CN207398268U - A kind of consersion unit for preparing ternary material precursor - Google Patents
A kind of consersion unit for preparing ternary material precursor Download PDFInfo
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- CN207398268U CN207398268U CN201721473432.XU CN201721473432U CN207398268U CN 207398268 U CN207398268 U CN 207398268U CN 201721473432 U CN201721473432 U CN 201721473432U CN 207398268 U CN207398268 U CN 207398268U
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Abstract
The utility model proposes a kind of consersion unit for preparing ternary material precursor, including：Complexing agent storage tank, alkali liquor storage tank, mixing salt solution storage tank；Microchannel reaction unit, sets that there are three feed inlet and a discharge ports on the microchannel reaction unit；Each storage tank is connected with a feed inlet on the reaction unit of microchannel；Accurate measurement pump is additionally provided between the storage tank and feed inlet；The outside of microchannel section is equipped with heat exchanger channels in the microchannel reaction unit；Crystallization kettle is connected with the discharge port of the microchannel reaction unit；The crystallization kettle includes agitating device and thermosistor；Filter device is connected with the discharge port of the crystallization kettle；The filter device includes liquid outlet opening and solid outlet；And drier, it is connected with the solid outlet of the filter device.The utility model is with microchannel reaction unit instead of the jacket reactor in traditional handicraft, and product quality obtained is stablized, uniform particle sizes.
Description
Technical field
The utility model is related to prepare the apparatus field of anode material of lithium battery, particularly relate to it is a kind of prepare ternary material before
Drive the consersion unit of body.
Background technology
Ternary material is one kind of anode material of lithium battery, due to that security is good, gram specific capacity height, price are low etc. is excellent
Gesture becomes one of following lithium battery industry development direction.The application technology relative maturity of ternary material, market prospects are optimistic.
The preparation process of ternary material precursor is mainly chemical coprecipitation at present, in particular by stirred autoclave system
Standby nickel-cobalt-manganese ternary material precursor.Tertiary cathode material precursor, preparation method and its use as disclosed in CN105070903A
On the way, a kind of preparation method of nickel-cobalt-manganese ternary material disclosed in CN103746110A is prepared using coprecipitation reaction kettle
Ternary material precursor.But the ternary material precursor prepared using reaction kettle, since material mixes not enough in a kettle
It is even, there are concentration difference during mixing, affect product quality；For controlling reaction temperature, charging cannot be too fast so that anti-per kettle
Between seasonable when 15-30 is small；Moreover, side border ring crystalline deposit so that reaction condition and crystallization condition were reacted entirely
There are apparent difference in journey, cause to match that variant, crystal grain is uneven, crystal grain control difficulty is big, and product stability is poor；And
In order to improve reaction condition, the rabbling mechanism of high rotating speed (600~1200rpm) is taken, not only energy consumption is big, also destroys crystal grain knot
Structure.
In view of this, it is necessary to research and develop a kind of consersion unit for preparing ternary material precursor, stablize its reaction product
Property it is good, the simultaneous reactions time is short and reaction condition control accuracy is high.
Utility model content
The utility model proposes a kind of consersion units for preparing ternary material precursor, and it is steady to solve product in the prior art
The problem of qualitative difference.
The utility model proposes a kind of consersion unit for preparing ternary material precursor, solve when reacting in the prior art
Between long, reaction condition the problem of being difficult to accurately control.
What the technical solution of the utility model was realized in：
A kind of consersion unit for preparing ternary material precursor, including：
Complexing agent storage tank, alkali liquor storage tank, mixing salt solution storage tank；
Microchannel reaction unit, sets that there are three feed inlet and a discharge ports on the microchannel reaction unit；Each institute
Storage tank is stated with a feed inlet on the reaction unit of microchannel to be connected；Accurate measurement is additionally provided between the storage tank and feed inlet
Pump；The outside of microchannel section is equipped with heat exchanger channels in the microchannel reaction unit；
Crystallization kettle is connected with the discharge port of the microchannel reaction unit；The crystallization kettle includes agitating device and tune
Warm device；
Filter device is connected with the discharge port of the crystallization kettle；The filter device includes liquid outlet opening and solid
Discharge port；And
Drier is connected with the solid outlet of the filter device.
As preferred technical solution, the heat exchanger channels connection cooling water inlet, cooling water outlet, hot oil inlet and heat
Oil export.
As preferred technical solution, material-handling pump is equipped between the crystallization kettle and filter device.
As preferred technical solution, the liquid outlet opening of the filter device is connected with fluid reservoir.
A kind of preparation method of ternary material precursor, including：
Nickel salt, cobalt salt, the salting liquid of manganese salt are mixed, obtains nickel cobalt manganese mixing salt solution；
Or
Nickel salt, cobalt salt, the salting liquid of aluminium salt are mixed, obtains nickel cobalt aluminium mixing salt solution；
The nickel cobalt manganese mixing salt solution, complexing agent and aqueous slkali are passed through in the reaction unit of microchannel, described micro-
It is fully reacted in the heat exchanging segment microchannel of pathway reaction device, subsequently enters crystallization kettle, post-processed after crystallization, obtain ternary
Material precursor.
As preferred technical solution, the temperature of the heat exchanging segment micro passage reaction is controlled between 40 DEG C~60 DEG C,
Temperature control precision is ± 0.5 DEG C~± 5 DEG C.
As preferred technical solution, the nickel salt is one or more of halide of nickel sulfate, nickel nitrate, nickel；
The cobalt salt is one or more of halide of cobaltous sulfate, cobalt nitrate, cobalt；The manganese salt is manganese sulfate, manganese nitrate, manganese
One or more of halide；The ternary material precursor of acquisition is nickel cobalt manganese hydroxide (NCM).
As preferred technical solution, the nickel salt is one or more of halide of nickel sulfate, nickel nitrate, nickel；
The cobalt salt is one or more of halide of cobaltous sulfate, cobalt nitrate, cobalt, and the aluminium salt is aluminum sulfate, aluminum nitrate, aluminium
One or more of halide；The ternary material precursor of acquisition is nickel cobalt aluminium hydroxide (NCA).
As preferred technical solution, the complexing agent is ammonium hydroxide.
As preferred technical solution, the aqueous slkali is sodium hydroxide solution.
As preferred technical solution, the post processing includes the step of separation of solid and liquid is with solid material is dried.
As preferred technical solution, the temperature of the drying solid material is 135 DEG C -290 DEG C.When temperature is 300 DEG C
When, obtained presoma powder has rotten possibility.
Advantageous effect
(1) the utility model with microchannel reaction unit instead of the jacket reactor in traditional handicraft, product obtained
Stable quality, uniform particle sizes.
(2) material of the utility model is after accurate measurement, is mixed in microchannel, and mixing uniformity is good；And
And the reaction time is short (0.1~1 second), instantaneous to complete to be sufficiently mixed and fully react during microchannel is flowed through, each drop
The reaction of material is completed under identical proportioning, and the reaction condition of entire technique is also precisely controlled, therefore
The ternary material precursor of high quality can be made.
(3) temperature control precision of the utility model can reach ± 0.5 DEG C, can be directed to different ternary material formulas, essence
True controlling reaction temperature improves product quality.
(4) crystallization of the utility model is completed in the crystallization kettle after fast reaction, and crystallization condition can be controlled precisely
System, grain structure are stablized, and grain size is controllable.
(5) stirring of the utility model crystallization kettle is low speed (30~60rpm) stirring, and low energy consumption, crystal grain is destroyed small.
(6) equipment connecting relation of the utility model is simple, small, convenient for industrial application.
Description of the drawings
It, below will be to implementing in order to illustrate more clearly of the utility model embodiment or technical solution of the prior art
Scheme or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, the accompanying drawings in the following description
Only some embodiments of the utility model for those of ordinary skill in the art, are not making the creative labor
On the premise of property, other attached drawings are can also be obtained according to these attached drawings.
Fig. 1 is a kind of structure diagram of consersion unit for preparing ternary material precursor in the present embodiment 1.
Specific embodiment
Below by the technical scheme in the utility model embodiment is clearly and completely described, it is clear that described
Embodiment is only the utility model part of the embodiment, instead of all the embodiments.Based on the implementation in the utility model
Example, those of ordinary skill in the art's all other embodiments obtained without making creative work, belongs to
The scope of the utility model protection.
The reagent referred in following embodiments is commercially available.
Embodiment 1
Shown in Figure 1, a kind of consersion unit for preparing ternary material precursor is stored up including complexing agent storage tank 11, lye
Tank 12, mixing salt solution storage tank 13；Microchannel reaction unit 16, crystallization kettle 17, filter device 18 and drier 19.It is micro- logical
It is set on road reaction unit 16 there are three feed inlet, is respectively 161,162 and 163.Go out there are one being set on microchannel reaction unit 16
Material mouth 164.Each storage tank is connected with a feed inlet on microchannel reaction unit 16.11 are connected with 161 in the present embodiment,
12 are connected with 162, and 13 are connected with 163.Accurate measurement pump 14 is also connected between each storage tank and feed inlet.Microchannel plate should fill
The outside for putting microchannel section in 16 is equipped with heat exchanger channels (not marked in figure).Heat exchange mode in the present embodiment drops for cooling water
Temperature, deep fat heating；Therefore cooling water inlet 211 and cooling water outlet 212, hot oil inlet 213 and hot oil outlet 214 are provided with.
Agitating device 171 and thermosistor 172, the discharge port 164 that material passes through microchannel reaction unit 16 are provided in the crystallization kettle 17
After in into crystallization kettle 17,171 low speed of agitating device (30~60rpm) stirring, low energy consumption, crystal grain is destroyed small.Filter device
18 are connected with the discharge port of crystallization kettle 17, which includes liquid outlet opening (not marked in figure) and solid outlet
181.The solid outlet 181 is connected with drier 19.The liquid of the liquid outlet opening outflow of filter device 18 is passed through fluid reservoir
(not marked in figure) stores.Material-handling pump 15 is additionally provided in the present embodiment between crystallization kettle 17 and filter device 18.By material
It delivers into filter device 18.Wherein filter device 18 can make choice according to the needs of those skilled in the art, this reality
Apply that be selected in example be filter press.
Application examples 1
Ternary material precursor is prepared using the equipment in embodiment 1.
A kind of preparation method of ternary material precursor, including：
(1) be respectively by isometric concentration 3.4mol/L, 1.5mol/L and 1.3mol/L nickel sulfate solution, cobaltous sulfate
Solution and manganese sulfate solution mixing, obtain mixing salt solution.
(2) mixing salt solution in step (1) is entered by feed inlet 163 in microchannel reaction unit 16, concentration is
The ammonium hydroxide of 0.5mol/L is entered by complexing agent feed inlet 161 in microchannel reaction unit 16, and concentration is that the NaOH of 4mol/L is molten
Liquid is passed through by aqueous slkali feed inlet 162 in microchannel reaction unit 16, the reaction unit 16 in microchannel (for adjusting pH)
Heat exchanging segment reacts in microchannel, and reaction temperature control is at 55 DEG C, pH=12.Reaction instantaneously can be completed.Temperature control precision is
± 0.5 DEG C~± 5 DEG C.
(3) solution after reaction is passed through by discharge port 164 in crystallization kettle 17, in the stirring at low speed of agitating device 171
Under, still aging 16h forms presoma colloid；Presoma colloid centrifugal concentrating is obtained into aqueous precursor gel；Into plate compression
In, by filtering, washing, the aqueous precursor gel after washing is passed through in drier 19, before dry 5h can be obtained at 135 DEG C
Drive body powder.
Powder particle pattern obtained above is spherical in shape, grain size be uniform normal distribution, total metal contents in soil 61.81%,
Specific surface area 4.3m2/g。
Application examples 2
A kind of preparation method of ternary material precursor, including：
(1) be respectively by isometric concentration 3.4mol/L, 1.5mol/L and 1.3mol/L nickel sulfate solution, cobaltous sulfate
Solution and manganese sulfate solution mixing, obtain mixing salt solution.
(2) it is 6mol/L's by ammonium hydroxide and concentration that the mixing salt solution in step (1) and concentration are 0.5mol/L
NaOH solution is passed through in the reaction unit of microchannel, the heat exchanging segment microchannel plate of reaction unit in microchannel jointly (for adjusting pH)
It answers in device and reacts, reaction temperature control is at 40 DEG C, pH=10.5.Reaction instantaneously can be completed.
(3) solution after reaction is passed through the still aging 13h of aging reactor and forms presoma colloid；By the presoma colloid
Centrifugal concentrating obtains aqueous precursor gel；By filtering, washing, the aqueous precursor gel after washing is dried into 5h at 150 DEG C
Obtain presoma powder.
Powder particle pattern obtained above is spherical in shape, grain size be uniform normal distribution, total metal contents in soil 61.83%,
Specific surface area 4.4m2/g。
Application examples 3
A kind of preparation method of ternary material precursor, including：
(1) be respectively by isometric concentration 3.4mol/L, 1.5mol/L and 2.0mol/L nickel sulfate solution, cobaltous sulfate
Solution and aluminum sulfate solution mixing, obtain mixing salt solution.
(2) it is 4mol/L's by ammonium hydroxide and concentration that the mixing salt solution in step (1) and concentration are 1.0mol/L
NaOH solution is passed through in the reaction unit of microchannel, the heat exchanging segment microchannel plate of reaction unit in microchannel jointly (for adjusting pH)
It answers in device and reacts, reaction temperature control is at 60 DEG C, pH=11.Reaction instantaneously can be completed.
(3) solution after reaction is passed through the still aging 15h of aging reactor and forms presoma colloid；By the presoma colloid
Centrifugal concentrating obtains aqueous precursor gel；By filtering, washing, the aqueous precursor gel after washing is dried into 5h at 300 DEG C
Obtain presoma powder.
Powder particle obtained above be bulk and its aggregate (rotten) not of uniform size, total metal contents in soil 62.21%,
Specific surface area 52.6m2/g.So drying temperature will be less than 300 DEG C.
The above is only the preferred embodiment of the utility model only, is not intended to limit the utility model, all at this
Within the spirit and principle of utility model, any modifications, equivalent replacements and improvements are made should be included in the utility model
Protection domain within.
Claims (4)
1. a kind of consersion unit for preparing ternary material precursor, which is characterized in that including：
Complexing agent storage tank, alkali liquor storage tank, mixing salt solution storage tank；
Microchannel reaction unit, sets that there are three feed inlet and a discharge ports on the microchannel reaction unit；Each storage
Tank is connected with a feed inlet on the reaction unit of microchannel；Accurate measurement pump is additionally provided between the storage tank and feed inlet；
The outside of microchannel section is equipped with heat exchanger channels in the microchannel reaction unit；
Crystallization kettle is connected with the discharge port of the microchannel reaction unit；The crystallization kettle includes agitating device and thermosistor；
Filter device is connected with the discharge port of the crystallization kettle；The filter device includes liquid outlet opening and solids exit
Mouthful；And
Drier is connected with the solid outlet of the filter device.
A kind of 2. consersion unit for preparing ternary material precursor according to claim 1, which is characterized in that the heat exchange
Passage connection cooling water inlet, cooling water outlet, hot oil inlet and hot oil outlet.
A kind of 3. consersion unit for preparing ternary material precursor according to claim 1, which is characterized in that the crystallization
Material-handling pump is equipped between kettle and filter device.
A kind of 4. consersion unit for preparing ternary material precursor according to claim 1, which is characterized in that the filtering
The liquid outlet opening of device is connected with fluid reservoir.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721473432.XU CN207398268U (en) | 2017-11-07 | 2017-11-07 | A kind of consersion unit for preparing ternary material precursor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721473432.XU CN207398268U (en) | 2017-11-07 | 2017-11-07 | A kind of consersion unit for preparing ternary material precursor |
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| CN207398268U true CN207398268U (en) | 2018-05-22 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107834046A (en) * | 2017-11-07 | 2018-03-23 | 衢州市鼎盛化工科技有限公司 | The preparation method and its consersion unit of ternary material precursor |
| CN111807422A (en) * | 2020-07-21 | 2020-10-23 | 桐乡比西新能源科技有限公司 | Ternary positive electrode material precursor liquid phase fusion modification process |
-
2017
- 2017-11-07 CN CN201721473432.XU patent/CN207398268U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107834046A (en) * | 2017-11-07 | 2018-03-23 | 衢州市鼎盛化工科技有限公司 | The preparation method and its consersion unit of ternary material precursor |
| CN111807422A (en) * | 2020-07-21 | 2020-10-23 | 桐乡比西新能源科技有限公司 | Ternary positive electrode material precursor liquid phase fusion modification process |
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| CB03 | Change of inventor or designer information |
Inventor after: Zhou Zhenfeng Inventor after: Dong Hanjie Inventor after: Ying Shengrong Inventor after: Jiang Zhan Inventor after: Ying Yue Inventor before: Zhou Zhenfeng Inventor before: Dong Hanjie Inventor before: Ying Shengrong |