CN108298569A - A kind of device and its production method producing hydronium(ion) lithia based on MVR - Google Patents
A kind of device and its production method producing hydronium(ion) lithia based on MVR Download PDFInfo
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- CN108298569A CN108298569A CN201810334614.1A CN201810334614A CN108298569A CN 108298569 A CN108298569 A CN 108298569A CN 201810334614 A CN201810334614 A CN 201810334614A CN 108298569 A CN108298569 A CN 108298569A
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- preheater
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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
- C01D15/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0094—Evaporating with forced circulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/28—Evaporating with vapour compression
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
- B01D1/305—Demister (vapour-liquid separation)
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a kind of devices producing hydronium(ion) lithia based on MVR, including head tank, condensation water preheater, vapor preheater, forced-circulation evaporator, thickener, centrifuge, compressor and divide drum, raw material in the head tank is input to by feed pump in condensation water preheater, and the condensation water preheater is connected to by pipeline with vapor preheater;Raw material in vapor preheater is input to by pipeline in forced-circulation evaporator, and the forced-circulation evaporator includes heater one, heater two and crystal separator, the beneficial effects of the invention are as follows:Polishing inside forced circulation heater heat exchanger tube can effectively reduce the adhesive force that crystal in solution glues wall, ensure solution flow rate 2.5m/s or more in heat exchanger tube, while washing away to tube wall, further decrease heat exchange in-tube fouling frequency;The degree of superheat for reducing heater outlet simultaneously effectively prevent flash distillation, plugging in pipe, reduces the plugging phenomenon caused by the local mass crystallization that the degree of superheat is formed.
Description
Technical field
The present invention is a kind of device and its production method producing hydronium(ion) lithia based on MVR.
Background technology
Lithium is as new energy battery material essential element, now in the world for lithium demand just in double growth, especially
China.Thus the big production of hydration lithium hydroxide is expedited the emergence of out.
Tradition generates the technique of hydronium(ion) lithia, general to be carried out to lithium hydroxide solution using traditional triple effect evaporation system
Evaporative crystallization crystallizes out hydronium(ion) lithia.Since lithium hydroxide solution belongs to strong basicity, it is easy in evaporation and crystal process
Bubble, especially in the state of the high heat transfer temperature difference of traditional multiple-effect, blistering is particularly acute.Simultaneity factor easily forms plugging, influences
The heat transfer of heat exchanger leads to the reduction of system volatility, leads to energy waste.
In recent years, many producers are also attempting using mechanical steam recompression evaporative crystallization technique (MVR) production essence
Product hydronium(ion) lithia, but effect is all less desirable.Mainly in hydronium(ion) lithia evaporation process, indirect steam entrainment
A large amount of foam(Contain lithium hydroxide), can not effectively remove, cause condensed water pH at strong basicity, also need further to recycle condensation
Lithium hydroxide in water.The selection of evaporating temperature is improper, causes lithium hydroxide solution in heat exchanger tube in thermal histories, and water is precipitated
It closes lithium hydroxide to be attached on heat exchange tube wall, leads to the reduction of heat exchanger tube heat transfer property, influence to produce, can not accomplish long-term continuous raw
Production.
Invention content
The purpose of the present invention is to provide it is a kind of based on MVR produce hydronium(ion) lithia device and its production method, with
Solve the problems mentioned above in the background art.
To achieve the above object, the present invention provides the following technical solutions:
A kind of device producing hydronium(ion) lithia based on MVR, including head tank, condensation water preheater, vapor preheater, pressure
Circulating evaporator, thickener, centrifuge, compressor and divide drum, the raw material in the head tank is input to cold by feed pump
In condensate preheater, the condensation water preheater is connected to by pipeline with vapor preheater;Raw material in vapor preheater passes through
Pipeline is input in forced-circulation evaporator, and the forced-circulation evaporator includes heater one, heater two and Crystallization Separation
Device, wherein heater one and heater two are installed in series, and pass through pipeline and knot one of in heater one and heater two
Brilliant separator connection, and axial-flow pump is equipped on the pipeline, the bottom of the crystal separator by discharging pump and pipeline with it is thick
Thick device connection, the bottom of thickener are connect by pipeline with centrifuge, and the outlet end of centrifuge is connect with mother liquor tank, in mother liquor tank
Mother liquor by mother liquor pump be input in forced-circulation evaporator, by heater one and heater two heating after again into
Enter into crystal separator;The top of the crystal separator is connect with deentrainment tower, and deentrainment tower side is connected by pipeline to be compressed
Machine, the outlet side of compressor are connect with drum is divided with external boiler steam pipe, divide drum to vapor preheater, heater
One and heater two in export high-temperature steam, the outlet end of compressor connect with hydrops tank.
As a further solution of the present invention:The bottom of the vapor preheater, heater one and heater two is equipped with
Condensate pipe, condensate pipe are connect with condensate water pot, and the condensate water pot is by pipeline and condensate pump to condensation water preheater
Condensed water is exported, the side for condensing water preheater is equipped with condensation-water drain.
As further scheme of the invention:The lower part of the crystal separator has growing the grain slot.
As further scheme of the invention:The condensation water preheater and vapor preheater are multitube distance shell and tube
Heat exchanger.
As further scheme of the invention:The internal heat exchange tubes of the heater one and heater two are draw ratio
Big interior polishing heat exchanger tube.
A method of hydronium(ion) lithia is produced based on MVR, is included the following steps:
S1, lithium hydroxide solution are driven by feed pump in condensation water preheater, make lithium hydroxide by condensing water preheater
Solution is tentatively warming up to 40 ~ 50 DEG C, and the lithium hydroxide solution condensed in water preheater is input in vapor preheater later, rises
Temperature is to 70 ~ 80 DEG C;
S2 will be input in concatenated heater one and heater two by the lithium hydroxide solution preheated twice, exchange heat
Heating, the degree of superheat are maintained at 0.8 ~ 1.0 DEG C, then squeeze into crystal separator lithium hydroxide solution and flash, and generate 70
DEG C saturation indirect steam and 75 DEG C of concentrate;
S3, concentrate start generation nucleus in crystal separator and start to crystal separator lower part since nucleus proportion is larger
The sedimentation of growing the grain slot, form nucleus grows at salt leg formation crystal, the concentrate that the solid content that salt leg is formed is about 8% by
Discharging pump is squeezed into thickener;Indirect steam is input to after carrying out initial gross separation after crystal separator in deentrainment tower;
S4 passes through centrifugation when concentrate is further cooled down in thickener, stiff, growing the grain to solid content are 25% ~ 35%
Machine throws away hydronium(ion) lithia sodium crystal, and mother liquor enters in mother liquor tank or be back to after preheating crystal separator;
S5 carries out high-pressure spraying water-bath using high temperature circulation washings in deentrainment tower to indirect steam, and indirect steam passes through later
Compressor compresses heating is via dividing drum to re-enter into vapor preheater, heater one after voltage stabilizing together with external boiler steam
It is utilized again in heater two.
As further scheme of the invention:High-temperature wash water in the deentrainment tower is when pH value is increased to 12, weight
It is new to replace high-temperature wash water, and concentration is evaporated to former high-temperature wash water, recycle lithium hydroxide.
As further scheme of the invention:Polishing treatment is passed through in gas-liquid separation portion in the crystal separator, and
The effective height in gas-liquid separation portion must assure that in 6m or more.
Compared with prior art, the beneficial effects of the invention are as follows:(1)In the actual production process, it is ensured that evaporative condenser
Water band lithium amount is less than or equal to 10PPm;
(2)Polishing inside forced circulation heater heat exchanger tube can effectively reduce the adhesive force that crystal in solution glues wall, ensure heat exchange
Solution flow rate 2.5m/s or more in pipe, while tube wall is washed away, further decrease heat exchange in-tube fouling frequency;It reduces simultaneously
The degree of superheat of heater outlet effectively prevent flash distillation, plugging in pipe, reduction to be led due to the local mass crystallization that the degree of superheat is formed
The plugging phenomenon of cause;
(3)Crystal separator increases gas-liquid separation height, removes mist eliminator, reduces the position for having pressure drop, and cylinder inboard wall uses
Polishing technology can effectively reduce internal incrustation, while reach initial gross separation effect;
(4)It before indirect steam enters compressor, carries out washing vapour, the mist containing lithium hydroxide in indirect steam can be substantially reduced
Drop effectively collects the lithium hydroxide in indirect steam, while protecting vapour compression machine;
(5)Improved MVR evaporation and crystallization systems, cleaning frequency are substantially reduced, the cleaning frequency be about 2 ~ March/time;
(6)Crystal separator crystallizes end and increases growing the grain slot, it is ensured that and hydronium(ion) lithia crystalline solid is uniform, grain graininess >=
0.65mm。
Description of the drawings
Fig. 1 is a kind of structural schematic diagram for the device producing hydronium(ion) lithia based on MVR.
In figure:1- head tanks, 2- feed pumps, 3- condensations water preheater, 4- vapor preheaters, 5- axial-flow pumps, 6- heaters
One, 7- heaters two, 8- crystal separators, 9- deentrainment towers, 10- thickeners, 11- centrifuges, 12- mother liquor tanks, 13- mother liquors pump,
14- discharging pumps, 15- hydrops tank, 16- compressors, 17- divide drum, 18- condensate water pots, 19- condensate pumps.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, in the embodiment of the present invention, a kind of device producing hydronium(ion) lithia based on MVR, including head tank
1, water preheater 3, vapor preheater 4, forced-circulation evaporator, thickener 10, centrifuge 11, compressor 16 are condensed and divides drum
17, the raw material in the head tank 1 is input to by feed pump 2 in condensation water preheater 3, by condensation water preheater 3 to raw material
Progress tentatively lifts temperature to 40 ~ 50 DEG C, and the condensation water preheater 3 is connected to by pipeline with vapor preheater 4, due to lithium hydroxide
Solution evaporating temperature is controlled at 70 DEG C, can effectively reduce the generation of foam, contributes to the growth of hydronium(ion) oxidation crystalline lithium, because
This, needs vapor preheater 4 to be further preheated to 70 ~ 80 DEG C to raw material, i.e. raw material is squeezed into again in vapor preheater 4;Steam is pre-
Raw material in hot device 4 is input to by pipeline in forced-circulation evaporator, the forced-circulation evaporator include heater 1,
Heater 27 and crystal separator 8, wherein heater 1 and heater 27 are installed in series, heater 1 and heater 27
In one of connect with crystal separator 8 by pipeline, and axial-flow pump 5 is installed on the pipeline, enters forced circulation
Raw material in evaporator heats up by double-heater series connection forced circulation, and keeps the degree of superheat at 0.8 ~ 1.0 DEG C, overheat
Raw material is pumped by axial-flow pump 5 in crystal separator 8, and under level pressure state, superheated feedstock is flashed, and generates 70 DEG C of saturation
Indirect steam and 75 DEG C of concentrate start to generate nucleus, due to nucleus ratio at this point, hydronium(ion) lithia is in supersaturated area
Weight is larger, starts to settle to the growing the grain slot of 8 lower part of crystal separator, forms the formation crystal at salt leg that grows to of nucleus, described
The bottom of crystal separator 8 is connect by discharging pump 14 and pipeline with thickener 10, salt leg formed solid content be about 8% it is dense
Contracting liquid by discharging pump 14 squeeze into 10 further cooling of thickener, stiff, growing the grain to solid content be 25% ~ 35%, thickener 10
Bottom is connect by pipeline with centrifuge 11, and the outlet end of centrifuge 11 is connect with mother liquor tank 12, concentrate after stiff, into
Enter centrifuge 11 and throw away hydronium(ion) lithia sodium crystal, mother liquor enters in mother liquor tank 12, and the mother liquor in mother liquor tank 12 passes through mother
Liquid pump 13 is input in forced-circulation evaporator, and crystallization is re-entered into after the heating of heater 1 and heater 27
In separator 8;The top of the crystal separator 8 is connect with deentrainment tower 9, in crystal separator 8 after initial gross separation
Indirect steam enters in deentrainment tower 9, using the high-temperature-hot-water in deentrainment tower 9, carries out high-pressure spraying water-bath to indirect steam, can have
Effect absorbs the remaining lithium hydroxide carried secretly in indirect steam, and 9 side of deentrainment tower is by pipeline connect compressor 16, for secondary
Steam carries out compression heating, and the outlet side of compressor 16 is connect with drum 17 is divided with external boiler steam pipe, divides drum
17 export high-temperature steam into vapor preheater 4, heater 1 and heater 27, facilitate its preheating or heating to raw material,
The outlet end of compressor 16 is connect with hydrops tank 15.
The bottom of the vapor preheater 4, heater 1 and heater 27 is equipped with condensate pipe, condensate pipe with it is cold
Condensate tank 18 connects, and condensate water pot 18 is used to collect the condensed water that vapor preheater 4, heater 1 and heater 27 generate,
The condensate water pot 18 exports condensed water by pipeline and condensate pump 20 to condensation water preheater 3, to the condensation containing residual temperature
Water is utilized again, and the side of condensation water preheater 3 is equipped with condensation-water drain.
The lower part of the crystal separator 8 has growing the grain slot, contributes to the growth of hydronium(ion) lithia sodium crystal nucleus.
The condensation water preheater 3 and vapor preheater 4 are multitube distance tubular heat exchanger, dense by lithium hydroxide solution
Degree is higher, and hydronium(ion) lithia solubility is reduced as temperature increases, easily generation plugging phenomenon, and common plate heat exchanger
Circulation area is relatively narrow, is easy to cause discharge not to the utmost, influences the condition of lithium hydroxide product, therefore condense water preheater 3 and steam
Preheater 4 uses the preferable multitube distance tubular heat exchanger of circulation.
The internal heat exchange tubes of the heater 1 and heater 27 are the big interior polishing heat exchanger tube of draw ratio, ensure pipe
The flow velocity of interior raw material is in 2.5m/s or more.
A method of hydronium(ion) lithia is produced based on MVR, is included the following steps:
S1, lithium hydroxide solution are driven by feed pump in condensation water preheater, make lithium hydroxide by condensing water preheater
Solution is tentatively warming up to 40 ~ 50 DEG C, and the lithium hydroxide solution condensed in water preheater is input in vapor preheater later, rises
Temperature is to 70 ~ 80 DEG C;
S2 will be input in concatenated heater one and heater two by the lithium hydroxide solution preheated twice, exchange heat
Heating, the degree of superheat are maintained at 0.8 ~ 1.0 DEG C, then squeeze into crystal separator lithium hydroxide solution and flash, and generate 70
DEG C saturation indirect steam and 75 DEG C of concentrate;The lower degree of superheat, it is ensured that due to the hydronium(ion) oxidation by thermosetting
Crystalline lithium is in few state;
S3, concentrate start generation nucleus in crystal separator and start to crystal separator lower part since nucleus proportion is larger
The sedimentation of growing the grain slot, form nucleus grows at salt leg formation crystal, the concentrate that the solid content that salt leg is formed is about 8% by
Discharging pump is squeezed into thickener;Indirect steam is input to after carrying out initial gross separation after crystal separator in deentrainment tower;
S4 passes through centrifugation when concentrate is further cooled down in thickener, stiff, growing the grain to solid content are 25% ~ 35%
Machine throws away hydronium(ion) lithia sodium crystal, and mother liquor enters in mother liquor tank or be back to after preheating crystal separator;
S5 carries out high-pressure spraying water-bath, for recycling indirect steam using high temperature circulation washings in deentrainment tower to indirect steam
In lithium hydroxide, can effectively ensure that the cleanliness factor of indirect steam and prevent FC crystal separators stirring, run material, it is secondary later
Steam is heated up by compressor compresses via dividing drum to re-enter into vapor preheater, heater one together with external boiler steam
It is utilized again in heater two, makes full use of the indirect steam latent heat of vaporization, reach effects of energy saving and emission reduction.
High-temperature wash water in the deentrainment tower 9 re-replaces high-temperature wash water, and to former high when pH value is increased to 12
Temperature laundering water is evaporated concentration, recycles lithium hydroxide.
Polishing treatment is passed through in gas-liquid separation portion in the crystal separator, and the effective height in gas-liquid separation portion must be protected
Card avoids dirty block enrichment, growth in 6m or more.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (8)
1. a kind of device producing hydronium(ion) lithia based on MVR, including head tank(1), condensation water preheater(3), steam it is pre-
Hot device(4), forced-circulation evaporator, thickener(10), centrifuge(11), compressor(16)With divide drum(17), feature exists
In the head tank(1)Interior raw material passes through feed pump(2)It is input to condensation water preheater(3)It is interior, the condensation water preheater
(3)Pass through pipeline and vapor preheater(4)Connection;Vapor preheater(4)In raw material by pipeline be input to forced circulation steam
It sends out in device, the forced-circulation evaporator includes heater one(6), heater two(7)And crystal separator(8), wherein heating
Device one(6)With heater two(7)It is installed in series, heater one(6)With heater two(7)In one of pass through pipeline with knot
Brilliant separator(8)Connection, and axial-flow pump is installed on the pipeline(5), the crystal separator(8)Bottom pass through discharging pump
(14)With pipeline and thickener(10)Connection, thickener(10)Bottom pass through pipeline and centrifuge(11)Connection, centrifuge
(11)Outlet end and mother liquor tank(12)Connection, mother liquor tank(12)Interior mother liquor is pumped by mother liquor(13)It is input to forced circulation steaming
It sends out in device, by heater one(6)With heater two(7)Heating after re-enter into crystal separator(8)It is interior;The knot
Brilliant separator(8)Top and deentrainment tower(9)Connection, deentrainment tower(9)Side passes through pipeline connect compressor(16), compressor
(16)Outlet side and external boiler steam pipe with divide drum(17)Connection, divides drum(17)To vapor preheater(4)、
Heater one(6)With heater two(7)Interior output high-temperature steam, compressor(16)Outlet end and hydrops tank(15)Connection.
2. a kind of device producing hydronium(ion) lithia based on MVR according to claim 1, which is characterized in that the steaming
Vapour preheater(4), heater one(6)With heater two(7)Bottom be equipped with condensate pipe, condensate pipe and condensate water pot
(18)Connection, the condensate water pot(18)Pass through pipeline and condensate pump(20)To condensation water preheater(3)Condensed water is exported, it is cold
Condensate preheater(3)Side be equipped with condensation-water drain.
3. a kind of device producing hydronium(ion) lithia based on MVR according to claim 1, which is characterized in that the knot
Brilliant separator(8)Lower part have growing the grain slot.
4. a kind of device producing hydronium(ion) lithia based on MVR according to claim 1, which is characterized in that described cold
Condensate preheater(3)And vapor preheater(4)It is multitube distance tubular heat exchanger.
5. a kind of device producing hydronium(ion) lithia based on MVR according to claim 1, which is characterized in that described to add
Hot device one(6)With heater two(7)Internal heat exchange tubes be the big interior polishing heat exchanger tube of draw ratio.
6. according to a kind of any production methods producing hydronium(ion) lithia based on MVR of claim 1-5, feature exists
In including the following steps:
S1, lithium hydroxide solution are driven by feed pump in condensation water preheater, make lithium hydroxide by condensing water preheater
Solution is tentatively warming up to 40 ~ 50 DEG C, and the lithium hydroxide solution condensed in water preheater is input in vapor preheater later, rises
Temperature is to 70 ~ 80 DEG C;
S2 will be input in concatenated heater one and heater two by the lithium hydroxide solution preheated twice, exchange heat
Heating, the degree of superheat are maintained at 0.8 ~ 1.0 DEG C, then squeeze into crystal separator lithium hydroxide solution and flash, and generate 70
DEG C saturation indirect steam and 75 DEG C of concentrate;
S3, concentrate start generation nucleus in crystal separator and start to crystal separator lower part since nucleus proportion is larger
The sedimentation of growing the grain slot, form nucleus grows at salt leg formation crystal, the concentrate that the solid content that salt leg is formed is about 8% by
Discharging pump is squeezed into thickener;Indirect steam is input to after carrying out initial gross separation after crystal separator in deentrainment tower;
S4 passes through centrifugation when concentrate is further cooled down in thickener, stiff, growing the grain to solid content are 25% ~ 35%
Machine throws away hydronium(ion) lithia sodium crystal, and mother liquor enters in mother liquor tank or be back to after preheating crystal separator;
S5 carries out high-pressure spraying water-bath using high temperature circulation washings in deentrainment tower to indirect steam, and indirect steam passes through later
Compressor compresses heating is via dividing drum to re-enter into vapor preheater, heater one after voltage stabilizing together with external boiler steam
It is utilized again in heater two.
7. a kind of production method producing hydronium(ion) lithia based on MVR according to claim 6, which is characterized in that institute
The high-temperature wash water in deentrainment tower is stated when pH value is increased to 12, re-replaces high-temperature wash water, and to former high-temperature wash water into
Row is concentrated by evaporation recycling lithium hydroxide.
8. a kind of production method producing hydronium(ion) lithia based on MVR according to claim 6, which is characterized in that institute
State gas-liquid separation portion in crystal separator and pass through polishing treatment, and the effective height in gas-liquid separation portion must assure that 6m with
On.
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Cited By (9)
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CN109911921A (en) * | 2019-03-13 | 2019-06-21 | 上海中腾环保科技有限公司 | Using the system and method for MVR evaporative crystallization technique consecutive production hydronium(ion) lithia |
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KR20210066418A (en) * | 2019-11-28 | 2021-06-07 | 두산중공업 주식회사 | Recovery system of lithium compound and recovery method of lithium compound |
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