CN108854915A - A kind of wet process mix grinding device and the method for preparing sulfide electrolyte precursor - Google Patents
A kind of wet process mix grinding device and the method for preparing sulfide electrolyte precursor Download PDFInfo
- Publication number
- CN108854915A CN108854915A CN201810795958.2A CN201810795958A CN108854915A CN 108854915 A CN108854915 A CN 108854915A CN 201810795958 A CN201810795958 A CN 201810795958A CN 108854915 A CN108854915 A CN 108854915A
- Authority
- CN
- China
- Prior art keywords
- valve
- reaction kettle
- wet process
- grinding device
- bottle
- 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.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/51—Methods thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/53—Mixing liquids with solids using driven stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/59—Mixing systems, i.e. flow charts or diagrams
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/83—Mixing plants specially adapted for mixing in combination with disintegrating operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83612—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by crushing or breaking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83613—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/75—Discharge mechanisms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/16—Mills in which a fixed container houses stirring means tumbling the charge
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Food Science & Technology (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of wet process mix grinding device and the method for preparing sulfide electrolyte precursor, wet process mix grinding device includes:Feed proportioning system, mixing system, crushing system, material-receiving system;Feed proportioning system is formed by being sequentially connected the liquid storage bottle connect, metering pump and solid sampling column, and the organic solvent in liquid storage bottle under the action of metering pump, can fall in the shape of a spiral along the inner wall of solid sampling column.By above-mentioned feed proportioning system it is found that the organic solvent in liquid storage bottle can fall in the shape of a spiral along the inner wall of solid sampling column, to take away the agglomeration of the viscous wall on inner wall, and then the operation for manually handling agglomeration is avoided.Therefore, wet process mix grinding device proposed by the present invention is able to solve the problem of raw material is easy viscous wall agglomeration, reduces operator's workload, solve the problems, such as the field at this stage.
Description
Technical field
The present invention relates to sulfide solid electrolyte precursor preparation fields, more specifically to a kind of wet process mix grinding
Device and the method for preparing sulfide electrolyte precursor.
Background technique
In recent years, with the development of new-energy automobile industry, the lithium battery as one of new-energy automobile core component is also
It is increasingly becoming the emphasis of the area research.Since all-solid lithium-ion battery replaces conventional organic solution using solid electrolyte
Matter, therefore be expected in the safety issue for fundamentally solving battery, and further promote the energy density and cycle life of lithium battery,
Meet the direction of the following high security lithium ion battery with high energy density development.For the prior art, all solid lithium is realized
The commercialized key of ion battery is that one kind to be developed is provided simultaneously with low cost, high conductivity, high chemical stability, Width funtion window
The solid lithium ion battery material of the advantages that mouth.In various electrolytes, sulfide causes extensive concern.
But since the aerial stability of the raw material of sulfide electrolyte precursor and its preparation is poor, it is easy
It reacts with water micro in air, influences sulfide electrolyte electrochemical performance;It releases a kind of inflammable and has simultaneously
There is the toxic gas hydrogen sulfide (H of rotten egg smell2S), thus related most of preparation process require in glove box into
Row.
At this stage, there are three types of the main preparation methods of sulfide solid electrolyte, i.e. ball-milling method, liquid phase method and melt quenching
Method.Wherein, ball-milling method, i.e., it is raw material mixed powder is broken, sulfide solid electrolyte presoma is obtained, it can also if it is high-energy ball milling
Glassy state sulfide solid electrolyte is obtained by raw material is decrystallized;And the method is easy to operate, and it is highly-safe, it is easy to control, but ball
During mill, since raw material is all the lesser sulfide of relative hardness such as Li2S、P2S5Deng, therefore it is easy viscous wall agglomeration, it need to be by inner wall
Above viscous agglomeration material scrapes off levigate, and ball milling again is taken out out of glove box, increases the workload of operator.Liquid phase method is
Add the raw material into organic solvent, and stir at a certain temperature, by be centrifuged or rotate method therefrom isolate reaction after
Solute, and dry and obtain sulfide solid electrolyte presoma;And the method operating temperature is low, morphology controllable is easy to operate, but just
For the biggish raw material of hardness such as LiCl, raw material can not be crushed by stirring, influence sulfide solid electrolyte presoma
Homogeneity, in addition, this method is only applicable to the preparation of a few sulfide electrolyte, universality is poor.Melt quenching method is
By raw material, high-temperature process is melted after evenly mixing, and glassy state sulfide solid electrolyte forerunner is obtained after melted material is quenched
Body;The method equipment investment is low and requires simply, but operating temperature high energy consumption is big, and yield is lower.
Therefore, how to solve the problems, such as that raw material is easy viscous wall agglomeration, reduce operator's workload, be the field at this stage
Problem urgently to be resolved.
Summary of the invention
In view of this, the device is able to solve raw material and is easy the purpose of the present invention is to provide a kind of wet process mix grinding device
The problem of viscous wall agglomeration, operator's workload is reduced, solves the problems, such as the field at this stage.The present invention also aims to
A kind of method for preparing sulfide electrolyte precursor is provided, this method is applied to above-mentioned wet process mix grinding device therefore can
It solves the problems, such as that raw material is easy viscous wall agglomeration, reduces operator's workload.
A kind of wet process mix grinding device, including:Feed proportioning system, mixing system, crushing system, material-receiving system;The ingredient system
System is formed by being sequentially connected the liquid storage bottle connect, metering pump and solid sampling column, and the organic solvent in the liquid storage bottle is described
Under the action of metering pump, it can fall in the shape of a spiral along the inner wall of the solid sampling column.
Preferably, the wet process mix grinding device, the mixing system include:Interlayer reaction kettle is plugged in the interlayer
The blender of reaction kettle, for controlling the temperature control cycles device of the interlayer temperature of reaction kettle;The interlayer reaction kettle and institute
Solid sampling column is stated to be connected.
Preferably, the wet process mix grinding device, the crushing system are made of the ball mill and peristaltic pump being connected;Institute
Peristaltic pump is stated to be connected with the interlayer reaction kettle, for the mixing in the interlayer reaction kettle to be delivered to the ball mill,
And send the mixing after mill back to the interlayer reaction kettle.
Preferably, the wet process mix grinding device, the material-receiving system include:The receipts being connected with the interlayer reaction kettle
The vacuum pump expecting bottle, being connected with the rewinding bottle.
Preferably, the wet process mix grinding device, the vacuum pump are circulating water type vacuum pump.
Preferably, the wet process mix grinding device, the first valve and the solid sampling column two on the liquid storage bottle
Second valve and third valve at end are three-way valve, in order to control the emptying of gas in the feed proportioning system.
Preferably, the wet process mix grinding device, for connecting the 4th valve of the ball mill on the interlayer reaction kettle
Door is three-way valve.
Preferably, the wet process mix grinding device, for connecting the 5th valve of the rewinding bottle on the interlayer reaction kettle
Door is two-way valve.
Preferably, the wet process mix grinding device, for connecting the 6th valve of the interlayer reaction kettle on the rewinding bottle
Door and the 7th valve for connecting the vacuum pump are two-way valve.
A method of preparing sulfide electrolyte precursor, including step:
Step 1, ingredient weigh various powder raw materials by the proportion of sulfide electrolyte in glove box, are placed in solid
In body sample introduction column, the second valve and third valve are closed;Organic solvent is added in liquid storage bottle and closes the first valve;Again by institute
It states solid sampling column and the liquid storage bottle takes out from the glove box;Configure clean zirconia ball be fitted into it is in ball mill and close
Seal the ball mill;
Step 2, exhaust, argon bottle is connected with first valve, by first valve and second valve it
Between pipeline and metering pump in air from three ports of second valve be discharged;It, first will be on the argon bottle after emptying
Pressure reducing valve auxiliary-valve is adjusted to small pressure, and successively opens second valve and first valve, finally closes the decompression
Valve auxiliary-valve;Similarly, the air in mixing system, crushing system, material-receiving system and associated pipe is emptied;
Step 3, feed fluid injection, opens third valve, the solid powder in the solid sampling column is made to fall to folder automatically
Layer reaction kettle;It opens metering pump and sets the fluid injection volume of organic solvent in the liquid storage bottle, make the organic solvent described in
The inner wall of solid sampling column falls in the shape of a spiral, agglomerates and flows into interlayer reaction kettle to take away viscous wall, closes after the completion of fluid injection
The metering pump and the third valve;
Step 4, mixing crush, and open simultaneously set temperature control loop device, the revolution for setting blender and runing time are simultaneously
Starting;After the slurry agitation in the interlayer reaction kettle is uniform, sets the flow of peristaltic pump and runing time and start;Setting
The revolution and runing time of ball mill simultaneously start;After the reaction was completed, the peristaltic pump, the ball mill and the stirring are closed
Device;The peristaltic pump is opened again and makes its reverse rotation, and the slurry in the ball mill and associated pipe is evacuated to the folder
Layer reaction kettle, finally closes the peristaltic pump;
Step 5, rewinding start circulating water type vacuum pump and open the 7th valve, to evacuate the gas in rewinding bottle;When
When the pressure of the circulating water type vacuum pump reaches maximum value, the 5th valve and the 6th valve are opened, the interlayer reaction kettle is made
Interior slurry flow to the rewinding bottle;After slurry fully flows into the rewinding bottle, the 5th valve, the 6th valve are closed
Door and the 7th valve, and close the circulating water type vacuum pump;Slurry in the rewinding bottle is evaporated under reduced pressure simultaneously
After drying, sulfide electrolyte precursor is obtained.
Wet process mix grinding device proposed by the present invention, including:Feed proportioning system, mixing system, crushing system, material-receiving system;Match
Material system is formed by being sequentially connected the liquid storage bottle connect, metering pump and solid sampling column, and the organic solvent in liquid storage bottle is measuring
Under the action of pump, it can fall in the shape of a spiral along the inner wall of solid sampling column.By above-mentioned feed proportioning system it is found that having in liquid storage bottle
Solvent can fall in the shape of a spiral along the inner wall of solid sampling column, to take away the agglomeration of the viscous wall on inner wall, and then avoid artificial
Handle manually the operation of agglomeration.Therefore, wet process mix grinding device proposed by the present invention is able to solve raw material and is easy asking for viscous wall agglomeration
Topic reduces operator's workload, solves the problems, such as the field at this stage.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the schematic diagram of wet process mix grinding device in the specific embodiment of the invention.
In Fig. 1:
First valve -1, the second valve -2, third valve -3, the 4th valve -4, the 5th valve -5, the 6th valve
Door -6, the 7th valve -7, circulating water type vacuum pump -8, liquid storage bottle -9, metering pump -10, solid sampling column -11, stirring
Device -12, interlayer reaction kettle -13, temperature control cycles device -14, ball mill -15, peristaltic pump -16, rewinding bottle -17.
Specific embodiment
The core of present embodiment is to provide a kind of wet process mix grinding device, the device be able to solve raw material be easy it is viscous
The problem of wall agglomerates reduces operator's workload, solves the problems, such as the field at this stage.
Hereinafter, being illustrated referring to attached drawing to embodiment.In addition, embodiments illustrated below is not to recorded in claim
Summary of the invention rise any restriction effect.In addition, the full content of composition represented by following example is not limited to as right
Necessary to the solution invented documented by it is required that.
Wet process mix grinding device proposed by the present invention, referring to Figure 1;Including:Feed proportioning system, mixing system, crushing system, receipts
Material system;Feed proportioning system is formed by being sequentially connected the liquid storage bottle connect 9, metering pump 10 and solid sampling column 11, and in liquid storage bottle 9
Organic solvent under the action of metering pump 10, can fall in the shape of a spiral along the inner wall of solid sampling column 11.By above-mentioned ingredient system
System is it is found that the organic solvent in liquid storage bottle 9 can fall in the shape of a spiral along the inner wall of solid sampling column 11, to take away on inner wall
Viscous wall agglomeration, and then avoid the operation for manually handling agglomeration.Therefore, wet process mix grinding device proposed by the present invention, can solve
Certainly raw material is easy the problem of viscous wall agglomeration, reduces operator's workload, solves the problems, such as the field at this stage.
Wet process mix grinding device proposed by the present invention, mixing system include:Interlayer reaction kettle 13 is plugged in interlayer reaction kettle 13
Blender 12, for controlling the temperature control cycles device 14 of 13 temperature of interlayer reaction kettle;Interlayer reaction kettle 13 and solid sampling
Column 11 is connected.Crushing system is made of the ball mill 15 and peristaltic pump 16 being connected;Peristaltic pump 16 and 13 phase of interlayer reaction kettle
Connection, for the mixing in interlayer reaction kettle 13 to be delivered to ball mill 15, and sends the mixing after mill back to interlayer reaction kettle 13.
Material-receiving system includes:The rewinding bottle 17 being connected with interlayer reaction kettle 13, the vacuum pump being connected with rewinding bottle 17.It is specific such as to scheme
Shown in 1.
Wet process mix grinding device proposed by the present invention, vacuum pump can be circulating water type vacuum pump 8 or other can be played
The pump of equivalent effect.
Wet process mix grinding device proposed by the present invention, 11 both ends of the first valve 1 and solid sampling column on liquid storage bottle 9
Second valve 2 and third valve 3 can be three-way valve, in order to control the emptying of gas in feed proportioning system;Similarly, interlayer
Being used to connect the 4th valve 4 of ball mill 15 on reaction kettle 13 can be three-way valve.
Wet process mix grinding device proposed by the present invention, the 5th valve 5 on interlayer reaction kettle 13 for connecting rewinding bottle 17 are
Two-way valve;The 7th valve on rewinding bottle 17 for the 6th valve 6 of connection interlayer reaction kettle 13 and for connecting vacuum pump
7 be two-way valve;Certainly, each valve type selection can according to the actual situation depending on.
The present invention also proposes a kind of method for preparing sulfide electrolyte precursor, including step:
Step 1, ingredient weigh various powder raw materials by the proportion of sulfide electrolyte in glove box, are placed in solid
In body sample introduction column 11, the second valve 2 and third valve 3 are closed;Organic solvent is added in liquid storage bottle 9 and closes the first valve 1;
Solid sampling column 11 and liquid storage bottle 9 are taken out from glove box again;Configure clean zirconia ball be fitted into it is in ball mill 15 and close
Seal ball mill 15;
Step 2, exhaust, argon bottle is connected with the first valve 1, by between the first valve 1 and the second valve 2 pipeline,
And the air in metering pump 10 is discharged from three ports of the second valve 2;After emptying, first by the pressure reducing valve auxiliary-valve tune on argon bottle
Extremely small pressure, and the second valve 2 and the first valve 1 are successively opened, finally close pressure reducing valve auxiliary-valve;Similarly, mixing system is emptied
Air in system, crushing system, material-receiving system and associated pipe;
Step 3, feed fluid injection, opens third valve 3, the solid powder in solid sampling column 11 is made to fall to folder automatically
Layer reaction kettle 13;It opens metering pump 10 and sets the fluid injection volume of organic solvent in liquid storage bottle 9, make organic solvent along solid sampling
The inner wall of column 11 falls in the shape of a spiral, agglomerates and flows into interlayer reaction kettle 13 to take away viscous wall, and metering is closed after the completion of fluid injection
Pump 10 and third valve 3;
Step 4, mixing crush, and open simultaneously set temperature control loop device 14, such as interlayer reaction kettle 13 is kept the temperature 30
DEG C or so;The revolution and runing time of setting blender 12 simultaneously start, such as revolution can be 200rpm, and runing time can be
2h;After the slurry agitation in interlayer reaction kettle 13 is uniform, the flow and runing time of setting peristaltic pump 16 simultaneously start, such as flow
Amount can be 500mL/mi n, and the time can be 10h;The revolution and runing time of setting ball mill 15 simultaneously start, such as revolution
It can be 500rpm, runing time can be 10h;After the reaction was completed, peristaltic pump 16, ball mill 15 and blender 12 are closed;Again
It opens peristaltic pump 16 and reversely rotates peristaltic pump 16, the slurry in ball mill 15 and associated pipe is evacuated to interlayer reaction
Kettle 13 finally closes peristaltic pump 16;In addition, above-mentioned parameter can specifically be set according to the actual situation in practical operation;
Step 5, rewinding start circulating water type vacuum pump 8 and open the 7th valve 7, to evacuate the gas in rewinding bottle 17
Body;When the pressure of circulating water type vacuum pump 8 reaches maximum value, the 5th valve 5 and the 6th valve 6 are opened, interlayer reaction kettle is made
Slurry in 13 flow to rewinding bottle 17;After slurry fully flows into rewinding bottle 17, the 5th valve 5, the 6th valve 6 and the 7th are closed
Valve 7, and close circulating water type vacuum pump 8;After slurry in rewinding bottle 17 is evaporated under reduced pressure and is dried, sulfide is obtained
Electrolyte precursor.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of wet process mix grinding device, which is characterized in that including:Feed proportioning system, mixing system, crushing system, material-receiving system;Institute
It states feed proportioning system and is formed by being sequentially connected the liquid storage bottle connect (9), metering pump (10) and solid sampling column (11), and the liquid storage bottle
(9) organic solvent under the action of the metering pump (10), can along the solid sampling column (11) inner wall helically
Shape falls.
2. wet process mix grinding device according to claim 1, which is characterized in that the mixing system includes:Interlayer reaction kettle
(13), it is plugged in the blender (12) of the interlayer reaction kettle (13), for controlling the temperature of interlayer reaction kettle (13) temperature
It spends control loop device (14);The interlayer reaction kettle (13) is connected with the solid sampling column (11).
3. wet process mix grinding device according to claim 2, which is characterized in that the crushing system is by the ball mill that is connected
(15) it is formed with peristaltic pump (16);The peristaltic pump (16) is connected with the interlayer reaction kettle (13), is used for the interlayer
Mixing in reaction kettle (13) is delivered to the ball mill (15), and sends the mixing after mill back to the interlayer reaction kettle (13).
4. wet process mix grinding device according to claim 2, which is characterized in that the material-receiving system includes:With the interlayer
Rewinding bottle (17) that reaction kettle (13) is connected, the vacuum pump being connected with the rewinding bottle (17).
5. wet process mix grinding device according to claim 4, which is characterized in that the vacuum pump is circulating water type vacuum pump
(8)。
6. wet process mix grinding device according to claim 1, which is characterized in that the first valve on the liquid storage bottle (9)
(1) and second valve (2) at the solid sampling column (11) both ends and third valve (3) are three-way valve, in order to control
Make the emptying of gas in the feed proportioning system.
7. wet process mix grinding device according to claim 3, which is characterized in that for connecting on the interlayer reaction kettle (13)
4th valve (4) of the ball mill (15) is three-way valve.
8. wet process mix grinding device according to claim 4, which is characterized in that for connecting on the interlayer reaction kettle (13)
5th valve (5) of the rewinding bottle (17) is two-way valve.
9. wet process mix grinding device according to claim 4, which is characterized in that described for connecting on the rewinding bottle (17)
6th valve (6) of interlayer reaction kettle (13) and the 7th valve (7) for connecting the vacuum pump are two-way valve.
10. a kind of method for preparing sulfide electrolyte precursor, which is characterized in that including step:
Step 1, ingredient weigh various powder raw materials by the proportion of sulfide electrolyte in glove box, be placed in solid into
In sample column (11), the second valve (2) and third valve (3) are closed;Organic solvent is added in liquid storage bottle (9) and closes the first valve
Door (1);The solid sampling column (11) and the liquid storage bottle (9) are taken out from the glove box again;Configure clean oxidation
Zirconium ball is fitted into ball mill (15) and seals the ball mill (15);
Step 2, exhaust, argon bottle is connected with first valve (1), by first valve (1) and second valve
(2) air in pipeline and metering pump (10) between is discharged from three ports of second valve (2);After emptying, first by institute
The pressure reducing valve auxiliary-valve stated on argon bottle is adjusted to small pressure, and successively opens second valve (2) and first valve
(1), the pressure reducing valve auxiliary-valve is finally closed;Similarly, it empties in mixing system, crushing system, material-receiving system and associated pipe
Air;
Step 3, feed fluid injection, opens third valve (3), the solid powder in the solid sampling column (11) is made to fall automatically
To interlayer reaction kettle (13);It opens metering pump (10) and sets the fluid injection volume of the liquid storage bottle (9) interior organic solvent, make described
Organic solvent falls in the shape of a spiral along the inner wall of the solid sampling column (11), agglomerates to take away viscous wall and flows into interlayer reaction kettle
(13) in, the metering pump (10) and the third valve (3) are closed after the completion of fluid injection;
Step 4, mixing crush, and open simultaneously set temperature control loop device (14), when setting revolution and the operation of blender (12)
Between and start;After the slurry agitation in the interlayer reaction kettle (13) is uniform, when setting flow and the operation of peristaltic pump (16)
Between and start;The revolution and runing time of setting ball mill (15) simultaneously start;After the reaction was completed, close the peristaltic pump (16),
The ball mill (15) and the blender (12);The peristaltic pump (16) is opened again and makes its reverse rotation, by the pearl
Slurry in grinding machine (15) and associated pipe is evacuated to the interlayer reaction kettle (13), finally closes the peristaltic pump (16);
Step 5, rewinding start circulating water type vacuum pump and open the 7th valve (7), to evacuate the gas in rewinding bottle (17);
When the pressure of the circulating water type vacuum pump reaches maximum value, the 5th valve (5) and the 6th valve (6) are opened, the folder is made
Slurry in layer reaction kettle (13) flow to the rewinding bottle (17);After slurry fully flows into rewinding bottle (17), institute is closed
The 5th valve (5), the 6th valve (6) and the 7th valve (7) are stated, and closes the circulating water type vacuum pump;To institute
It states after the slurry in rewinding bottle (17) is evaporated under reduced pressure and dried, obtains sulfide electrolyte precursor.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810795958.2A CN108854915A (en) | 2018-07-19 | 2018-07-19 | A kind of wet process mix grinding device and the method for preparing sulfide electrolyte precursor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810795958.2A CN108854915A (en) | 2018-07-19 | 2018-07-19 | A kind of wet process mix grinding device and the method for preparing sulfide electrolyte precursor |
Publications (1)
Publication Number | Publication Date |
---|---|
CN108854915A true CN108854915A (en) | 2018-11-23 |
Family
ID=64303623
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810795958.2A Pending CN108854915A (en) | 2018-07-19 | 2018-07-19 | A kind of wet process mix grinding device and the method for preparing sulfide electrolyte precursor |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108854915A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109604607A (en) * | 2018-12-19 | 2019-04-12 | 技锋精密刀具(马鞍山)有限公司 | A kind of production technology effectively improving hard alloy dise knife blank qualification rate |
CN110327865A (en) * | 2019-05-28 | 2019-10-15 | 浙江锋锂新能源科技有限公司 | The device and treatment process for being heat-treated and being modified suitable for sulfide solid electrolyte |
CN113410513A (en) * | 2021-06-16 | 2021-09-17 | 多氟多新能源科技有限公司 | Preparation method of sulfide solid electrolyte |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103769030A (en) * | 2014-02-20 | 2014-05-07 | 枣庄市荣宝莱建材科技发展有限公司 | Automatic production equipment for polycarboxylate superplasticizer |
CN104474994A (en) * | 2014-11-12 | 2015-04-01 | 昆明贵研催化剂有限责任公司 | Integrated slurry preparation system and preparation method |
WO2016167302A1 (en) * | 2015-04-17 | 2016-10-20 | 出光興産株式会社 | Method for producing sulfide solid electrolyte and sulfur-based material |
CN108075182A (en) * | 2016-11-16 | 2018-05-25 | 现代自动车株式会社 | The method that the solid electrolyte based on sulfide is manufactured by wet process |
-
2018
- 2018-07-19 CN CN201810795958.2A patent/CN108854915A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103769030A (en) * | 2014-02-20 | 2014-05-07 | 枣庄市荣宝莱建材科技发展有限公司 | Automatic production equipment for polycarboxylate superplasticizer |
CN104474994A (en) * | 2014-11-12 | 2015-04-01 | 昆明贵研催化剂有限责任公司 | Integrated slurry preparation system and preparation method |
WO2016167302A1 (en) * | 2015-04-17 | 2016-10-20 | 出光興産株式会社 | Method for producing sulfide solid electrolyte and sulfur-based material |
CN108075182A (en) * | 2016-11-16 | 2018-05-25 | 现代自动车株式会社 | The method that the solid electrolyte based on sulfide is manufactured by wet process |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109604607A (en) * | 2018-12-19 | 2019-04-12 | 技锋精密刀具(马鞍山)有限公司 | A kind of production technology effectively improving hard alloy dise knife blank qualification rate |
CN109604607B (en) * | 2018-12-19 | 2020-12-29 | 技锋精密刀具(马鞍山)有限公司 | Production process for effectively improving qualified rate of hard alloy circular cutter blank |
CN110327865A (en) * | 2019-05-28 | 2019-10-15 | 浙江锋锂新能源科技有限公司 | The device and treatment process for being heat-treated and being modified suitable for sulfide solid electrolyte |
CN113410513A (en) * | 2021-06-16 | 2021-09-17 | 多氟多新能源科技有限公司 | Preparation method of sulfide solid electrolyte |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108854915A (en) | A kind of wet process mix grinding device and the method for preparing sulfide electrolyte precursor | |
CN206139178U (en) | Chemistry chemical reaction tank | |
CN108636145A (en) | A kind of dry method slurry preparation technique | |
CN206868363U (en) | A kind of processing tank of bio-fuel | |
CN206304741U (en) | A kind of polyurethane resin reactor | |
CN109465965A (en) | A kind of architectural engineering agitating device and its application method | |
CN201954926U (en) | Vacuum stirring-up drying machine | |
CN110282664B (en) | Production method and continuous production equipment of nickel cobalt lithium manganate anode material | |
CN210885340U (en) | Continuous production equipment for nickel cobalt lithium manganate positive electrode material | |
CN204911507U (en) | Melamine resin reation kettle | |
CN108405175A (en) | A kind of solid waste impurity automatic electromagnetic screening plant and method | |
CN212632476U (en) | High-purity gallium oxide raw material processing equipment | |
CN210321274U (en) | Efficient smelting device for manufacturing copper artware | |
CN208557918U (en) | A kind of easy-to-dismount cement mixer transmission waterproof case | |
CN221108086U (en) | Powder material injection device of electrolyte blending kettle | |
CN214521061U (en) | Cement dry powder mixing arrangement | |
CN210163187U (en) | Flocculating agent charge device | |
CN206457504U (en) | One kind is used to prepare catalase reaction axe | |
CN207480886U (en) | A kind of blender | |
CN206444484U (en) | A kind of high efficiency fertilizer agitating device | |
CN206355852U (en) | A kind of honey agitator of efficient material-saving | |
CN207131046U (en) | A kind of automanual plastering plate | |
CN205731237U (en) | Reactor | |
CN205886755U (en) | Ball formula agitating unit | |
CN205699509U (en) | A kind of continuous drier for lithium ion cell positive powder body material |
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 | ||
TA01 | Transfer of patent application right | ||
TA01 | Transfer of patent application right |
Effective date of registration: 20190725 Address after: 315040 Room 305, 3/F, 044 Building, 66 Qingyi Road, Ningbo High-tech Zone, Zhejiang Province Applicant after: Zhejiang Feng Li Amperex Technology Limited Address before: No. 519 Road, 315201 Zhejiang Zhuang Zhenhai District of city of Ningbo Province Applicant before: Ningbo Institute of Material Technology and Engineering Chinese Academy of Scien |
|
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181123 |