK-UHFFFAOYSA-N dihydroxidosulfur Chemical compound OSO HRKQOINLCJTGBK-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 smart mobile phone Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/10—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/086—Cooling after atomisation
- B22F2009/0876—Cooling after atomisation by gas
Abstract
The invention discloses a kind of passive metal lithium microsphere production device, including molten lithium tank, passivation tank and product screening collecting device, the molten lithium tank is provided with heater I, top in the passivation tank is provided with molten lithium atomizer, the molten lithium atomizer is connected by conveyance conduit with the molten lithium tank, the passivation tank is provided with air-flow cooling recirculation system and discharging portion, and the product screening collecting device is connected with the discharging portion of the passivation tank.The present invention uses dry production, process route is simple, solvent need not be used in preparation process, the lithium metal microsphere surface of preparation is cleaner, the passive metal lithium microsphere diameter of acquisition is 0.010~0.120mm, the product of different meshes can be sieved into according to different applications, negative pole, secondary battery negative pole or the positive pole of the secondary cell as high power capacity mend lithium and as lithium ion super capacitor lithium source, can be greatly enhanced the capacity of secondary cell.
Description
Technical field
The invention belongs to secondary cell field, more particularly to a kind of passive metal lithium microsphere production device.
Background technology
In recent years, as the electric equipment products such as smart mobile phone, tablet personal computer, electric automobile are to high-energy-density electrochmical power source
Demand, the specific capacity to secondary cell requires also more and more higher.But existing secondary cell by material because being limited, specific capacity hair
Open up space limited, therefore, be badly in need of the battery material of research high power capacity.Passive metal lithium microspheres quality is light, and electrode potential is low, as
The cell negative electrode material of high power capacity has many advantages, can be used as lithium-sulfur cell, lithium-air battery, lithium all-solid-state battery, lithium
The negative pole of polymer battery and other secondary cells using passive metal lithium microballoon as negative pole；Passive metal lithium microballoon can be with
Lithium is mended applied to anode or negative material to use, and the lithium ion of SEI films consumption is formed during supplement circulating battery, reaches and carries
The effect of high battery capacity；Passive metal lithium microballoon can also as lithium ion super capacitor lithium source, improve battery appearance
Amount.
Current lithium metal microballoon is mainly prepared using wet method, and it is micro- to prepare lithium metal disclosed in patent document CN101213039A
The method of ball is：The lithium metal of solid is added in solvent hydrocarbon ils, heating stirring, lithium metal fusing, then pass through high-speed stirred, system
It is standby to obtain lithium metal microballoon, add fluorization agent and be passivated, obtain the lithium metal microballoon for thering is lithium fluoride to protect to surface, after pass through
Supercooling is filtered, and obtains the lithium metal microballoon for having hydrocarbon ils to surface, by three cleanings of solvent hexane, and solvent pentane is once cleaned,
Obtain product.Wet method prepares the problem of existing：1) process route is long, and preparation process is complicated；2) product surface has a small amount of molten
Agent (hydrocarbon ils, hexane, pentane) is remained, and the chemical property performance to product has a certain impact.
The content of the invention
The present invention provides a kind of passive metal lithium microsphere production device to solve technical problem present in known technology,
The device need not use solvent, and the lithium metal microsphere surface of preparation is cleaner.
The present invention is adopted the technical scheme that to solve technical problem present in known technology：A kind of passive metal lithium
Microsphere production device, including molten lithium tank, passivation tank and product screening collecting device, the molten lithium tank is provided with heater I, described
The top being passivated in tank is provided with molten lithium atomizer, and the molten lithium atomizer is connected by conveyance conduit with the molten lithium tank,
The passivation tank is provided with air-flow cooling recirculation system and discharging portion, the discharging of the product screening collecting device and the passivation tank
Portion is connected.
The air-flow cooling recirculation system includes backwind tube, air exhauster, cooler II and the air feed pipe being sequentially connected, described
The outlet of air feed pipe be arranged on it is described passivation tank in and positioned at the molten lithium atomizer lower section, the backwind tube with it is described blunt
Change the top connection of tank, filter is provided with the backwind tube, the air exhauster and the cooler II are arranged on described blunt
Change the outside of tank.
The air-flow cooling recirculation system also includes passivator atomizer, and the air-flow cooling recirculation system includes connecting successively
The backwind tube, the air exhauster, the cooler II, the passivator atomizer and the air feed pipe connect, the passivation
Agent atomizer is put in the outside of the passivation tank.
Heat preservation structure is provided with the outside of the conveyance conduit.
Cooler I is provided with the outside of the middle part of the passivation tank.
The discharging portion of the passivation tank is the splicing funnel in the passivation tank, and the splicing funnel is located at described
Below the outlet of air-flow cooling recirculation system, the product screening collecting device is arranged on the bottom in the passivation tank, including
The sifter and Material collecting box for harvesting being connected successively from top to bottom, the sifter are located at the lower section of the splicing funnel, the two linking,
The side wall of the passivation pot bottom is provided with transition hatch door.
The discharging portion of the passivation tank is the discharging opening for being arranged on its bottom, and the product screening collecting device is arranged on institute
The lower section of passivation tank, including argon gas glove box and sifter and collecting box in the argon gas glove box are stated, it is described
The feeding mouth for being passivated the discharging opening and the argon gas glove box of tank is tightly connected, and the collecting box is arranged under the sifter
Side, the sifter is connected with the discharging opening of the passivation tank, and transition hatch door is provided with the argon gas glove box.
Valve is provided with the conveyance conduit.
The molten lithium atomizer uses ultrasonic atomizer or centrifugal atomizer.
The present invention has the advantages and positive effects of：The lithium metal of solid-state is melt into by using dry molten lithium tank
The lithium metal of liquid, and in dry passivation tank be atomized into the lithium metal of liquid under trickle lithium metal drop makes it scattered
Fall, met in dropping process with cooling passivation air-flow, be cooled and be frozen into lithium metal microballoon, react micro- in lithium metal with passivator
The surface of ball forms passivating film, obtains passivated lithium metal microballoon, and surface-active is relatively low.The present invention uses dry production,
Process route is simple, solvent need not be used in preparation process, the lithium metal microsphere surface of preparation is cleaner, the passivation of acquisition
Lithium metal microsphere diameter is 0.010~0.120mm, the product of different meshes can be sieved into according to different applications, as height
Negative pole, secondary battery negative pole or the positive pole of the secondary cell of capacity mend lithium and as lithium ion super capacitor lithium source, can be greatly
Improve the capacity of secondary cell in ground.And the present invention can improve production efficiency, it is ensured that product quality.
Brief description of the drawings
Fig. 1 is the structural representation of the embodiment of the present invention 1；
Fig. 2 is the structural representation of the embodiment of the present invention 2.
In figure：1st, heater I；2nd, lithium tank is melted；3rd, sifter；4th, splicing funnel；5th, cooler I；6th, it is passivated tank；7th, convey
Pipeline；8th, valve；9th, heater II；10-1, ultrasonic atomizer；10-2, centrifugal atomizer；11st, filter；12nd, air exhauster；
13rd, cooler II；14th, air feed pipe, 15, backwind tube；16th, passivator atomizer；17th, collecting box；18th, transition hatch door；19th, argon gas
Glove box；20th, high-speed electric expreess locomotive.
Embodiment
In order to further understand the content, features and effects of the present invention, hereby enumerating following examples, and coordinate accompanying drawing
Describe in detail as follows：
Refer to Fig. 1~Fig. 2, a kind of passive metal lithium microsphere production device, including molten lithium tank 2, passivation tank 6 and product sieve
Divide collecting device, the molten lithium tank 2 is provided with heater I 1, the top in the passivation tank 6 is provided with molten lithium atomizer, described
Molten lithium atomizer is connected by conveyance conduit 7 with the molten lithium tank 2, the passivation tank 6 provided with air-flow cooling recirculation system and
Discharging portion, the product screening collecting device is connected with the discharging portion of the passivation tank 6.
Embodiment 1：
Referring to Fig. 1, a kind of productions of use ultrasonic atomizer 10-1 as molten lithium atomizer passive metal lithium microballoon
Device, concrete structure includes molten lithium tank 2 and passivation tank 6, and the molten lithium tank 2 is provided with heater I 1, and the bottom of the molten lithium tank 2 leads to
The top that conveyance conduit 7 is crossed with the passivation tank 6 is connected, and the export department of the conveyance conduit 7 is stretched into the passivation tank 6,
Top in the passivation tank 6 is fixed with exports the ultrasonic atomizer 10-1 being connected with conveyance conduit, and the passivation tank 6 is provided with
Air-flow cooling recirculation system, the bottom in the passivation tank 6 is provided with the sifter 3 and collecting box 17 being mutually linked, described to receive
Header 17 is arranged on the lower section of the sifter 3, and transition hatch door 18 is provided with the side wall of passivation tank 6 bottom.
In the present embodiment, in order that cooling passivation air-flow and the lithium metal droplet formation convection current of scattered whereabouts, are improved blunt
Change quality, the air-flow cooling recirculation system includes backwind tube 15, air exhauster 12, cooler II 13 and the air feed pipe being sequentially connected
14, the air feed pipe 14 is horizontally set on the bottom in the passivation tank 6, provided with outlet, described time on the air feed pipe 14
Airduct 15 is connected with the top of the passivation tank 6, and filter 11 is provided with the backwind tube 15, and filter 11 is arranged on described
The end of backwind tube 15, in the passivation tank 6, the air exhauster 12 and the cooler II 13 are arranged on the passivation tank
6 outside.The use of on-gaseous passivator for convenience, the air-flow cooling recirculation system also includes passivator atomizer 16,
The air-flow cooling recirculation system includes the backwind tube 15 being sequentially connected, the air exhauster 12, the cooler II 13, institute
Passivator atomizer 16 and the air feed pipe 14 are stated, the passivator atomizer 16 is arranged on the outside of the passivation tank 6.Using
The passivator of on-gaseous is atomized by the passivator atomizer 16, passivator is mixed into lithium metal protection gas with steam form, is used
Air-flow is passivated in forming cooling.For the ease of the conveying and atomization of lithium metal liquid, in the outside of the conveyance conduit 7 provided with insulation
Heating arrangement, the temperature for making conveyance conduit 7 is 200~300 DEG C, and heater II is provided with the export department of the conveyance conduit 7
9, the temperature for making the exit of conveyance conduit 7 is 200~1000 DEG C.In order to prevent trickle lithium metal drop in the mistake of scattered whereabouts
Sticked in journey on tank skin, be provided with cooler I 5 on the outside of the middle part of the passivation tank 6, the temperature for making passivation tank is 0~80 DEG C.
In order that cooling passivation air-flow is distributed more uniformly across in the horizontal, the air feed pipe 14 uses loop configuration, in annular air feed
Pipe is provided with multiple outlets upward.In the present embodiment, the discharging portion of the passivation tank 6 is installed in the passivation tank
Splicing funnel 4 in 6, the splicing funnel 4 is located at below the outlet of the air-flow cooling recirculation system.The product screening is received
Collect the inside that equipment is arranged on the passivation tank 6, including the sifter 3 and collecting box 17 being connected successively from top to bottom, the sieve
Device 3 is divided to be located at the lower section of the splicing funnel 4, the two linking.In order to adjust the flow of control liquid metal lithium, in the conveying
Pipeline 7 is provided with valve 8, and the outside of valve 8 is provided with Heat preservation structure.
The course of work and principle to the present embodiment 1 exemplified by using on-gaseous passivator are described as follows：
Lithium ingot is removed after packaging, adds dry molten lithium tank 2, and lithium metal protection gas is filled after vacuumizing, in the present embodiment,
Lithium metal protects gas frequently with argon gas.Start heater I 1, by heating lithium metal to melting；Then argon gas is used in molten lithium tank 2
Pressurizeed 0.005~0.1Mp, and liquid metal lithium is entered in passivation tank 6 by conveyance conduit 7 through valve 8, now in passivation tank 6
It is already formed with cooling passivation air-flow.Conveyance conduit 7 and valve 8 need heating and thermal insulation to 200~300 DEG C；II 9 pairs of heater is defeated
The export department of pipeline 7 is sent to heat, it is 200~1000 DEG C to make the temperature at this.The high temperature gold gone out from the export department's drip of conveyance conduit 7
Belong to lithium liquid and enter ultrasonic atomizer 10-1, the frequency for controlling ultrasonic atomizer is 10~100KHz, and high-temperature metal lithium liquid is atomized
Fall into trickle lithium metal droplet distribution.Simultaneously be passivated tank 6 in cooling passivating gas flow through air exhauster 12 be pressurized, cooler II
13 coolings, into passivator atomizer 16, enter air feed after the passivator of steam form after atomization is mixed into cooling passivation air-flow
Pipe 14, the outlet through air feed pipe 14 controls the exit of air feed pipe 14 in the bottom discharge of passivation tank 6 by adjusting cooler II 13
The temperature of cooling passivation air-flow is 0~80 DEG C.In the presence of air exhauster 12, cooling passivation air-flow slowly equably rises, with
The trickle lithium metal droplet formation convection current of scattered whereabouts, trickle lithium metal drop solidifies in the presence of cooling passivation air-flow
Into lithium metal microballoon, while forming diaphragm on surface with the passivator reaction of steam form in cooling passivation air-flow, acquisition is blunt
Change lithium metal microballoon.Passive metal lithium microballoon falls into sifter 3 through splicing funnel 4 and sieved, the product of particle diameter needed for obtaining
Fall into collecting box 17.Collecting box 17 can be taken out with the transition hatch door 18 on passivated tank 6.
Embodiment 2：
Referring to Fig. 2, a kind of productions of use centrifugal atomizer 10-2 as molten lithium atomizer passive metal lithium microballoon
Device, including molten lithium tank 2 and passivation tank 6, the molten lithium tank 2 are provided with heater I 1, and the bottom of the molten lithium tank 2 passes through delivery pipe
Road 7 is connected with the top of the passivation tank 6, and the export department of the conveyance conduit 7 is stretched into the passivation tank 6, described blunt
Change the top in tank 6 and be fixed with the centrifugal atomizer 10-2 being connected with conveyance conduit outlet, the passivation tank 6 is cooled down provided with air-flow
The circulatory system, discharging opening, the discharging opening of the passivation tank 6 and entering for argon gas glove box 19 are provided with the bottom of the passivation tank 6
Material mouth is tightly connected, provided with the sifter 3 and collecting box 17 being mutually linked, the collecting box 17 in the argon gas glove box 19
The lower section of the sifter 3 is arranged on, the sifter 3 is connected with the discharging opening of the passivation tank 6, in the argon gas glove box
19 are provided with transition hatch door 18.
In the present embodiment, in order that cooling passivation air-flow and the lithium metal droplet formation convection current of scattered whereabouts, are improved blunt
Change quality, the air-flow cooling recirculation system includes backwind tube 15, air exhauster 12, cooler II 13 and the air feed pipe being sequentially connected
14, the outlet of the air feed pipe 14 stretches to the bottom being passivated in tank 6, the top of the backwind tube 15 and the passivation tank 6
Portion is connected, and filter 11 is provided with the backwind tube 15, the air exhauster 12 and the cooler II 13 are arranged on described blunt
Change the outside of tank 6.The use of on-gaseous passivator for convenience, the air-flow cooling recirculation system also includes passivator atomizer
16, the air-flow cooling recirculation system includes the backwind tube 15, the air exhauster 12, the cooler II being sequentially connected
13rd, the passivator atomizer 16 and air feed pipe 14, the passivator atomizer 16 are arranged on the outside of the passivation tank 6.For
It is easy to the conveying and atomization of lithium metal liquid, Heat preservation structure is provided with the outside of the conveyance conduit 7, for ensures conveying
The temperature in the exit of pipeline 7 is 200~800 DEG C.In order to prevent the adhesion during scattered whereabouts of trickle lithium metal drop
On tank skin, cooler I 5 is provided with the outside of the middle part of the passivation tank 6, for ensureing that the temperature of passivation tank is relatively low, tank is passivated
Temperature be advisable with 0~80 DEG C.In order to ensure that production is smooth, the passivation tank 6 uses the small olive-type structure broad in the middle in two.
In the present embodiment, the discharging portion of the passivation tank 6 is the discharging opening for being arranged on its bottom, the product screening collecting device peace
Mounted in the lower section of the passivation tank, including argon gas glove box 19 and the He of sifter 3 in the argon gas glove box 19
Collecting box 17, the feeding mouth of the discharging opening and the argon gas glove box 19 of the passivation tank 6 is tightly connected, and the collecting box 17 is set
Put in the lower section of the sifter 3, the sifter 3 is connected with the discharging opening of the passivation tank 6, in the argon gas glove box 19
It is provided with transition hatch door 18.In order to adjust the flow of control liquid metal lithium, valve 8, valve are provided with the conveyance conduit 7
8 outside is provided with Heat preservation structure.
The course of work and principle to the present embodiment exemplified by using on-gaseous passivator are described as follows：
Lithium ingot is removed after packaging, adds dry molten lithium tank 2, and lithium metal protection gas is filled after vacuumizing, in the present embodiment,
Lithium metal protection gas uses argon gas.Start heater I 1, by heating lithium metal to melting；Then add in the interior argon gas of molten lithium tank 2
0.005~0.1Mp is pressed, liquid metal lithium is entered in passivation tank 6 by conveyance conduit 7 through valve 8, in passivation tank 6 now
Through being formed with cooling passivation air-flow.Conveyance conduit 7 and valve 8 need heating and thermal insulation, and the temperature for making the exit of conveyance conduit 7 is
200~800 DEG C；The high-temperature metal lithium liquid gone out from the outlet of conveyance conduit 7 drip enters centrifugal atomizer 10-2, centrifugal atomizer
10-2 is driven by high-speed electric expreess locomotive 20, and the rotating speed of high-speed electric expreess locomotive 20 is up to 1~80,000 revs/min.High-temperature metal lithium liquid is by centrifugal atomizer
10-2 is atomized into trickle lithium metal droplet distribution and fallen.Simultaneously be passivated tank 6 in cooling passivating gas flow through air exhauster 12 be pressurized,
Cooled down through cooler II 13, into passivator atomizer 16, the passivator of steam form after atomization is mixed into cooling passivation air-flow
Enter air feed pipe 14 afterwards, through being discharged for wind tube outlet in the bottom of passivation tank 6, air feed pipe 14 is controlled by adjusting cooler II 13
The temperature of exit cooling passivation air-flow is 0~80 DEG C.In the presence of air exhauster 12, cooling passivation air-flow it is slow equably on
Rise, the trickle lithium metal droplet formation convection current with scattered whereabouts, trickle lithium metal drop is passivated the effect of air-flow in cooling
Under be frozen into lithium metal microballoon, while with cooling passivation air-flow in steam form passivator reaction surface formed diaphragm,
Obtain passive metal lithium microballoon.Passive metal lithium microballoon is fallen into argon gas glove box 19 by being passivated the discharging opening of the bottom of tank 6
Sifter 3 is sieved, and the product of particle diameter falls into collecting box 17 needed for obtaining.Collecting box 17 can be through on argon gas glove box 19
Transition hatch door 18 takes out.
In the present invention, it is that the lithium metal protection gas incorporation passivator in passivation tank is formed that above-mentioned cooling, which is passivated air-flow,
, passivator be used for lithium metal microsphere surface is passivated, can using phosphoric acid class, phosphoric acid ester, sulfuric acid, thio-alcohol,
Type siloxane, fluorine-containing compound and atoleine etc., it would however also be possible to employ the gas such as carbon dioxide and oxygen mix.If used
Gaseous state passivator, only need to directly be filled with passivation tank by gaseous state passivator, and gaseous state passivator is mixed with the lithium metal protection gas in tank,
Cooling passivation air-flow is formed in the presence of air-flow cooling recirculation system, now the air-flow cooling recirculation system does not include passivation
Agent atomizer 16.If using on-gaseous passivator, it is necessary to which after on-gaseous passivator is atomized, passivator atomizing steam is added
Lithium metal protects gas, and cooling passivation air-flow is formed in the presence of air-flow cooling recirculation system, now the air-flow cooling circulation
System should include passivator atomizer 16.Lithium metal protects gas that inertia that argon gas etc. do not react with lithium metal or stably can be used
Gas.
Above-mentioned process units be there are certain requirements to the relative humidity of environment, and preferably passivation tank is placed in drying room.On
Stating passive metal lithium microballoon includes doping aluminium element in passivation pure metal lithium microballoon, in addition to passivation lithium metal, element silicon, boron member
The lithium alloy microballoon of the other elements such as element, magnesium elements, phosphide element, Zn-ef ficiency, doping way can use unit, binary, ternary
Or multi-element doping, the content of doped chemical is 0.01%~40%.For example：It is passivated lithium-aluminium alloy microballoon, passivation of lithium magnesium boron alloy
Microballoon, passivation of lithium magnesium borosilicate alloy microballoon etc..
Although the preferred embodiments of the present invention are described above in conjunction with accompanying drawing, the invention is not limited in upper
The embodiment stated, above-mentioned embodiment is only schematical, be not it is restricted, this area it is common
Technical staff is under the enlightenment of the present invention, in the case where not departing from present inventive concept and scope of the claimed protection, also
Many forms can be made, these are belonged within protection scope of the present invention.
Claims (9)
1. a kind of passive metal lithium microsphere production device, it is characterised in that set including molten lithium tank, passivation tank and product screening collection
Standby, the molten lithium tank is provided with heater I, and the top in the passivation tank is provided with molten lithium atomizer, the molten lithium atomization
Device is connected by conveyance conduit with the molten lithium tank, and the passivation tank is provided with air-flow cooling recirculation system and discharging portion, the production
Product sieve collecting device and are connected with the discharging portion of the passivation tank.
2. passive metal lithium microsphere production device according to claim 1, it is characterised in that the air-flow cools down cyclic system
System includes backwind tube, air exhauster, cooler II and the air feed pipe being sequentially connected, and the outlet of the air feed pipe is arranged on the passivation
In tank and positioned at the lower section of the molten lithium atomizer, the backwind tube is connected with the top of the passivation tank, in the return air
Pipe is provided with filter, and the air exhauster and the cooler II are arranged on the outside of the passivation tank.
3. passive metal lithium microsphere production device according to claim 2, it is characterised in that the air-flow cools down cyclic system
System also include passivator atomizer, the air-flow cooling recirculation system include be sequentially connected the backwind tube, the air exhauster,
The cooler II, the passivator atomizer and the air feed pipe, the passivator atomizer are put in the outer of the passivation tank
Portion.
4. passive metal lithium microsphere production device according to claim 1, it is characterised in that in the outer of the conveyance conduit
Side is provided with Heat preservation structure.
5. passive metal lithium microsphere production device according to claim 1, it is characterised in that at the middle part of the passivation tank
Outside is provided with cooler I.
6. passive metal lithium microsphere production device according to claim 1, it is characterised in that the discharging portion of the passivation tank
For the splicing funnel in the passivation tank, the splicing funnel is located under the outlet of the air-flow cooling recirculation system
Side, the product screening collecting device is arranged on the bottom in the passivation tank, including the sifter being connected successively from top to bottom
And Material collecting box for harvesting, the sifter is positioned at the lower section of the splicing funnel, and the two is connected, and is set on the side wall of the passivation pot bottom
There is transition hatch door.
7. passive metal lithium microsphere production device according to claim 1, it is characterised in that the discharging portion of the passivation tank
To be arranged on the discharging opening of its bottom, the product screening collecting device is arranged on the lower section of the passivation tank, including argon gas hand
Casing and sifter and collecting box in the argon gas glove box, the discharging opening of the passivation tank and the argon gas hand
The feeding mouth of casing is tightly connected, and the collecting box is arranged on the lower section of the sifter, the sifter and the passivation tank
Discharging opening linking, on the argon gas glove box be provided with transition hatch door.
8. passive metal lithium microsphere production device according to claim 1, it is characterised in that set on the conveyance conduit
There is valve.
9. passive metal lithium microsphere production device according to claim 1, it is characterised in that the molten lithium atomizer is adopted
With ultrasonic atomizer or centrifugal atomizer.
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