CN110304643A - A kind of the hypergravity preparation method and system of the ultra-fine lithium carbonate of LITHIUM BATTERY - Google Patents
A kind of the hypergravity preparation method and system of the ultra-fine lithium carbonate of LITHIUM BATTERY Download PDFInfo
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- CN110304643A CN110304643A CN201910023755.6A CN201910023755A CN110304643A CN 110304643 A CN110304643 A CN 110304643A CN 201910023755 A CN201910023755 A CN 201910023755A CN 110304643 A CN110304643 A CN 110304643A
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- lithium
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- hypergravity
- lithium battery
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
Abstract
The present invention relates to a kind of hypergravity preparation methods of the ultra-fine lithium carbonate of LITHIUM BATTERY, it mainly uses the hypergravity effect of Impinging Stream-Rotating Packed Bed that reaction mass is promoted to flow contact in porous media, it tears to generate significant shear power for liquid into nanoscale liquid film, brin or drop, strengthen interior microscopic mixing to act on reaction mass transfer, prepares the ultra-fine carbonic acid powder for lithium of LITHIUM BATTERY in combination with reaction crystallization process control technology.The hypergravity preparation method is mainly using high brine containing lithium and sodium carbonate liquor as raw material, wherein the lithium concentration control in raw brine is 1-50g/L, sodium carbonate synchronizes addition by 0.5-0.7 times of lithium ion molal quantity, and material is 50-4000m/s in acceleration2Elevated Gravity in reactive crystallization, the crystal material of acquisition can be prepared by ultra-fine carbonic acid powder for lithium after the ageing of 3-8h.
Description
Technical field
The present invention relates to chemical crystallization technical fields, specifically, being a kind of hypergravity system of ultra-fine lithium carbonate of LITHIUM BATTERY
Preparation Method and system.
Background technique
Lithium is known as " important element for pushing the world to advance " as a kind of indispensable strategic resource.Lithium carbonate is made
It is most basic, most critical product in lithium industry for a kind of basic lithium salts, has that stability is good, production cost is relatively low
Advantage can be directly used as the intermediate product of the various lithium salts productions such as lithium hydroxide, lithium chloride, lithium bromide.
Since the fields such as new energy battery, new material require lithium carbonate purity, granularity and pattern very high, domestic scholars warp
The research of more than 30 years is gone through, it is just basic to establish using brine as the lithium carbonate preparative separation method of raw material.But current research hotspot
It is confined to the raising of lithium carbonate yield, then rarely has to the investigation of lithium carbonate partial size and is related to, and lithium carbonate has multilevel structure, with poly-
It is serious to become main secondary crystallization phenomenon, greatly affected properties of product.Especially battery-level lithium carbonate, granularity requirements
Height, to be clearly present that product cut size is big, particle diameter distribution is uneven, settling property is poor in routinely production preparation process etc. a series of to ask
Topic.
Impinging Stream-Rotating Packed Bed (IS-RPB) is effective production equipment of superfine powdery material, under Elevated Gravity,
Reaction mass carries out flowing contact in porous media or duct, and the huge shearing force of generation promotes liquid to be torn into receive
Film, silk or the drop of meter level effectively enhance microcosmic mixing and the mass transfer of reaction, promote the generation of ultra-fine grain powder.Mesh
Before, IS-RPB has been successfully applied to the production of a variety of nano-powders, but there are no the report about the preparation of ultra-fine carbonic acid powder for lithium.
The present invention mainly uses Impinging Stream-Rotating Packed Bed equipment, proposes a kind of hypergravity preparation of ultra-fine lithium carbonate
Method, by interior microscopic mixing, the reinforcing of peptizaiton, the control of association reaction crystallization process realizes that battery-level lithium carbonate produces
The particle size of product controls, and prepares ultra-fine carbonic acid powder for lithium.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of hypergravity systems of the ultra-fine lithium carbonate of LITHIUM BATTERY
Preparation Method and system, mainly by hypergravity process intensification technology, association reaction crystallization process optimal control realizes that lithium carbonate is brilliant
The Effective Regulation of body size, to prepare the ultra-fine carbonic acid powder for lithium of LITHIUM BATTERY.
Technical solution of the present invention:
A kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY is mainly acted on by hypergravity and strengthens reaction mass
Mixing and dispersion, and then prepare the ultra-fine carbonic acid powder for lithium of LITHIUM BATTERY, which is characterized in that main body hypergravity equipment using hit
The rotary packed bed device form of stream-.
It technically says, the hypergravity effect of Impinging Stream-Rotating Packed Bed promotes reaction mass to flow in porous media, produces
Raw significant shear power tears liquid at nanoscale liquid film, brin or drop, thus strengthen material mixing and peptizaiton,
To promote formation and its size of sub-micron-powder quantitatively to control.
A kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY of the present invention, the ultra-fine lithium carbonate preparation of LITHIUM BATTERY
Using high brine containing lithium and sodium carbonate liquor as raw material, charge pump is opened, aqueous salt brine is added with certain charging rate, by reaction
Molar ratio adds sodium carbonate liquor, meanwhile, start supergravity reactor, adjusts rotary speed, adults power acceleration；Divided
Scattered material is impinged upon on reactor wall after radial throw away under the influence of centrifugal force, and the liquid finally converged is in gravitational field
Under the action of flowed out from liquid outlet, be collected in product storage tank, by ageing, after alcohol washes, filters, it is ultra-fine that LITHIUM BATTERY can be obtained
Carbonic acid powder for lithium.
To guarantee the effect of hypergravity process intensification, hypergravity Acceleration Control is 50-4000m/s2, preferably 200-
4000m/s2。
On the basis of hypergravity process intensification, reaction crystallization process optimal control is the pass of ultra-fine carbonic acid powder for lithium preparation
One of key.The preparation of the ultra-fine lithium carbonate of LITHIUM BATTERY with high brine containing lithium and sodium carbonate liquor (200-400g/L) for raw material, for guarantor
Product size size and its homogeneity are demonstrate,proved, the lithium concentration of raw brine requires to be 1-50g/L, preferably 5-30g/L.
To guarantee the sufficient precipitation and separation of lithium ion, aqueous sodium carbonate is excessively added, specifically, sodium carbonate and lithium from
Son is by the synchronous addition of reaction molar ratio 0.5-0.7.
Further, the charging rate control of aqueous salt brine is 100-500ml/min.
The control of crystal grain digestion time is 3-8h after reactive crystallization, to promote product size homogeneity.
The present invention also provides a kind of hypergravity preparation systems of the ultra-fine lithium carbonate of LITHIUM BATTERY, and it is molten that the system comprises sodium carbonate
Liquid storage tank 1 and brine storage tank 2, the sodium carbonate liquor storage tank 1 and brine storage tank 2 by pump accordingly respectively with percussion flow-rotation
The solution inlet 4 and aqueous salt brine entrance 5 for turning packed bed supergravity reactor connect, and Impinging Stream-Rotating Packed Bed hypergravity is anti-
The products export 7 of device is answered to connect with product storage tank 9.
Further, the Impinging Stream-Rotating Packed Bed supergravity reactor includes liquid distribution trough, in the liquid distribution
Filler turntable is set in device, central axis is set among the liquid distribution trough, and the central axis is connect with rotating electric machine, in
Feed(raw material)inlet is nearby arranged in mandrel, and products export is arranged in filler turntable outer side edges.
Compared with prior art, the positive effect of the present invention is:
The hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY is proposed the present invention is based on Impinging Stream-Rotating Packed Bed and is
System strengthens the microcosmic mixing and peptizaiton of reaction mass, association reaction by the hypergravity effect of Impinging Stream-Rotating Packed Bed
Crystallization process Optimized-control Technique realizes continous way production preparation and the carbonic acid crystalline lithium ruler of the ultra-fine carbonic acid powder for lithium of LITHIUM BATTERY
Very little Effective Regulation.
Detailed description of the invention
Fig. 1 is the ultra-fine carbonic acid powder for lithium preparation facilities schematic diagram of LITHIUM BATTERY；
Wherein: 1- sodium carbonate liquor storage tank, 2- brine storage tank, 3- pump, 4- solution inlet, 5- aqueous salt brine entrance, 6- liquid
Body distributor, 7- products export, 8- filler, 9- product storage tank, 10- motor.
Fig. 2 is Impinging Stream-Rotating Packed Bed supergravity reactor schematic diagram.
Specific embodiment
A kind of specific embodiment of the ultra-fine lithium carbonate hypergravity preparation method of LITHIUM BATTERY of the present invention presented below.
Embodiment 1
Attached drawing 1 is referred to, the hypergravity preparation process device of the ultra-fine lithium carbonate of LITHIUM BATTERY mainly includes raw material storage tank, product
Storage tank and Impinging Stream-Rotating Packed Bed supergravity reactor, wherein the specific device principle of supergravity reactor is then such as 2 institute of attached drawing
Show, main body includes liquid distribution trough, filler turntable and rotating electric machine, and feed(raw material)inlet is arranged near spindle central, turntable
Products export is arranged in outer side edges.Specifically, concentration prewired first is the sodium carbonate liquor of 280mg/L and lithium concentration is
The old brine of 25g/L is stored respectively to respective raw material storage tank, opens charge pump, adds halogen with the charging rate of 250mL/min
Aqueous solution adds sodium carbonate liquor in excessive 1.1 times of the ratio of reaction molar ratio, meanwhile, start supergravity reactor, adjusts and turn
Disk rotating speed, adults power acceleration are 2000m/s2.Under motor drive, the acceleration of gravity that turntable high speed rotation generates makes
Distributor charging is obtained by dispersion tearing into nanometer or micron-sized droplet, huge phase interface is generated, is greatly promoted
The microcosmic mixing of material and mass transport process promote to form ultra-fine carbonic acid crystalline lithium to generate invigoration effect to reaction crystallization process
Particle.Scattered material is impinged upon on reactor wall after radial throw away under the influence of centrifugal force, the liquid finally converged
Body flows out under the action of gravitational field from liquid outlet, is collected in product storage tank, further increases by 6 hours A-si seasoning effects
The ultra-fine carbonic acid powder for lithium of LITHIUM BATTERY can be obtained after washing filter in crystal grain size homogeneity, alcohol.The above process is practical to be prepared
Carbonic acid powder for lithium is having a size of d10=1.394 μm, d50=4.709 μm, d90=9.825 μm, index has reached China national row
Particle size requirements of the industry standard to battery-level lithium carbonate.
Embodiment 2
Attached drawing 1 is referred to, the hypergravity preparation process device of the ultra-fine lithium carbonate of LITHIUM BATTERY mainly includes raw material storage tank, product
Storage tank and Impinging Stream-Rotating Packed Bed supergravity reactor, wherein the specific device principle of supergravity reactor is then such as 2 institute of attached drawing
Show, main body includes liquid distribution trough, filler turntable and rotating electric machine, and feed(raw material)inlet is arranged near spindle central, turntable
Products export is arranged in outer side edges.Specifically, concentration prewired first is the sodium carbonate liquor of 280mg/L and lithium concentration is
The old brine of 25g/L is stored respectively to respective raw material storage tank, opens charge pump, adds halogen with the charging rate of 250mL/min
Aqueous solution adds sodium carbonate liquor in excessive 1.1 times of the ratio of reaction molar ratio, meanwhile, start supergravity reactor, adjusts and turn
Disk rotating speed, adults power acceleration are 2000m/s2.Under motor drive, the acceleration of gravity that turntable high speed rotation generates makes
Distributor charging is obtained by dispersion tearing into nanometer or micron-sized droplet, huge phase interface is generated, is greatly promoted
The microcosmic mixing of material and mass transport process promote to form ultra-fine carbonic acid crystalline lithium to generate invigoration effect to reaction crystallization process
Particle.Scattered material is impinged upon on reactor wall after radial throw away under the influence of centrifugal force, the liquid finally converged
Body flows out under the action of gravitational field from liquid outlet, is collected in product storage tank, further increases by 3 hours A-si seasoning effects
The ultra-fine carbonic acid powder for lithium of LITHIUM BATTERY can be obtained after washing filter in crystal grain size homogeneity, alcohol.The above process is practical to be prepared
Carbonic acid powder for lithium is having a size of d10=2.163 μm, d50=7.422 μm, d90=16.404 μm.
Embodiment 3
Attached drawing 1 is referred to, the hypergravity preparation process device of the ultra-fine lithium carbonate of LITHIUM BATTERY mainly includes raw material storage tank, product
Storage tank and Impinging Stream-Rotating Packed Bed supergravity reactor, wherein the specific device principle of supergravity reactor is then such as 2 institute of attached drawing
Show, main body includes liquid distribution trough, filler turntable and rotating electric machine, and feed(raw material)inlet is arranged near spindle central, turntable
Products export is arranged in outer side edges.Specifically, concentration prewired first is the sodium carbonate liquor of 280mg/L and lithium concentration is
The old brine of 25g/L is stored respectively to respective raw material storage tank, opens charge pump, adds halogen with the charging rate of 100mL/min
Aqueous solution adds sodium carbonate liquor in excessive 1.1 times of the ratio of reaction molar ratio, meanwhile, start supergravity reactor, adjusts and turn
Disk rotating speed, adults power acceleration are 2000m/s2.Under motor drive, the acceleration of gravity that turntable high speed rotation generates makes
Distributor charging is obtained by dispersion tearing into nanometer or micron-sized droplet, huge phase interface is generated, is greatly promoted
The microcosmic mixing of material and mass transport process promote to form ultra-fine carbonic acid crystalline lithium to generate invigoration effect to reaction crystallization process
Particle.Scattered material is impinged upon on reactor wall after radial throw away under the influence of centrifugal force, the liquid finally converged
Body flows out under the action of gravitational field from liquid outlet, is collected in product storage tank, and it is ultra-fine that LITHIUM BATTERY can be obtained after the washed filter of alcohol
Carbonic acid powder for lithium.The above process practical carbonic acid powder for lithium prepared is having a size of d10=3.934 μm, d50=9.334 μm, d90=
18.654μm。
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, without departing from the inventive concept of the premise, can also make several improvements and modifications, these improvements and modifications also should be regarded as
In protection scope of the present invention.
Claims (10)
1. a kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY is mainly acted on by hypergravity and strengthens reaction mass
Mixing and dispersion, and then prepare the ultra-fine carbonic acid powder for lithium of LITHIUM BATTERY, which is characterized in that hypergravity main equipment uses percussion flow-
Rotary packed bed device form.
2. a kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY as described in claim 1, which is characterized in that LITHIUM BATTERY
Ultra-fine lithium carbonate preparation starts supergravity reactor, adjusts rotary speed using high brine containing lithium and aqueous sodium carbonate as raw material,
Adults power acceleration；Scattered material is impinged upon on reactor wall after radial throw away under the influence of centrifugal force,
The liquid finally converged flows out under the action of gravitational field from liquid outlet, is collected in product storage tank, washes by ageing, alcohol, mistake
After filter, the ultra-fine carbonic acid powder for lithium of LITHIUM BATTERY can be obtained.
3. a kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY as claimed in claim 2, which is characterized in that the height
Lithium concentration in brine containing lithium is 1-50g/L, aqueous sodium carbonate 200-400g/L.
4. a kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY as claimed in claim 2, which is characterized in that the height
Lithium concentration in brine containing lithium is 5-30g/L.
5. a kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY as claimed in claim 2, which is characterized in that sodium carbonate
It is 0.5-0.7 with lithium ion molar reactive ratio.
6. a kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY as claimed in claim 2, which is characterized in that described super
Acceleration of gravity is 50-4000m/s2。
7. a kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY as claimed in claim 2, which is characterized in that brine is molten
The charging rate control of liquid is 100-500ml/min.
8. a kind of hypergravity preparation method of the ultra-fine lithium carbonate of LITHIUM BATTERY as described in claim 1, which is characterized in that reaction knot
Crystal grain digestion time is 3-8h after crystalline substance, to improve powder dimensional homogeneity.
9. a kind of hypergravity preparation system of the ultra-fine lithium carbonate of LITHIUM BATTERY, which is characterized in that the system comprises sodium carbonate liquors
Storage tank (1) and brine storage tank (2), the sodium carbonate liquor storage tank (1) and brine storage tank (2) by pump accordingly respectively with shock
Stream-rotary packed bed supergravity reactor solution inlet (4) and aqueous salt brine entrance (5) connection, Impinging Stream-Rotating Packed Bed
The products export (7) of supergravity reactor is connect with product storage tank (9).
10. a kind of hypergravity preparation system of the ultra-fine lithium carbonate of LITHIUM BATTERY as claimed in claim 9, which is characterized in that described to hit
Hitting stream-rotary packed bed supergravity reactor includes liquid distribution trough, filler turntable is arranged in the liquid distribution trough, in institute
It states and central axis is set among liquid distribution trough, the central axis is connect with rotating electric machine, feed(raw material)inlet is set near central axis,
Products export is arranged in filler turntable outer side edges.
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| CN111252787A (en) * | 2020-03-19 | 2020-06-09 | 北京化工大学 | Method for preparing battery-grade lithium carbonate by using micro-liquid membrane reactor |
| CN115432718A (en) * | 2022-11-08 | 2022-12-06 | 浙江钠创新能源有限公司 | Hypergravity synthesis method and application of prussian blue material |
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| CN108356276A (en) * | 2018-02-02 | 2018-08-03 | 中北大学 | A kind of the hypergravity preparation method and device of cellulose modified nano zero valence iron |
| CN108793204A (en) * | 2018-08-24 | 2018-11-13 | 中国科学院青海盐湖研究所 | A kind of feed liquid containing lithium prepares the method and system of lithium carbonate |
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| CN102180488A (en) * | 2010-04-09 | 2011-09-14 | 清华大学 | Method for preparing nano lithium carbonate |
| CN108356276A (en) * | 2018-02-02 | 2018-08-03 | 中北大学 | A kind of the hypergravity preparation method and device of cellulose modified nano zero valence iron |
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Cited By (2)
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| CN111252787A (en) * | 2020-03-19 | 2020-06-09 | 北京化工大学 | Method for preparing battery-grade lithium carbonate by using micro-liquid membrane reactor |
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