CN114377641A - Continuous lithium-precipitating reaction kettle - Google Patents
Continuous lithium-precipitating reaction kettle Download PDFInfo
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- CN114377641A CN114377641A CN202111667001.8A CN202111667001A CN114377641A CN 114377641 A CN114377641 A CN 114377641A CN 202111667001 A CN202111667001 A CN 202111667001A CN 114377641 A CN114377641 A CN 114377641A
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- 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
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- 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
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- 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
- B01J19/0013—Controlling the temperature of the process
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- 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
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- 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
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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
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- 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
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00027—Process aspects
- B01J2219/00033—Continuous processes
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00054—Controlling or regulating the heat exchange system
- B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
- B01J2219/00058—Temperature measurement
- B01J2219/00063—Temperature measurement of the reactants
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
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Abstract
The invention provides a continuous lithium precipitation reaction kettle. It sinks lithium reation kettle body, locates to sink including the thickening lithium reation kettle body, the thickening sinks lithium sulfate solution elevated tank and the soda solution elevated tank of lithium reation kettle body top, accept in this internal inner tube of lithium reation kettle and distributing device are sunk in the thickening, and locate the thickening sinks thermometer on the lithium reation kettle body, this internal (mixing) shaft that is equipped with of lithium reation kettle is sunk in the thickening. The continuous lithium precipitation reaction kettle provided by the invention has the advantages that the production efficiency of equipment is increased, the equipment investment is reduced, the two-stage thickening design is adopted, the equipment load of the rear working section is reduced, the production efficiency of the rear working section is improved, the reverse blade delays the precipitation of crystals, the crystal granularity is increased, the subsequent centrifugal separation is facilitated, the multi-stage distributor is more uniform in adding of a lithium sulfate solution, the coating of the crystals produced by reaction on the lithium sulfate is reduced, the sulfuric acid heel content in the product is reduced, and the product quality is improved.
Description
Technical Field
The invention relates to a continuous lithium precipitation reaction kettle.
Background
In recent years, with the rapid development of lithium power batteries, especially with the increase of the application market of lithium iron phosphate, the demand for lithium carbonate is rapidly increased at home and abroad, and the production scale of lithium salts at home is rapidly expanded in recent years. At present, the lithium extraction process in the industry mainly comprises two processes of extracting lithium from salt lakes and extracting lithium from ores. With the maturity of the ore lithium extraction technology, the spodumene-sulfuric acid method is widely used in the industrial production of lithium carbonate, firstly, spodumene (with the content of Li2O being 4.0-7.5%) concentrate is crushed, then is roasted at high temperature in a rotary kiln to generate beta-spodumene, is cooled and ball-milled until the particle size is about 0.1mm, then is mixed with sufficient sulfuric acid and is sent into an acidification rotary furnace for sulfation roasting, after a roasted product is leached in a stirring tank, lime milk is introduced to adjust the pH value of the dissolved and discharged material to remove impurities, and then sodium carbonate is used for further removing calcium and magnesium, so that a pure lithium sulfate solution is obtained. The lithium sulfate solution is further concentrated and then reacts with a sodium carbonate solution to generate lithium deposition reaction to generate lithium carbonate crystals. Because the concentration, the adding sequence, the adding amount, the reaction temperature, the reaction time, the stirring speed and the like of the lithium sulfate solution and the sodium carbonate solution have strict requirements in the reaction process, the parameters need to be accurately controlled. The volume of a single reaction kettle for depositing lithium is limited, a large-scale lithium carbonate production line usually needs a plurality of reaction kettles to be alternately operated at the same time, the lithium deposition reaction is carried out intermittently, the feeding amount, the temperature and the discharging are automatically controlled, but the operation precision is low, so that the quality of lithium carbonate obtained by depositing lithium is greatly different.
In the existing process for producing lithium carbonate by spodumene at home and abroad, a lithium sulfate solution is leached out by mixing pulp with washing water after transformation roasting and acidification roasting of spodumene, the leaching solution is subjected to multi-step impurity removal to obtain a sulfuric acid solution, and the sulfuric acid solution is concentrated and then sent to a subsequent lithium precipitation process for use.
Pumping the lithium sulfate solution and the soda solution into a lithium precipitation tank according to a certain proportion and a certain flow rate for reaction to generate lithium carbonate slurry. At present, batch production is mostly adopted in the lithium precipitation process at home and abroad, and the process is repeated after discharging and cleaning are carried out once a kettle is reacted. Also have domesticly to adopt the heavy lithium reation kettle of continuous type, this kind of heavy lithium groove in succession includes through material connection's heavy lithium groove and crosses the silo, wherein, heavy lithium groove includes A groove and B groove through the baffle separation, is provided with two openings about being provided with on the baffle, A groove, B groove and cross the inslot and all be provided with the agitator, heavy lithium reaction is at first sent into A groove with pure alkali solution, through steam heating, open the stirring, then add the heavy lithium of concentrated lithium sulfate purifying liquid.
In the production of preparing battery-grade lithium carbonate by a spodumene-sulfuric acid method, the lithium deposition process is intermittent. Adding soda solution into the lithium precipitation kettle, heating, finishing feeding when the cumulative flow of the single kettle feeding reaches a set value, and starting heating. And (3) when the temperature of the soda solution rises to 90-95 ℃, adjusting the stirring rotation speed to 100-170 rpm, starting feeding the lithium sulfate solution, and finishing feeding when the cumulative flow of the single kettle reaches a set value. After the feeding of the lithium sulfate solution is finished, the stirring speed is adjusted after the reaction is carried out for 5-30 minutes, the discharging is started, and the batching of the next period is started after the discharging is finished.
The intermittent lithium deposition process has the following disadvantages: 1. the single lithium deposition reaction kettle is limited by the volume, and the production efficiency is lower. 2. When the reaction kettle discharges materials, because the reaction kettle is kept warm at a higher temperature all the time, when the liquid level of the discharged materials is reduced, the wall of the reaction kettle and the stirring shaft are easy to scale and need to be cleaned frequently. 3. Due to the inconsistent reaction time of lithium precipitation, part of lithium carbonate crystals are extremely small, which is not beneficial to subsequent centrifugal separation. 4. Excessive sodium carbonate is not easy to maintain in the lithium precipitation reaction, so that the sulfate radical of the impurity exceeds the standard. 5. The lithium carbonate crystal slurry generated in the whole lithium deposition reaction has low concentration, and the load of subsequent centrifugal separation is increased.
Disclosure of Invention
Based on this, the invention provides a continuous lithium precipitation reaction kettle.
The invention relates to a continuous lithium precipitation reaction kettle, which comprises a thickening lithium precipitation reaction kettle body, a lithium sulfate solution high-level tank body and a soda solution high-level tank body which are arranged above the thickening lithium precipitation reaction kettle body, an inner cylinder and a distributor which are accommodated in the thickening lithium precipitation reaction kettle body, and a thermometer arranged on the thickening lithium precipitation reaction kettle body, wherein a stirring shaft is arranged in the thickening lithium precipitation reaction kettle body, the upper end of the stirring shaft is provided with a stirring machine, the stirring machine is positioned outside, the stirring shaft is provided with a reverse paddle blade, a horizontal paddle blade and a forward paddle blade, and the reverse paddle blade, the horizontal paddle blade and the forward paddle blade are all positioned at the bottom of the thickening lithium precipitation reaction kettle body.
Furthermore, an outlet, a condensed water outlet and a clear liquid outlet which are communicated with the outside are formed at the lower end of the thickening lithium precipitation reaction kettle body.
Further, the lower end of the thickening lithium-precipitating reaction kettle body is connected with a thickener, and the thickener is connected with the thickening lithium-precipitating reaction kettle body through a pipeline.
Furthermore, an overflow port communicated with the outside is arranged above the side part of the inner barrel, a steam regulating valve is arranged above the side part of the thickening lithium-precipitating reaction kettle body, and a steam inlet is formed in the steam regulating valve.
Furthermore, the reverse paddle, the horizontal paddle and the forward paddle are sequentially arranged from top to bottom along the axial direction of the stirring shaft.
Further, the height H of the thickening lithium precipitation reaction kettle body is 1-50 m, and the height difference H between the lithium sulfate solution high-level tank body and the soda solution high-level tank body and the thickening lithium precipitation reaction kettle body is 3-20 m.
Further, the distributor is 2-8 sections.
Further, the gap between the inner cylinder and the thickening lithium deposition reaction kettle body is 50-500 mm.
According to the continuous lithium precipitation reaction kettle, firstly, continuous feeding and discharging are carried out, so that the production efficiency of a single device is greatly increased, and the continuous operation of production is kept; secondly, a multi-section distributor of the lithium sulfate concentrated solution solves the problem of uniform addition of the lithium sulfate concentrated solution and reduces the problem of lithium sulfate coating by lithium carbonate crystals; in addition, in the process of continuously precipitating lithium, the liquid level in the reaction kettle is kept unchanged, so that the scaling problem of the reaction kettle and the stirring shaft is greatly reduced; thirdly, a certain granularity of lithium carbonate crystals is ensured, and the problem that fine particles are not beneficial to centrifugal separation is solved; and two-stage thickening is designed at the final discharge end, so that the concentration of the lithium carbonate crystal slurry is greatly increased, and the load of a centrifugal machine during centrifugal separation of the lithium carbonate slurry is reduced.
According to the continuous lithium precipitation reaction kettle, the continuous lithium precipitation process of the scheme is adopted, the production efficiency of equipment is increased, and the equipment investment is reduced. And a two-stage thickening design is adopted, so that the equipment load of the rear working section is reduced, and the production efficiency of the rear working section is improved. The reverse blade retards the sedimentation of the crystal, increases the granularity of the crystal and is beneficial to the subsequent centrifugal separation. The multi-section distributor enables the lithium sulfate solution to be added more uniformly, reduces the coating of the crystals produced by reaction on the lithium sulfate, reduces the content of sulfuric acid in the product and improves the product quality.
Drawings
Fig. 1 is a schematic structural diagram of a continuous lithium precipitation reaction kettle of the invention.
Description of reference numerals:
the device comprises a lithium sulfate solution elevated tank body 1, a soda solution elevated tank body 2, a stirrer 3, a thermometer 4, a thickening lithium precipitation reaction kettle body 5, a stirring shaft 6, a reverse paddle 7, a horizontal paddle 8, a forward paddle 9, an outlet 10, a condensed water outlet 11, an overflow port 12, an inner cylinder 13, a distributor 14, a thickener 15, a clear liquid discharge port 16, a steam regulating valve 17 and a steam inlet 18.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Referring to fig. 1, the invention provides a continuous lithium precipitating reaction kettle, which comprises a thickening lithium precipitating reaction kettle body 5, a lithium sulfate solution elevated tank body 1 and a soda solution elevated tank body 2 which are arranged above the thickening lithium precipitating reaction kettle body, an inner tank 13 and a distributor 14 which are accommodated in the thickening lithium precipitating reaction kettle body, and a thermometer 4 which is arranged on the thickening lithium precipitating reaction kettle body, wherein a stirring shaft 6 is arranged in the thickening lithium precipitating reaction kettle body, a stirrer 3 is arranged at the upper end of the stirring shaft, the stirrer is positioned outside, a reverse paddle 7, a horizontal paddle 8 and a forward paddle 9 are arranged on the stirring shaft, and the reverse paddle, the horizontal paddle and the forward paddle are all positioned at the bottom of the thickening lithium precipitating reaction kettle body.
In one embodiment, the lower end of the thickening lithium deposition reaction kettle body is provided with an outlet 10 communicated with the outside, a condensed water outlet 11 and a clear liquid discharge port 16.
In one embodiment, the thickening and lithium precipitating reaction kettle body is connected with a thickener 15 at the lower end, and the thickener is connected with the thickening and lithium precipitating reaction kettle body through a pipeline.
In one embodiment, an overflow port 12 communicated with the outside is arranged above the side part of the inner cylinder, a steam regulating valve 17 is arranged above the side part of the thickening lithium-precipitating reaction kettle body, and a steam inlet 18 is arranged on the steam regulating valve.
In one embodiment, the reverse blade, the horizontal blade and the forward blade are sequentially arranged from top to bottom along the axial direction of the stirring shaft.
The lithium sulfate solution high-level tank body is connected with a multi-section distributor through a pipeline, the lithium sulfate solution enters the distributor through the pipeline, and the solution is uniformly dispersed to a lower inner cylinder reaction area through the distributor. The sodium carbonate solution is extended into the inner cylinder through a pipeline, and the discharge port is positioned at the position 1/4 on the inner cylinder. The stirring shaft is positioned in the middle of the reaction kettle, three blades are distributed on the shaft, the reverse blade enables the fluid to face upwards, and the forward blade enables the fluid to face downwards. The inner cylinder and the outer cylinder have a certain gap, and the lower part has a clear liquid outlet. The magma enters the thickener through the pipeline after being thickened at the bottom of the inner cylinder. Thickening by a thickener and then entering the next working procedure.
The lithium sulfate solution elevated tank and the sodium carbonate solution elevated tank are designed to uniformly add the solution participating in the reaction, so that the stable proportion of the materials is ensured in the reaction; the multi-section distributor is used, so that the lithium sulfate solution is added more uniformly, the lithium sulfate coating is reduced, and the product quality is improved; the use of the blades in the reverse, horizontal and forward directions prolongs the growth time of the crystal and also plays a role in concentrating the crystal at the bottom; an inner cylinder design is used, so that the crystal mush and the clear liquid are shunted; the thermometer is interlocked with the steam control valve to ensure the stable reaction temperature in the reaction kettle; the secondary thickener further concentrates the crystal mush, reduces the load of subsequent procedures and increases the productivity in unit time; the advantages can effectively improve the efficiency of the lithium deposition reaction and the subsequent production and better control the product quality.
In one embodiment, the height difference h between the high-level tank for the lithium sulfate solution and the high-level tank for the sodium carbonate solution and the thickening and lithium-precipitating reaction kettle body is 3-20 m.
In one embodiment, the distributor is in 2-8 sections.
In one embodiment, the height H of the thickening lithium-precipitating reaction kettle body is 1-50 meters.
In one embodiment, the lithium precipitation reaction temperature is in the range of 70-98 ℃.
In one embodiment, the clearance between the inner cylinder and the thickening lithium deposition reaction kettle body is 50mm-500 mm.
In one embodiment, the outer wall of the reactor has a clear liquid overflow port located at 1/6-1/5 from the top of the reactor.
In one embodiment, the outlet of the lithium precipitation reaction kettle is connected with a thickener.
According to the continuous lithium precipitation reaction kettle, firstly, continuous feeding and discharging are carried out, so that the production efficiency of a single device is greatly increased, and the continuous operation of production is kept; secondly, a multi-section distributor of the lithium sulfate concentrated solution solves the problem of uniform addition of the lithium sulfate concentrated solution and reduces the problem of lithium sulfate coating by lithium carbonate crystals; in addition, in the process of continuously precipitating lithium, the liquid level in the reaction kettle is kept unchanged, so that the scaling problem of the reaction kettle and the stirring shaft is greatly reduced; thirdly, a certain granularity of lithium carbonate crystals is ensured, and the problem that fine particles are not beneficial to centrifugal separation is solved; and two-stage thickening is designed at the final discharge end, so that the concentration of the lithium carbonate crystal slurry is greatly increased, and the load of a centrifugal machine during centrifugal separation of the lithium carbonate slurry is reduced.
According to the continuous lithium precipitation reaction kettle, the continuous lithium precipitation process of the scheme is adopted, the production efficiency of equipment is increased, and the equipment investment is reduced. And a two-stage thickening design is adopted, so that the equipment load of the rear working section is reduced, and the production efficiency of the rear working section is improved. The reverse blade retards the sedimentation of the crystal, increases the granularity of the crystal and is beneficial to the subsequent centrifugal separation. The multi-section distributor enables the lithium sulfate solution to be added more uniformly, reduces the coating of the crystals produced by reaction on the lithium sulfate, reduces the content of sulfuric acid in the product and improves the product quality.
The above examples only express embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. A continuous lithium precipitation reaction kettle is characterized in that: sink lithium reation kettle body, locate including the thickening lithium sulfate solution elevated tank and the soda solution elevated tank of lithium reation kettle body top are sunk in the thickening, accept in this internal inner tube of lithium reation kettle and distributing device are sunk in the thickening, and locate thermometer on the thickening lithium reation kettle body is sunk in the thickening, this internal (mixing) shaft that is equipped with of lithium reation kettle is sunk in the thickening, the upper end of (mixing) shaft is equipped with the mixer, the mixer is located the external world, be equipped with reverse paddle leaf, horizontal paddle leaf and forward paddle leaf on the (mixing) shaft, reverse paddle leaf horizontal paddle leaf and forward paddle leaf all is located the bottom of lithium reation kettle body is sunk in the thickening.
2. The continuous lithium deposition reaction vessel of claim 1, wherein: the lower end of the thickening lithium precipitation reaction kettle body is provided with an outlet, a condensed water outlet and a clear liquid outlet which are communicated with the outside.
3. The continuous lithium deposition reaction vessel of claim 2, wherein: the lower end of the thickening lithium-precipitating reaction kettle body is connected with a thickener, and the thickener is connected with the thickening lithium-precipitating reaction kettle body through a pipeline.
4. The continuous lithium deposition reaction vessel of claim 3, wherein: an overflow port communicated with the outside is arranged above the side part of the inner barrel, a steam regulating valve is arranged above the side part of the thickening lithium precipitation reaction kettle body, and a steam inlet is formed in the steam regulating valve.
5. The continuous lithium deposition reaction vessel of claim 4, wherein: the reverse paddle, the horizontal paddle and the forward paddle are sequentially arranged from top to bottom along the axial direction of the stirring shaft.
6. The continuous lithium deposition reaction vessel of claim 5, wherein: the height H of the thickening lithium precipitation reaction kettle body is 1-50 m, and the height difference H between the lithium sulfate solution high-level tank body and the soda solution high-level tank body and the thickening lithium precipitation reaction kettle body is 3-20 m.
7. The continuous lithium deposition reaction vessel of claim 6, wherein: the distributing device is 2-8 sections.
8. The continuous lithium deposition reaction vessel of claim 7, wherein: the clearance between the inner cylinder and the thickening lithium-precipitating reaction kettle body is 50mm-500 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111667001.8A CN114377641A (en) | 2021-12-31 | 2021-12-31 | Continuous lithium-precipitating reaction kettle |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111667001.8A CN114377641A (en) | 2021-12-31 | 2021-12-31 | Continuous lithium-precipitating reaction kettle |
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| CN114377641A true CN114377641A (en) | 2022-04-22 |
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| CN202111667001.8A Pending CN114377641A (en) | 2021-12-31 | 2021-12-31 | Continuous lithium-precipitating reaction kettle |
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- 2021-12-31 CN CN202111667001.8A patent/CN114377641A/en active Pending
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