CN115448523A - Device for recovering lithium in lithium precipitation mother liquor - Google Patents
Device for recovering lithium in lithium precipitation mother liquor Download PDFInfo
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- CN115448523A CN115448523A CN202211346136.9A CN202211346136A CN115448523A CN 115448523 A CN115448523 A CN 115448523A CN 202211346136 A CN202211346136 A CN 202211346136A CN 115448523 A CN115448523 A CN 115448523A
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- lithium
- mother liquor
- centrifuge
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/041—Treatment of water, waste water, or sewage by heating by distillation or evaporation by means of vapour compression
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
Abstract
The invention discloses a device for recovering lithium from a lithium precipitating mother liquor, wherein the water inlet end of a crystallization separator is connected with a lithium precipitating mother liquor water inlet pipe, the water outlet end of the crystallization separator is connected with the water inlet end of a heater, the steam outlet of the crystallization separator is connected with the steam inlet of the heater, the water outlet end of the heater is connected with the water return port of the crystallization separator, the crystal slurry outlet of the crystallization separator is connected with the slurry inlet of a thickener, the crystal slurry outlet of the thickener is connected with the feed inlet of a first centrifuge, the solid material outlet of the first centrifuge is connected with the feed inlet of a salt washing tank, the liquid outlet of the first centrifuge is connected with the feed inlet of a mother liquor tank, the liquid outlet of the thickener is connected with the feed inlet of the mother liquor tank, the discharge end of the salt washing tank is connected with the feed inlet of a second centrifuge through a centrifuge feed pump, and the liquid outlet of the second centrifuge is connected with the liquid inlet of the salt washing tank. The lithium recovery device has a simple structure, can effectively improve the lithium recovery rate, and has relatively low energy consumption.
Description
Technical Field
The invention relates to the field of lithium recovery devices, in particular to a device for recovering lithium from lithium precipitation mother liquor.
Background
Lithium is an important new energy material, and the demand of lithium in the fields of automobiles, wind power, IT and the like is continuously increased. Particularly, as the sales of electric automobiles in China rapidly increase, the demand of lithium also rapidly increases.
At present, the treatment methods for the lithium precipitation mother liquor are more, new impurities are not introduced in the process of recovering lithium carbonate by carrying out evaporation crystallization after freezing crystallization on the lithium precipitation mother liquor, and the quality of the recovered lithium carbonate product is better, so the lithium carbonate is widely applied, but the temperature in the lithium precipitation process is generally about 85-95 ℃, the freezing temperature is-10-0 ℃, the temperature difference is larger, and the energy consumption and the treatment efficiency are lower for treating a large amount of the lithium precipitation mother liquor.
The Chinese patent CN106882822A proposes to recover lithium in the lithium precipitation mother liquor by a freezing salting-out method, and the process comprises the following steps: freezing, crystallizing and finely filtering the lithium precipitation mother liquor, removing sodium sulfate decahydrate formed by crystallization, then carrying out evaporation concentration, adding sodium carbonate to form lithium carbonate precipitate, and filtering to obtain a filter cake, namely a lithium carbonate crude product, wherein the lithium carbonate crude product is subjected to sodium sulfate removal and repeated washing to obtain high-purity lithium carbonate; the mother liquor is returned to the freezing and crystallizing process. However, this method has the following problems: in the process of removing sodium sulfate by a freezing salting-out method, a large amount of Li is carried, so that the lithium recovery rate is low, the circulation volume of the frozen fine filtration material is large, the energy consumption is high, the process is complex, and the production cost is greatly increased.
Therefore, the existing method and device for recovering lithium from the lithium precipitation mother liquor are to be further improved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the device for recovering lithium from the lithium precipitation mother liquor, which has a simple structure, can effectively improve the recovery rate of lithium and has relatively low energy consumption.
In order to achieve the purpose, the invention adopts the following scheme: the utility model provides a device of retrieving lithium in lithium mother liquor sinks, is including crystallization separator, crystallization separator's the end of intaking is connected with lithium mother liquor inlet tube that sinks, crystallization separator's the end of giving out water is connected with the end of intaking of heater, crystallization separator's steam outlet with the steam inlet of heater is connected, the play water end of heater is connected with crystallization separator's return water mouth, crystallization separator's magma export is connected with the thick liquid mouth that advances of ware, the magma export of thick liquid ware is connected with first centrifuge's feed inlet, first centrifuge's solid material export is connected with the feed inlet of salt washing groove, first centrifuge's liquid outlet is connected with the feed inlet of mother liquor jar, the liquid outlet of thick liquid ware is connected with the feed inlet of mother liquor jar the discharge end of salt washing groove is connected with the feed inlet of second centrifuge through centrifuge feed pump, the liquid outlet of second centrifuge with the feed liquor end of salt washing groove is connected, still includes saturated sodium chloride solution jar, the liquid outlet of saturated sodium chloride solution jar respectively with the feed liquor end of first centrifuge, the feed liquor end of second centrifuge is connected.
As another improvement of the device for recovering lithium in the lithium precipitation mother liquor, the liquid outlet end of the mother liquor tank is connected with the liquid inlet end of the crystallization separator through a mother liquor pump.
As another improvement of the device for recovering lithium in the lithium precipitation mother liquor, the liquid outlet end of the heater is connected with the liquid inlet end of the distilled water tank.
As another improvement of the device for recovering lithium from the lithium precipitation mother liquor, the liquid outlet end of the distilled water tank is connected with the second liquid inlet end of the distilled water heat exchanger through a distilled water pump, the lithium precipitation mother liquor water inlet pipe is connected with the first liquid inlet end of the distilled water heat exchanger, and the first liquid outlet end of the distilled water heat exchanger is connected with the water inlet end of the crystallization separator.
As another improvement of the device for recovering lithium in the lithium precipitation mother liquor, the lithium precipitation mother liquor inlet pipe is connected with the liquid inlet end of the raw liquor tank, and the water outlet end of the raw liquor tank is connected with the first liquid inlet end of the distilled water heat exchanger through the raw liquor pump.
As another improvement of the device for recovering lithium from the lithium precipitation mother liquor, a compressor is arranged on a pipeline between the steam outlet of the crystallization separator and the steam inlet of the heater.
As another improvement of the device for recovering lithium in the lithium precipitation mother liquor, a first stirring device can be arranged in the thickener.
As another improvement of the device for recovering lithium from the lithium precipitation mother liquor, a second stirring device is arranged in the salt washing tank.
As another improvement of the device for recovering lithium from the lithium precipitation mother liquor, the liquid outlet end of the circulating liquid of the crystallization separator is connected with the liquid inlet end of the heater through a circulating pump.
As another improvement of the device for recovering lithium from the lithium precipitation mother liquor, the liquid outlet end of the circulating pump is connected with the separation chamber, the concentrated liquid outlet end of the separation chamber is connected with the concentrated liquid temporary storage tank, and the liquid outlet end of the separation chamber is connected with the liquid inlet end of the crystallization separator.
In summary, compared with the prior art, the invention has the beneficial effects that: the invention changes the lithium deposition mother liquor into valuable, improves the utilization rate of lithium, has great economic benefit and reduces the discharge of waste water. According to the invention, the lithium content in the lithium precipitation mother liquor can be concentrated from 1g/L to more than 30g/L, and the lithium precipitation mother liquor can be directly recycled to a lithium precipitation workshop; distilled water obtained by evaporation can be reused for production, and sodium chloride obtained by evaporation can be used as a byproduct, namely industrial salt. The invention is used for ensuring the recovery rate of lithium by repeated washing of crystallized salt, and the actual recovery rate of lithium exceeds 99 percent.
Drawings
FIG. 1 is a schematic diagram of the present invention.
In the figure: 1. a crystallization separator; 2. a lithium precipitation mother liquor inlet pipe; 3. a heater; 4. a thickener; 5. a first centrifuge; 6. a salt washing tank; 7. a mother liquor tank; 8. a centrifuge feed pump; 9. a second centrifuge; 10. a saturated sodium chloride solution tank; 11. a flush pump; 12. a mother liquor pump; 13. a distilled water tank; 14. a distilled water pump; 15. a distilled water heat exchanger; 16. a stock solution tank; 17. a stock solution pump; 18. a compressor; 19. a first stirring device; 20. a second stirring device; 21. a circulation pump; 22. a separation chamber; 23. and (5) a concentrated solution temporary storage tank.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principles of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
As shown in fig. 1, a device for recovering lithium from a lithium precipitation mother liquor comprises a crystal separator 1, wherein a water inlet end of the crystal separator 1 is connected with a lithium precipitation mother liquor water inlet pipe 2, the lithium precipitation mother liquor water inlet pipe 2 is connected with a liquid inlet end of a raw liquid tank 16, the lithium precipitation mother liquor is fed into the raw liquid tank 16 through the lithium precipitation mother liquor water inlet pipe 2 in the production process, wherein the lithium precipitation mother liquor contains a large amount of carbonate, concentrated hydrochloric acid is added into the raw liquid tank 16 before the lithium precipitation mother liquor enters an evaporation system, the pH is adjusted to 3-5, and the carbonate in the lithium precipitation mother liquor is removed.
The water outlet end of the raw liquid tank 16 is connected with the first liquid inlet end of the distilled water heat exchanger 15 through a raw liquid pump 17. In the production process, the energy of distilled water evaporated from the heater 3 is recovered through the distilled water heat exchanger 15, the lithium precipitation mother liquor is preheated and then enters the crystallization separator 1, and is continuously concentrated in the heater 3 to be crystallized to obtain sodium chloride crystals. The distilled water obtained by evaporation has good water quality and can be reused for production. The energy consumption can be effectively reduced by the distilled water heat exchanger 15.
The water outlet end of the crystallization separator 1 is connected with the water inlet end of the heater 3, the steam outlet of the crystallization separator 1 is connected with the steam inlet of the heater 3, the water outlet end of the heater 3 is connected with the water return port of the crystallization separator 1, and the circulating liquid outlet end of the crystallization separator 1 is connected with the liquid inlet end of the heater 3 through a circulating pump 21. A compressor 18 is arranged on a pipeline between the steam outlet of the crystallization separator 1 and the steam inlet of the heater 3.
The crystallization separator 1, the heater 3, the circulating pump 21, the compressor 18 and the like constitute the forced MVR circulation in the present invention. In the invention, the lithium deposition mother liquor is heated by steam in a shell pass in a tube pass of a heater 3, the temperature is raised, the lithium deposition mother liquor is deposited under the action of a circulating pump 21 and rises to a crystallization separator 1, and the lithium deposition mother liquor is evaporated in the crystallization separator 1 due to the static pressure drop of the lithium deposition mother liquor. The secondary steam generated by evaporation overflows from the lithium deposition mother liquor, the lithium deposition mother liquor is concentrated to generate supersaturation so as to enable crystals to grow, the supersaturation-removed lithium deposition mother liquor enters a forced circulation pump 21 and enters a heater 3 under the action of the forced circulation pump 21, and the lithium deposition mother liquor is circulated in such a way to be continuously evaporated, concentrated or concentrated and crystallized. Obtaining sodium chloride crystal slurry; the crystal mush is output and input by a crystal mush pump. The secondary steam in the crystallization separator 1 is purified by a separation and defoaming device at the upper part of the crystallization separator 1 and then is conveyed to a compressor 18, and the compressor 18 compresses the secondary steam and then conveys the compressed secondary steam to the shell side of a heater 3 to be used as evaporator heating steam, thereby realizing the heat energy circulation continuous evaporation.
The magma outlet of the crystallization separator 1 is connected with the magma inlet of the thickener 4, the magma outlet of the thickener 4 is connected with the feed inlet of the first centrifuge 5, sodium chloride magma is enriched by the thickener, solids are separated from low-concentration semi-finished product magma by utilizing the gravity settling principle, the magma flows in from the central liquid feeding tank, and clear liquid is discharged from the periphery through the overflow port. The sediment or sediment in the thickener is collected to the center of the bottom of the thickener and is discharged through a discharge hole after being collected, thereby increasing the consistency of the material. The sodium chloride solid is then centrifuged by a first centrifuge 5. The liquid outlet of the first centrifuge 5 is connected with the feed inlet of the mother liquor tank 7, and the liquid outlet end of the mother liquor tank 7 is connected with the liquid inlet end of the crystallization separator 1 through a mother liquor pump 12. The centrifugal mother liquor enters a mother liquor tank 7 and is pumped to an evaporation system through a mother liquor pump for treatment.
The solid material export of first centrifuge 5 is connected with the feed inlet of salt washing groove 6, states the liquid outlet of stiff ware 4 and is connected with the feed inlet of mother liquor jar 7 the discharge end of salt washing groove 6 is connected with the feed inlet of second centrifuge 9 through centrifuge charge pump 8, the liquid outlet of second centrifuge 9 with the feed inlet of salt washing groove 6 is connected. The lithium possibly carried over on the surface of the sodium chloride solid is washed and recovered, so that the recovery rate of the lithium is improved.
The washed slurry enters a second centrifuge 9 and is centrifuged to obtain a byproduct sodium chloride. The centrifugal mother liquor returns to the salt washing tank, and washing liquor in the salt washing tank is discharged to the mother liquor tank discontinuously and then returns to the evaporation system for treatment.
The invention also comprises a saturated sodium chloride solution tank 10, wherein the liquid outlet end of the saturated sodium chloride solution tank 10 is respectively connected with the liquid inlet end of the first centrifugal machine 5 and the liquid inlet end of the second centrifugal machine 9 through a flushing pump 11.
According to the invention, the liquid outlet end of the distilled water tank 13 is connected with the second liquid inlet end of the distilled water heat exchanger 15 through the distilled water pump 14, the lithium precipitation mother liquor inlet pipe 2 is connected with the first liquid inlet end of the distilled water heat exchanger 15, and the first liquid outlet end of the distilled water heat exchanger 15 is connected with the water inlet end of the crystallization separator 1.
In the present invention, the thickener 4 can be provided with a first stirring device 19. A second stirring device 20 is arranged in the salt-washing tank 6.
In the invention, the liquid outlet end of the circulating pump 21 is connected with the separation chamber 22, the concentrated liquid outlet end of the separation chamber 22 is connected with the concentrated liquid temporary storage tank 23, and the liquid outlet end of the separation chamber 22 is connected with the liquid inlet end of the crystallization separator 1.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The utility model provides a device of retrieving lithium in lithium mother liquor sinks, is including crystal separator (1), the end of intaking of crystal separator (1) is connected with lithium mother liquor inlet tube (2) that sinks, the play water end of crystal separator (1) is connected with the end of intaking of heater (3), the steam outlet of crystal separator (1) with the steam inlet of heater (3) is connected, the play water end of heater (3) is connected with the return water mouth of crystal separator (1), the magma export of crystal separator (1) is connected with the thick liquid mouth that advances of thickener (4), the magma export of thickener (4) is connected with the feed inlet of first centrifuge (5), the solid material export of first centrifuge (5) is connected with the feed inlet of salt bath (6), the liquid outlet of first centrifuge (5) is connected with the feed inlet of mother liquor pot (7), the liquid outlet of thickener (4) is connected with the feed inlet of mother liquor pot (7), the discharge end of salt bath (6) includes that the discharge end of second centrifuge (9) is connected with the saturated solution tank (10) of sodium chloride solution pot (10) and the feed inlet of second centrifuge (10) are connected with the saturated solution pot (10) of sodium chloride solution pot (10), the saturated solution pot (10) of centrifuge (10) are connected with the feed inlet of centrifuge (10) and the feed inlet of second centrifuge (10) and the saturated solution pot (10) of centrifuge (10) are connected with the feed liquor pot (10) of centrifuge (10) respectively, the liquid inlet end of the second centrifugal machine (9) is connected.
2. The device for recovering lithium from a lithium precipitation mother liquor according to claim 1, wherein the liquid outlet end of the mother liquor tank (7) is connected with the liquid inlet end of the crystallization separator (1) through a mother liquor pump (12).
3. The device for recovering lithium in lithium precipitating mother liquor according to claim 1, wherein the liquid outlet end of the heater (3) is connected with the liquid inlet end of the distilled water tank (13).
4. The device for recovering lithium from the lithium precipitating mother liquor according to claim 3, wherein a liquid outlet end of the distilled water tank (13) is connected with a second liquid inlet end of the distilled water heat exchanger (15) through a distilled water pump (14), the lithium precipitating mother liquor inlet pipe (2) is connected with a first liquid inlet end of the distilled water heat exchanger (15), and a first liquid outlet end of the distilled water heat exchanger (15) is connected with a water inlet end of the crystallization separator (1).
5. The device for recovering lithium in lithium precipitating mother liquor according to claim 4, wherein the lithium precipitating mother liquor inlet pipe (2) is connected with a liquid inlet end of a raw liquor tank (16), and a liquid outlet end of the raw liquor tank (16) is connected with a first liquid inlet end of the distilled water heat exchanger (15) through a raw liquor pump (17).
6. The device for recovering lithium in the lithium precipitation mother liquor as claimed in claim 1, characterized in that a compressor (18) is arranged on a pipeline between a steam outlet of the crystallization separator (1) and a steam inlet of the heater (3).
7. The device for recovering lithium from the lithium precipitating mother liquor as claimed in claim 1, characterized in that the thickener (4) can be provided with a first stirring device (19).
8. The device for recovering lithium from the lithium precipitating mother liquor according to claim 1, wherein a second stirring device (20) is arranged in the salt washing tank (6).
9. The device for recovering lithium in lithium precipitation mother liquor according to claim 1, wherein the liquid outlet end of the circulation liquid of the crystallization separator (1) is connected with the liquid inlet end of the heater (3) through a circulation pump (21).
10. The device for recovering lithium from lithium precipitating mother liquor according to claim 9, wherein the liquid outlet end of the circulating pump (21) is connected with the separation chamber (22), the concentrated liquid outlet end of the separation chamber (22) is connected with the concentrated liquid temporary storage tank (23), and the liquid outlet end of the separation chamber (22) is connected with the liquid inlet end of the crystallization separator (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211346136.9A CN115448523A (en) | 2022-10-31 | 2022-10-31 | Device for recovering lithium in lithium precipitation mother liquor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211346136.9A CN115448523A (en) | 2022-10-31 | 2022-10-31 | Device for recovering lithium in lithium precipitation mother liquor |
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| Publication Number | Publication Date |
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| CN115448523A true CN115448523A (en) | 2022-12-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202211346136.9A Pending CN115448523A (en) | 2022-10-31 | 2022-10-31 | Device for recovering lithium in lithium precipitation mother liquor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116808701A (en) * | 2023-08-31 | 2023-09-29 | 山东齐鲁华信高科有限公司 | Device for preparing high-purity lithium chloride solution and high-purity sodium chloride |
-
2022
- 2022-10-31 CN CN202211346136.9A patent/CN115448523A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116808701A (en) * | 2023-08-31 | 2023-09-29 | 山东齐鲁华信高科有限公司 | Device for preparing high-purity lithium chloride solution and high-purity sodium chloride |
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