CN211688287U - Lithium hydroxide monohydrate crystallization separation purification device - Google Patents
Lithium hydroxide monohydrate crystallization separation purification device Download PDFInfo
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- CN211688287U CN211688287U CN201921299192.5U CN201921299192U CN211688287U CN 211688287 U CN211688287 U CN 211688287U CN 201921299192 U CN201921299192 U CN 201921299192U CN 211688287 U CN211688287 U CN 211688287U
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Abstract
A lithium hydroxide monohydrate crystal separation and purification device comprises a washing machine shell, wherein a telescopic motor and a rotating motor are installed on the washing machine shell, and a stirring scraper is connected below the telescopic motor through a telescopic rod; a filter disc and an ultrasonic generator are arranged in a washing machine shell, and a discharging oil cylinder is fixedly connected to the surface of the washing machine shell; a first filtrate tank and a second filtrate tank are connected to the lower part of the shell of the washing machine, and the outlet end of the second filtrate tank is connected with a washing water tank; the outlet end of the washing water tank is connected with a washing liquid feeding pipe, and the other end of the washing liquid feeding pipe is connected with a spraying device. The utility model overcomes the defects of the prior art, and realizes the separation of other soluble impurities by utilizing the difference of the solubility of the lithium hydroxide; the crystal hardening form is destroyed by stirring in the filtering process, and a spray washing process and an ultrasonic wave cavitation effect are matched, so that the free water wrapped in the crystal and the dissolved impurities are removed in the filtering process, and the aim of purifying the lithium hydroxide is fulfilled.
Description
Technical Field
The utility model relates to a chemicals purification technical field, concretely relates to lithium hydroxide monohydrate crystallization separation purification device.
Background
With the widespread use of lithium and lithium salts and the continuous development of high and new technologies, "lithium" is transformed from industrial metals to "energy metals that promote world progress". The demand of the international market for lithium products is continuously increasing, the demand is increased at a speed of 7-11% per year on average, and high-purity lithium hydroxide is a main source of lithium ions in products of national defense, electronics, energy and aviation technologies.
The existing purification treatment of lithium hydroxide mainly comprises the processes of separation by a centrifuge, washing, plate-frame filter pressing, filter cake washing, multiple washing and excessive washing water consumption, so that the energy consumption of a concentration unit is large, the operation cost is increased, process equipment does not have an air isolation condition, oxygen and carbon dioxide in the air are in contact with lithium hydroxide to release reaction in the dehydration process, and in the centrifugation or filter pressing dehydration process, impurity ions dissolved in water contained in a filter material are wrapped by crystals and are not easy to remove, and the product purity is low; the granularity of the product cannot be controlled, the product is easy to agglomerate and block an equipment pipeline, the physical and chemical property change gradient of turbid liquid substances in the dehydration process caused by heat loss in operation cannot be avoided, the penetration phenomenon is serious in the centrifugal dehydration process, the discontinuous and stable operation of equipment production is caused, the filtrate contains more crystallized lithium hydroxide, the filter material is washed for multiple times, and the dehydrated lithium hydroxide monohydrate is contacted with air for multiple times, so that the operation is difficult to realize automatic operation, the production capacity is low, the investment is high, the water consumption of the washing process is high, the evaporation water quantity of a front-end concentration process is large, the energy consumption is high, the lithium yield in the reaction and production process is low, the quality is poor, the resource utilization rate is low, and the requirement of the current clean production process cannot be.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the utility model provides a lithium hydroxide monohydrate crystallization separation and purification device, which overcomes the defects of the prior art, has reasonable design and compact structure, and realizes the separation of other soluble impurities contained in a lithium hydroxide solution by utilizing the different solubility of various substances in a mixed system after the lithium hydroxide is evaporated and concentrated; the crystal hardening form is destroyed by stirring in the filtering process, and a spray washing process and an ultrasonic wave cavitation effect are matched, so that the free water wrapped in the crystal and the dissolved impurities are removed in the filtering process, and the aim of purifying the lithium hydroxide is fulfilled.
In order to achieve the above purpose, the utility model discloses a following technical scheme realizes:
a lithium hydroxide monohydrate crystal separation and purification device comprises a washing machine shell, wherein a telescopic motor and a rotating motor are fixedly mounted on the upper surface of the washing machine shell, the lower part of the telescopic motor is movably connected with one end of a telescopic rod, the other end of the telescopic rod penetrates through the surface of the washing machine shell and is fixedly connected with a stirring scraper, and the rotating motor is connected with the telescopic rod through a rotating shaft in a transmission manner; the surface of the washing machine shell is respectively provided with a seed crystal feeding hole and a raw material liquid feeding hole, a filter disc and an ultrasonic generator are fixedly arranged in an inner cavity of the washing machine shell, the surface of the washing machine shell is fixedly connected with a discharging oil cylinder, the surface of the discharging oil cylinder is provided with a discharging valve, and the lower surface of the washing machine shell is fixedly communicated with a vacuum pump through a pipeline; the lower part of the washing machine shell is fixedly connected with an inlet end of a first filtrate tank and an inlet end of a second filtrate tank through pipelines respectively, control valves are arranged on the pipelines connecting the first filtrate tank and the second filtrate tank with the washing machine shell, the outlet end of the first filtrate tank is connected with a secondary evaporation device through a first filtrate pump, and the outlet end of the second filtrate tank is connected with the inlet end of the washing water tank through a second filtrate pump; the entrance point of washing water pitcher still is connected with pure water source, the exit end of washing water pitcher passes through the one end of tube coupling washing liquid inlet pipe, and fixed mounting has a washing water pump on the pipeline, the other end of washing liquid inlet pipe passes washing machine casing fixedly connected with sprinkler.
Preferably, the lower surface of the washing machine shell is provided with a general filtering valve.
Preferably, the surface of the washing machine shell is fixedly connected with one end of a nitrogen gas inlet pipe, and the other end of the nitrogen gas inlet pipe is connected to a nitrogen supply device.
Preferably, the outer surface of the washing machine shell is coated with a jacket water-cooling pipe, a circulating water feeding port is formed above the jacket water-cooling pipe, a circulating water discharging port is formed below the jacket water-cooling pipe, the circulating water feeding port is communicated with the circulating water discharging port through a circulating water pipe, and a cooler is fixedly mounted in the middle of the circulating water pipe.
Preferably, the height of the filter disc from the bottom of the washer housing is 0.32-0.35 times the diameter of the washer housing.
Preferably, sprinkler includes collector pipe and shower nozzle, the collector pipe is linked together with the washing liquid inlet pipe, two are no less than in the shower nozzle setting, and even fixed mounting is in the collector pipe below.
The utility model provides a lithium hydroxide monohydrate crystallization separation purification device. The method has the following beneficial effects: the separation of other soluble impurities contained in the lithium hydroxide solution is realized by utilizing the different solubility of various substances in a mixed system after the lithium hydroxide is evaporated and concentrated; the crystal hardening form is destroyed by stirring in the filtering process, and a spray washing process and an ultrasonic wave cavitation effect are matched, so that the free water wrapped in the crystal and the dissolved impurities are removed in the filtering process, and the aim of purifying the lithium hydroxide is fulfilled.
Drawings
In order to more clearly illustrate the present invention or the technical solutions in the prior art, the drawings used in the description of the prior art will be briefly described below.
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the internal structure of the washing machine housing of the present invention;
the reference numbers in the figures illustrate:
1. a washer housing; 2. a telescopic motor; 3. rotating the motor; 4. a telescopic rod; 5. stirring and scraping the knife; 6. a seed crystal feeding hole; 7. a raw material liquid feeding port; 8. a filter disc; 9. an ultrasonic generator; 10. a discharging oil cylinder; 11. a discharge valve; 12. a first filtrate tank; 13. a second filtrate tank; 14. a first filtrate pump; 15. a second filtrate pump; 16. washing the water tank; 17. a source of pure water; 18. a washing liquid feeding pipe; 19. a spraying device; 20. a vacuum pump; 21. a nitrogen inlet pipe; 22. circulating the water feeding port; 23. circulating a water drainage port; 24. a water collection pipe; 25. a spray head; 26. a main filtering valve; 27. and washing the water pump.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the drawings of the present invention will be combined below to clearly and completely describe the technical solutions of the present invention.
In the first embodiment, as shown in fig. 1 to 2, a lithium hydroxide monohydrate crystallization separation and purification device includes a washing machine housing 1, a telescopic motor 2 and a rotating motor 3 are fixedly installed on the upper surface of the washing machine housing 1, one end of a telescopic rod 4 is movably connected below the telescopic motor 2, the other end of the telescopic rod 4 penetrates through the surface of the washing machine housing 1 and is fixedly connected with a stirring scraper 5, and the rotating motor 3 is connected with the telescopic rod 4 through a rotating shaft in a transmission manner; the surface of a washing machine shell 1 is respectively provided with a seed crystal feeding hole 6 and a raw material liquid feeding hole 7, a filter disc 8 and an ultrasonic generator 9 are fixedly arranged in the inner cavity of the washing machine shell 1, the surface of the washing machine shell 1 is fixedly connected with a discharging oil cylinder 10, the surface of the discharging oil cylinder 10 is provided with a discharging valve 11, and the lower surface of the washing machine shell 1 is fixedly communicated with a vacuum pump 20 through a pipeline; the lower part of the washing machine shell 1 is fixedly connected with the inlet end of a first filtrate tank 12 and the inlet end of a second filtrate tank 13 through pipelines respectively, the pipelines of the first filtrate tank 12 and the second filtrate tank 13 connected with the washing machine shell 1 are provided with control valves, the outlet end of the first filtrate tank 12 is connected with a secondary evaporation device through a first filtrate pump 14, and the outlet end of the second filtrate tank 13 is connected with the inlet end of a washing water tank 16 through a second filtrate pump 15; the inlet end of the washing water tank 16 is also connected with a pure water source 17, the outlet end of the washing water tank 16 is connected with one end of a washing liquid feeding pipe 18 through a pipeline, a washing water pump 27 is fixedly installed on the pipeline, and the other end of the washing liquid feeding pipe 18 penetrates through the shell 1 of the washing machine and is fixedly connected with a spraying device 19; the lower surface of the washing machine housing 1 is provided with a main filtering valve 26.
The working process is an intermittent separation process, each separation process comprises four steps of feeding, filtering, washing and discharging, 2500-mesh filter cloth is laid on a filter disc 8 by utilizing the granularity of 5 mu m of lithium hydroxide monohydrate crystals, so that interception of lithium hydroxide monohydrate crystals can be basically realized, the crystallized lithium hydroxide monohydrate cannot flow into a separated liquid phase through the filter cloth, and separation of other soluble impurities in a lithium hydroxide solution is realized by utilizing the difference of the solubility of various substances in a mixed system after evaporation and concentration of the lithium hydroxide;
firstly, raw material liquid is added into a washing machine shell 1 through a raw material liquid feeding hole 7, then a vacuum degree is established in a system below a filter disc 8 in the washing machine shell 1 through a vacuum pump 20, the pressure difference between the upper part and the lower part of the filter disc 8 is increased, the filtering driving force is improved, simultaneously gives electric signals to the telescopic motor 2 and the rotating motor 3, so that the telescopic motor 2 and the rotating motor 3 drive the telescopic rod 4 to move, then drives the stirring scraper 5 to rotate left and right and move up and down simultaneously, so as to realize the preliminary crystallization, separation and pretreatment of the lithium hydroxide, dissolve impurities by a large amount of soluble impurities, initially obtain a lithium hydroxide monohydrate filter cake on the filter disc 8, open the control valve connected with the inlet end of the first filtrate tank 12 at the moment, and after the impurities dissolved in the solution enter the first filtrate tank 12, then the sodium hydroxide (or other soluble substances) left after the lithium hydroxide is further concentrated and separated is sent to a secondary evaporation device by a first filtrate pump 14 and is used as a byproduct for process production; the following table 1 shows the lithium hydroxide index obtained by one filtration.
TABLE 1 lithium hydroxide index obtained by one-time filtration
| Components | LiOH.H2O | CO3 2- | K | Ca | Na | CL- | SO4 2- | Cu/Mg/Si |
| Content (wt.) | 98.4％ | 0.001％ | 0.002％ | 0.001％ | 1.4％ | 0.105％ | 0.0002％ | ND |
Then, the pure water in the washing water tank 16 is sprayed in the washing machine shell 1 through the spraying device 19 through the washing water pump 27, and simultaneously electric signals are given to the telescopic motor 2 and the rotating motor 3, so that the telescopic motor 2 and the rotating motor 3 drive the telescopic rod 4 to move, then the stirring scraper 5 is driven to rotate left and right and move up and down simultaneously, and the ultrasonic generator 9 is started simultaneously, so that the solution generates local high temperature and high pressure through the 'cavitation effect' generated by the ultrasonic generator 9, a strong shock wave is formed, the solution turbulence is accelerated, the surface of the solid lithium hydroxide is continuously washed, the mechanical vibration of the solvent water is caused, the dispersion and dissolution of the lithium hydroxide solute are accelerated, and the dissolubility and the insoluble impurities carried in the lithium hydroxide crystal hardening are dissolved in the solvent water again; in the process, seed crystal lithium hydroxide is rapidly added into the washing machine shell 1 through the seed crystal feeding hole 6, the lithium hydroxide is recrystallized by utilizing the crystallization formation mechanism of the lithium hydroxide and controlling the supersaturation degree of the solution and lowering the temperature of the system to 35 ℃, and the growth of crystal particles is promoted; opening a control valve connected with the inlet end of a second filtrate tank 13 to enable the solution with most lithium hydroxide dissolved at the bottom of a shell 1 of the washing machine after the cavitation effect to enter the second filtrate tank 13, sending the solution into a washing water tank 16 through a second filtrate pump 15 for backflow and filtration washing, adding seed crystals under the action of an ultrasonic generator 9 and cooling to recrystallize the lithium hydroxide in a supersaturated zone, and removing the free water wrapped in the crystals and the dissolved impurities in the crystals in the filtering process for the second time, thereby achieving the purpose of purifying the lithium hydroxide; after the washing is filtered for the second time, draw together sword 5 downstream to the filter disc surface through flexible motor 2 drive stirring, the rethread rotates motor 3 and drives the stirring and draw together sword 5 stirring filter cake and with the not hard up filter material of intensive dispersion, rethread nitrogen gas intake pipe 21 lets in high temperature nitrogen gas, and start vacuum pump 20, further weather filter material moisture through dry nitrogen gas, and the steam suction vacuum pump that the filter material formed cools off into water behind the vacuum pump, noncondensable gas nitrogen gas is got rid of, the filter cake of staying on filter disc 8 is under the effect of stirring scraper, be caught up to side discharge valve 11 next door gradually, open discharge valve 11, the filter cake can be through outside discharge cylinder 10 discharges, following 2 is the gained lithium hydroxide index after the secondary filtration.
TABLE 2 lithium hydroxide index obtained after the second filtration
As can be seen from the table above, the lithium hydroxide monohydrate produced by the device has high purity, large crystal particles, small pure water consumption and low production energy consumption by adopting circular washing, is more practical for the index requirements of high and new technologies such as new energy sources and the like, and has larger production capacity of monomer equipment.
In the second embodiment, based on the further improvement of the first embodiment, one end of the nitrogen inlet pipe 21 is fixedly connected to the surface of the washing machine shell 1, and the other end of the nitrogen inlet pipe 21 is connected to the nitrogen supply device. During preliminary separation pretreatment, nitrogen is introduced into the washing machine shell 1 to strengthen slurry filtration, so that the pressure in the washing machine shell 1 is gradually increased along with the filtration to ensure complete liquid filtration; after washing, nitrogen is also introduced into the shell 1 of the washing machine to increase the pressure difference between the upper and lower parts of the filter disc 8 and enhance the filtration of slurry, the pressure in the filtration washing machine is gradually increased along with the filtration, and when the pressure is increased to 0.3-0.5 MPa, the liquid is basically filtered completely.
In the third embodiment, based on the further improvement of the first embodiment, the outer surface of the washer housing 1 is coated with a jacket water-cooling pipe, a circulating water feeding port 22 is formed above the jacket water-cooling pipe, a circulating water discharging port 23 is formed below the jacket water-cooling pipe, the circulating water feeding port 22 is communicated with the circulating water discharging port 23 through a circulating water pipe, and a cooler is fixedly installed in the middle of the circulating water pipe. The cooling in the washing machine shell 1 is realized through a jacket water-cooling pipe, and the water is recycled through a circulating water pipe.
In the fourth embodiment, based on the further improvement of the first embodiment, the size of the washing machine housing 1 of the present application can be designed according to the tap density of LiOH · H2O, the solid content of the solid-liquid mixture and the density of the solid-liquid mixture, and in order to save the washing water and the steam consumption in the evaporation process, the volume and height of the filter disc of the vacuum suction filter from the bottom of the washing machine housing 1 are designed, and in this embodiment, the height of the filter disc 8 from the bottom of the washing machine housing 1 is 0.33 times of the diameter of the washing machine housing 1.
Fifth, based on the further improvement of the first embodiment, the spraying device 19 comprises a water collecting pipe 24 and spraying nozzles 25, the water collecting pipe 24 is communicated with the washing liquid feeding pipe 18, and the spraying nozzles 25 are arranged in four numbers and uniformly and fixedly arranged below the water collecting pipe 24. The four spray heads 25 are uniformly distributed on the water collecting pipe 24, so that when the washing water is sprayed, the washing water can be sprayed inside the filtering washing machine in an all-around and uniform manner, and the internal washing and material washing of the machine can be realized.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention in its corresponding aspects.
Claims (6)
1. A lithium hydroxide monohydrate crystallization separation purification device comprises a washing machine shell (1), and is characterized in that: a telescopic motor (2) and a rotating motor (3) are fixedly mounted on the upper surface of the washing machine shell (1), one end of a telescopic rod (4) is movably connected below the telescopic motor (2), the other end of the telescopic rod (4) penetrates through the surface of the washing machine shell (1) and is fixedly connected with a stirring scraper (5), and the rotating motor (3) is connected with the telescopic rod (4) through a rotating shaft in a transmission manner; the surface of the washing machine shell (1) is respectively provided with a seed crystal feeding hole (6) and a raw material liquid feeding hole (7), the inner cavity of the washing machine shell (1) is fixedly provided with a filter disc (8) and an ultrasonic generator (9), the surface of the washing machine shell (1) is fixedly connected with a discharging oil cylinder (10), the surface of the discharging oil cylinder (10) is provided with a discharging valve (11), and the lower surface of the washing machine shell (1) is fixedly communicated with a vacuum pump (20) through a pipeline;
the lower part of the washing machine shell (1) is fixedly connected with an inlet end of a first filtrate tank (12) and an inlet end of a second filtrate tank (13) through pipelines respectively, control valves are arranged on pipelines connecting the first filtrate tank (12) and the second filtrate tank (13) with the washing machine shell (1), an outlet end of the first filtrate tank (12) is connected with a secondary evaporation device through a first filtrate pump (14), and an outlet end of the second filtrate tank (13) is connected with an inlet end of a washing water tank (16) through a second filtrate pump (15);
the entrance point of washing water tank (16) still is connected with pure water source (17), the exit end of washing water tank (16) passes through the one end of tube coupling washing liquid inlet pipe (18), and fixed mounting has washing water pump (27) on the pipeline, the other end of washing liquid inlet pipe (18) passes washing machine casing (1) fixedly connected with sprinkler (19).
2. The lithium hydroxide monohydrate crystallization separation and purification device according to claim 1, characterized in that: the lower surface of the washing machine shell (1) is provided with a main filtering valve (26).
3. The lithium hydroxide monohydrate crystallization separation and purification device according to claim 1, characterized in that: the surface of the washing machine shell (1) is fixedly connected with one end of a nitrogen inlet pipe (21), and the other end of the nitrogen inlet pipe (21) is connected to a nitrogen supply device.
4. The lithium hydroxide monohydrate crystallization separation and purification device according to claim 1, characterized in that: the washing machine is characterized in that a jacket water-cooling pipe is coated on the outer surface of the washing machine shell (1), a circulating water feeding port (22) is formed in the upper portion of the jacket water-cooling pipe, a circulating water discharging port (23) is formed in the lower portion of the jacket water-cooling pipe, the circulating water feeding port (22) is communicated with the circulating water discharging port (23) through a circulating water pipe, and a cooler is fixedly mounted in the middle of the circulating water pipe.
5. The lithium hydroxide monohydrate crystallization separation and purification device according to claim 1, characterized in that: the height of the filter disc (8) from the bottom of the washing machine shell (1) is 0.32-0.35 times of the diameter of the washing machine shell (1).
6. The lithium hydroxide monohydrate crystallization separation and purification device according to claim 1, characterized in that: sprinkler (19) include collector pipe (24) and shower nozzle (25), collector pipe (24) are linked together with washing liquid inlet pipe (18), shower nozzle (25) set up to be no less than two, and even fixed mounting is in collector pipe (24) below.
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| CN201921299192.5U CN211688287U (en) | 2019-08-12 | 2019-08-12 | Lithium hydroxide monohydrate crystallization separation purification device |
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| CN201921299192.5U CN211688287U (en) | 2019-08-12 | 2019-08-12 | Lithium hydroxide monohydrate crystallization separation purification device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112279279A (en) * | 2020-10-26 | 2021-01-29 | 荆门市格林美新材料有限公司 | Preparation method of battery-grade lithium hydroxide monohydrate |
| CN112755944A (en) * | 2020-12-26 | 2021-05-07 | 河南省大潮炭能科技有限公司 | Super-capacitor carbon filtering and washing device and using method thereof |
| CN114773362A (en) * | 2022-06-15 | 2022-07-22 | 上海欣峰制药有限公司 | Cefoxitin sodium compound and preparation method thereof |
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2019
- 2019-08-12 CN CN201921299192.5U patent/CN211688287U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112279279A (en) * | 2020-10-26 | 2021-01-29 | 荆门市格林美新材料有限公司 | Preparation method of battery-grade lithium hydroxide monohydrate |
| CN112279279B (en) * | 2020-10-26 | 2023-05-12 | 荆门市格林美新材料有限公司 | Preparation method of battery grade lithium hydroxide monohydrate |
| CN112755944A (en) * | 2020-12-26 | 2021-05-07 | 河南省大潮炭能科技有限公司 | Super-capacitor carbon filtering and washing device and using method thereof |
| CN114773362A (en) * | 2022-06-15 | 2022-07-22 | 上海欣峰制药有限公司 | Cefoxitin sodium compound and preparation method thereof |
| CN114773362B (en) * | 2022-06-15 | 2023-12-29 | 上海欣峰制药有限公司 | Cefoxitin sodium compound and preparation method thereof |
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Denomination of utility model: A crystal separation and purification device for lithium hydroxide monohydrate Effective date of registration: 20230110 Granted publication date: 20201016 Pledgee: Agricultural Bank of China Limited Golmud Branch Pledgor: QINGHAI TUS-MEMBRANE NEW MATERIAL Co.,Ltd. Registration number: Y2022630000004 |
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