CN108996528B - A kind of old halogen in salt pan proposes lithium method - Google Patents
A kind of old halogen in salt pan proposes lithium method Download PDFInfo
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- CN108996528B CN108996528B CN201811133636.8A CN201811133636A CN108996528B CN 108996528 B CN108996528 B CN 108996528B CN 201811133636 A CN201811133636 A CN 201811133636A CN 108996528 B CN108996528 B CN 108996528B
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/80—Compositional purity
Abstract
A kind of old halogen in salt pan proposes lithium method, comprising the following steps: (1) adsorbs demagging；(2) Shift speed segmentally elutes de- lithium；(3) ion exchange resin adsorption deeply demagging；(4) reverse osmosis；(5) prepared by lithium carbonate.The present invention comprehensively utilizes absorption demagging, Shift speed segmentally elutes the kinds of processes such as de- lithium, the demagging of ion exchange resin adsorption deeply, reverse osmosis, thoroughly solve the problems, such as that the old halogen Mg/Li ratio in salt pan is excessively high, production cost is low, project cost is low, have compared with strong adaptability, product lithium carbonate purity is up to electronics level lithium carbonate purity.
Description
Technical field
The present invention relates to the methods that a kind of old halogen in salt pan mentions lithium, and in particular to a kind of old halogen in salt pan of chloride type brine is adopted
The method for extracting lithium carbonate with the techniques such as reverse osmosis are adsorbed.
Background technique
Lithium metal and lithium salts are the important strategic resources of country, be widely used in aerospace, electronics, metal material,
The various fields such as equipment manufacturing, nuclear energy and national defense industry, in the case where electronics industry and the demand of metal material industry drive, the need of lithium
The amount of asking is huge, and demand of the annual whole world to lithium carbonate is still constantly increasing.Therefore, the utilization rate of lithium resource is improved, reduction is opened
Hair cost is of great significance to the support national economic development.
70% lithium resource derives from brine in the world.In the world 4 maximum brine lithium deposites be distributed in Bolivia,
The Salt Lake Zabuye of Chile, Argentina and China, containing lithium all at 100,000 tons or more.
It is both at home and abroad exploitation brine lithium resource, the extracting method of various brine lithium salts is had conducted extensive research.Currently, state
It is inside and outside to extract brine lithium resource technical matters mainly have evaporative crystallization method, the precipitation method, extraction, ion exchange adsorption,
Calcine leaching method, solar pond method, Xu Shi method and electroosmose process etc..The wherein precipitation method, extraction, ion exchange adsorption and carbonization
Method is studied extensively and profoundly, is that main salt lake bittern proposes lithium method.Above method by salt lake resources condition limited it is more or
It is required that brine lithium resource is high-quality or high production cost or project cost it is expensive, it is difficult to various types salt lake all be unfolded greatly
Scale development.And each salt lake feature is multifarious.
The lithium resource in China, 80% contains in salt lake bittern.But the lithium resource Exploitation degree in salt lake is very low, mainly
Be because the most of magnesium ion contents of China's salt lake bittern it is higher, cause Mg/Li ratio higher, magnesium lithium chemical physical property again extremely
It is close, and magnesium ion must be removed during mentioning lithium.Salt lake bittern magnesium ion content is high, causes to mention from salt lake bittern
The cost of lithium greatly improves.Part lithium can be lost during demagging simultaneously, makes the reduction of lithium yield, keeps product quality not up to standard.Such as
Mg/Li ratio is mostly in 50:1 or more in Qinghai Salt Lake Bittern, and it is even more to exist containing the old halogen Mg/Li ratio of lithium that main salt lake bittern, which mentions after potassium,
200:1 or more, this is that Qinghai Salt Lake lithium resource abundant is caused not obtain the main reason for large-scale developing and utilizing.
Currently, the salt lake bittern for high Mg/Li ratio is developed, it is thus proposed that absorption method, calcination method, electrodialysis, extraction etc.
Method.Wherein, selective absorption will be helpful to solve the problems, such as this, but adsorbent this key technology fails effectively to be dashed forward
It is broken；The problems such as calcination method mentions lithium, due to its energy consumption and pollutes, is not also promoted；Electroosmose process need special device with
Permeable membrane, the presence of these problems seriously constrain the development that salt lake bittern proposes lithium industry.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide one kind and be produced into
This is low, project cost is low, has compared with strong adaptability, and the old halogen in salt pan of product lithium carbonate purity is high proposes lithium method.
The technical solution adopted by the present invention to solve the technical problems is, a kind of old halogen in salt pan proposes lithium method, including following
Step:
(1) demagging is adsorbed
A) adsorb: the old halogen in salt pan flows automatically from old halogen reservoir enters old halogen conditioning tank, in old halogen conditioning tank, clear old halogen
With the discharge liquor or brackish water or mixing of fresh water for washing magnesium, then it being pumped into adsorption tower, the old halogen in salt pan enters from adsorption tower top,
It is flowed out from the bottom of adsorption tower, the liquid flowed out from absorption tower bottom is known as adsorption tail liquid, is discharged into old halogen canal；Adsorption tower tower is inhaled
Attached saturation terminates absorption, arranges halogen operational sequence into compressed air；
B) compressed air arranges brine: after saturation adsorption tower adsorption saturation, upper space is still filled with brine, using compression
Air empties this part brine as far as possible, and discharge liquor returns to old halogen conditioning tank；
C) wash demagging: the saturation adsorption tower after row's halogen turns water washing operations, by fresh water or brackish water by being saturated adsorption tower,
Saturation adsorption tower is washed, discharge liquor is discharged into old halogen conditioning tank；
(2) Shift speed segmentally elutes de- lithium
A) one section of elution: the saturation adsorption tower after washing, elution will be passed through from one section of leacheate of following b) steps
Liquid is entered by the top of the saturation adsorption tower, and bottom outflow, efflux is qualified lithium leacheate, is store into qualified lithium leacheate
Pond；
B) two sections of elution: will be entered from two sections of leacheates in step c) by the top of the saturation adsorption tower, bottom stream
Out, it is spare to be discharged into one section of leacheate reservoir as one section of leacheate for the efflux；
C) three sections of elution: the fresh water of the reverse osmosis output of fresh water or fresh water and part, as three sections of elution wash waters, by described
The top for being saturated adsorption tower enters, and bottom outflow, the efflux of this section is discharged into two sections of leacheate reservoirs as two sections of leacheates
It is spare；
It runs for the first time, is from c) step 3 section feeding, two sections at this time, one section are void towers, are completed to three sections of elution processing, stream
Liquid enters two sections out, makees b) step 2 section leacheate, completes to two sections of elution processing, efflux is eluted as a) step 1 section
Liquid；
(3) depth demagging
A) a depth demagging: being adsorbed using single column, and one time depth demagging tower loads Cation adsorption resin, and lithium is eluted
Liquid is pumped into a depth demagging tower from leacheate reservoir, enters from the top of tower, and bottom outflow, this process efflux is primary
Demagging lithium leacheate, the material liquid into a demagging lithium leacheate reservoir, as secondary deep demagging；
B) secondary deep demagging: being adsorbed using single column, and secondary deep demagging tower also loads Cation adsorption resin, will be primary
Demagging lithium leacheate is pumped into secondary deep demagging tower from a demagging lithium leacheate reservoir, enters from tower top, bottom outflow, this
Process efflux is secondary demagging lithium leacheate, into secondary demagging lithium leacheate reservoir, as reverse osmosis material liquid；
(4) secondary demagging lithium leacheate is imported into reverse osmosis unit by reverse osmosis process, and dope returns to old halogen field, seeps
Transparent liquid enters vaporising device, is concentrated by evaporation, and obtains high lithium mother liquor, is sent into lithium carbonate preparation section；
(5) lithium carbonate prepares workshop section
A) it filters refining step: high lithium mother liquor obtained by step (4) being pumped directly into flame filter press filtering and is desilted, filtrate warp
After microfroc filter further cleans, it is pumped into the high lithium solution head tank of purification；It will be through the filtered saturation soda ash of microfroc filter
Solution is delivered to head tank, the raw material as sinker reaction；
B) sinker process: being added reaction kettle with saturation soda ash solution for the high lithium mother liquor after secondary filter and react,
Lithium carbonate is generated, after sedimentation separation, the solution of lithium carbonate containing enters centrifuge centrifugation, is emitted into after the acidified tune pH value of clear liquid old
Lithium is further recycled in halogen reservoir, filter cake is Crude lithium Carbonate, after second adverse current washing and centrifugal filtration, is into dry
System；
C) dry, packaging.
Further, the sub-step a) in step (1), the adsorption tower include No. 1 tower, No. 2 towers, No. 3 towers, No. 4 towers, wherein
No. 1 tower, No. 2 towers, No. 3 towers are sequentially connected in series, tower headed by No. 1 tower, and No. 3 towers are tailing column, the old halogen in salt pan from No. 1 tower, that is, top Shou Ta into
Enter, flowed out from No. 3 tower, that is, tailing column bottoms, the liquid flowed out from tailing column bottom is known as adsorption tail liquid, is discharged into old halogen canal；Operation
After 200-500 minutes (preferably 300-400 minutes), adsorbent adsorption saturation in No. 1 tower terminates absorption, under No. 1 tower switching
Come, arranges halogen operational sequence into compressed air；Hereafter, No. 2 towers become first tower, meanwhile, upper No. 4 towers of connecting behind No. 3 towers, 4
Number tower becomes tailing column, and adsorbed state is No. 2 towers, No. 3 towers, No. 4 towers series connection absorption, operating parameter and No. 1 tower, No. 2 at this time
Tower, No. 3 tower series connection adsorption operations parameters are identical, and then No. 2 towers are switched, and arrange halogen operational sequence into compressed air；Such as
This circulate operation so far completes an operation circulation until being returned to No. 1 tower, No. 2 towers, No. 3 tower series connection absorption.
Further, the sub-step c) in step (1), the fresh water or brackish water are with 300-1000m3The preferred 500- of/h(
800m3/ h) flow by saturation adsorption tower, the used time be 5-25 minutes (preferably 10-20 minutes).
Further, the sub-step a) in step (2), one section of leacheate is with 40-100m3The preferred 50-80m of/h(3/ h) flow
By the saturation adsorption tower after washing, the time that bottom is flowed out is entered to from top, is the preferred 2.0-3.5h of 1.5-4.0h().
Further, the sub-step b) in step (2), two sections of leacheates are with 150-200m3The flow of/h is inhaled by the saturation
The top of attached tower enters, and bottom outflow is 1-3h by the time.
Further, the sub-step c) in step (2), fresh water is with 160-200m3The preferred 170-190m of/h(3/ h) flow by
The top of the saturation adsorption tower enters, and bottom outflow is the preferred 2.0-2.5h of 1.5-3.0h(by the time).
Further, the sub-step a) in step (3), in a depth demagging tower, the filling of the Cation adsorption resin
Amount is 40.0-50.0 m3(preferably 44-46m3)；Lithium leacheate is with 150-300m3The preferred 180-250m of/h(3/ h) flow be pumped into
Depth demagging tower, lithium leacheate from tower top enter tower bottom outflow, the total time be 120-180 minutes (preferably
140-160 minutes).
Further, the sub-step b) in step (3), in secondary deep demagging tower, the filling of the Cation adsorption resin
Amount is 40.0-50.0 m3；Lithium leacheate is with 200-360m3The preferred 300-340m of/h(3/ h) flow be pumped into secondary deep demagging
Tower, lithium leacheate enter tower bottom outflow from tower top, and the total time is the preferred 32-34h of 30-36h().
Further, in step (4), the lithium ion content of the high lithium mother liquor is 2-10g/l.
Further, the sub-step a) in step (5), after the high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, heating
To 70~90 DEG C.
The adsorbent loaded in the adsorption tower can be aluminium system adsorbent, be also possible to manganese systems adsorbent or its
His compound-type adsorbent.
The present invention comprehensively utilizes conventional absorbtion, Shift speed segmentally takes off lithium, the demagging of ion exchange resin adsorption deeply, reverse osmosis etc.
Kinds of processes thoroughly solves the problems, such as that the old halogen Mg/Li ratio in salt pan is excessively high, and production cost is low, and project cost is low, has compared with strong adaptability,
Product lithium carbonate purity is high, up to electronics level lithium carbonate purity.
Specific embodiment
The invention will be further described with reference to embodiments.
Original halogen used in the embodiment of the present invention is the old old halogen in halogen pond of China Qinghai Area sylvite manufacturing enterprise.
Embodiment 1
(1) demagging is adsorbed:
A) adsorb: old halogen flows automatically from old halogen reservoir enters old halogen conditioning tank, in old halogen conditioning tank, clear old halogen and water
The discharge liquor (running for the first time, do not wash and wash magnesium discharge liquor, use fresh water) for washing magnesium mixes, and is pumped into absorption by brine pump
Tower, adsorption tower include No. 1 tower, No. 2 towers, No. 3 towers, No. 4 towers, and No. 1 tower, No. 2 towers, No. 3 towers are sequentially connected in series, brine by No. 1 tower (i.e.
First tower) top entrance, it is flowed out from No. 3 tower (i.e. tailing column) bottoms, the adsorption tail liquid flowed out from No. 3 towers is discharged into old halogen canal；Operation
Time 300 minutes, No. 1 tower adsorption saturation terminated absorption, and No. 1 tower switches into compressed air row's halogen operation workshop section；This
Afterwards, No. 2 towers become first tower, meanwhile, upper No. 4 towers of connecting behind No. 3 towers, No. 4 towers become tailing column, at this point, adsorbed state is 2
Number, No. 3, the series connection absorption of No. 4 towers, operating parameter is same as above；Then, No. 2 towers, which are switched into compressed air, arranges halogen operative employee
Section；Such circulate operation so far completes an operation circulation until being returned to No. 1, No. 2, No. 3 tower series connection absorption；
B) compressed air arranges brine: after saturation adsorption tower is switched, upper space is still filled with brine, using compression
Air empties this part brine as far as possible, and discharge liquor returns to old halogen pond；Saturator under switching each time all passes through compressed air
Arrange the operation of brine；
C) wash demagging: the saturation adsorption tower after row's halogen turns water washing operations: by fresh water with 700m3The flow of/h quickly through
It is switched the saturation adsorption tower to get off, the used time is 15 minutes, and discharge liquor is discharged into old halogen conditioning tank；
(2) Shift speed segmentally elutes de- lithium:
A) one section of elution, by one section of leacheate with 60m3The flow of/h is entered by adsorption tower, leacheate by the top of tower
It is flowed out to bottom, by 3 hours, efflux entered qualified leacheate reservoir, lithium concentration 400g/L, magnesium density 3.5g/L；
B) two sections of elution, by two sections of leacheates with 160m3The flow of/h is entered by the top of tower, bottom outflow, the used time 1.5
Hour, efflux is discharged into one section of leacheate reservoir as one section of leacheate；
C) three sections of elution, the fresh water of the reverse osmosis output of fresh water and part as three sections of elution wash waters, this part fresh water with
180m3The flow of/h is entered by the top of tower, bottom outflow, and by 2 hours, the efflux of this section was as two sections of leacheates, row
It is put into two sections of leacheate reservoirs；
It runs for the first time, is from c) step 3 section feeding, two sections at this time, one section are void towers, are completed to three sections of elution processing, stream
Liquid enters two sections out, makees b) step 2 section leacheate, completes to two sections of elution processing, efflux is eluted as a) step 1 section
Liquid；
(3) depth demagging:
A) a depth demagging: being adsorbed using single column, and adsorption tower loads resin cation, and absorption resin loading is 45.3
m3, by lithium leacheate from leacheate reservoir with 210m3The flow of/h is pumped into depth demagging tower, is flowed into tower lower part from tower top and flows
Out, used time 150 minutes in total；This workshop section efflux, once to remove magnesium liquid, into once except magnesium liquid reservoir；After being sufficiently mixed, make
For the material liquid of secondary deep demagging；
B) secondary deep demagging: being adsorbed using single column, and resin loadings are 45.3 m3, by lithium leacheate from a demagging
Liquid reservoir is with 320m3The flow of/h is pumped into secondary deep demagging tower, in total used time 33.3 hours；This workshop section efflux is secondary
Except magnesium liquid, magnesium liquid reservoir is removed into secondary, as reverse osmosis material liquid；
(4) reverse osmosis process:
By secondary except magnesium liquid imported into reverse osmosis unit, dope returns to old halogen field, and penetrating fluid enters vaporising device, concentration
It is 7g/l to lithium ion content, is sent into lithium carbonate and prepares workshop section；
(5) prepared by lithium carbonate:
A) it filters refining step: the high lithium mother liquor after concentration being pumped directly into flame filter press filtering and is desilted, filtrate is through essence
After close filter further cleans, it is pumped into the high lithium solution head tank of purification, is heated to 85 DEG C；By the soda ash solution of saturation, through essence
After close filter filtering, it is delivered to head tank with pump, the raw material as sinker reaction:
B) sinker process: by the soda ash solution of the high lithium mother liquor after secondary filter and saturation be proportionally added into reaction kettle into
Row reaction, generates lithium carbonate, after sedimentation separation, the solution of lithium carbonate containing enters centrifuge centrifugal filtration, the acidified tune of clear liquid
It after pH value, is emitted into old halogen pond, further recycles lithium, filter cake is Crude lithium Carbonate, by secondary secondary countercurrent washing and is centrifuged
After filter, into drying, packaging system；
C) dry, packaging: wet lithium carbonate is sent into flash dryer by belt conveyor, with the cigarette from coal combustion furnace
Gas co-current contact makes lithium carbonate finished product obtain drying；Lithium carbonate after drying is sent into finished product packing machine, automatic gauge, packaging, people
Work stacking.For lithium carbonate dust after sack cleaner recycles, tail gas is directly discharged into atmosphere.
Through detecting, lithium carbonate product purity obtained by the present embodiment is 99.8%.
Embodiment 2
The present embodiment and the difference of embodiment 1 are only that:
(1) demagging is adsorbed:
A), old halogen enters tailing column bottom from the top Shou Ta and flows out, and runing time is 500 minutes；
C), washing demagging uses brackish water, flow 500m3/ h, used time are 10 minutes；
(2) Shift speed segmentally elutes de- lithium:
A), the flow of one section of leacheate is 90m3/h；Leacheate enters bottom outflow by the top of tower, is by the time
3.5 hours, the lithium concentration of efflux was about 550g/L, magnesium density 3g/L；
B), the flow of two sections of leacheates is 200m3/ h, leacheate enter bottom by the top of tower and flow out, and the used time 2 is small
When；
C), three sections of elution, the flow of three sections of elution wash waters are 180m3/ h, washing water enter bottom by the top of tower and flow
Out, by 2 hours；
(3) depth demagging:
A), the flow of lithium leacheate is 210m3/h；It is flowed into tower lower part from tower top to flow out, in total used time 150 minutes；
B) flow of lithium leacheate is 340m3/ h is flowed into tower lower part from tower top and flows out, in total used time 34 hours；
(4) reverse osmosis workshop section:
Being concentrated to lithium ion content is 9g/l, is sent into lithium carbonate and prepares workshop section；
(5) prepared by lithium carbonate:
A), it will be pumped into the high lithium mother liquor for refining high lithium solution head tank, is heated to 85 DEG C；
Remaining same embodiment 1.
Through detecting, lithium carbonate product purity obtained by the present embodiment is 99.6%.
Embodiment 3
The present embodiment and the difference of embodiment 1 are only that:
(1) demagging is adsorbed:
A), the top Cong Shouta enters the outflow of tailing column bottom, and runing time is 250 minutes；
C), washing demagging uses fresh water, flow 800m3/ h, used time are 20 minutes；
(2) Shift speed segmentally elutes de- lithium:
A), the flow of one section of leacheate is 50m3/h；Leacheate enters bottom outflow by the top of tower, is by the time
2.5 hours, the lithium concentration of efflux was 500g/L, magnesium density 3g/L；
B), the flow of two sections of leacheates is 150m3/ h, leacheate enter bottom by the top of tower and flow out, and the used time 2 is small
When；
C), three sections of elution, the flow of three sections of elution wash waters are 160m3/ h, washing water enter bottom by the top of tower and flow
Out, by 2 hours；
(3) depth demagging:
A), the flow of lithium leacheate is 210m3/h；It is flowed into tower lower part from tower top to flow out, in total used time 160 minutes；
B) flow of lithium leacheate is 200m3/ h is flowed into tower lower part from tower top and flows out, in total used time 32 hours；
(4) reverse osmosis workshop section:
Being concentrated to lithium ion content is 8g/l, is sent into lithium carbonate and prepares workshop section；
(5) prepared by lithium carbonate:
A), it will be pumped into the high lithium mother liquor for refining high lithium solution head tank, is heated to 88 DEG C；
Remaining same embodiment 1.
Through detecting, lithium carbonate product purity obtained by the present embodiment is 99.7%.
The prior art that the content being not described in detail in specification is known to the skilled person.
Claims (41)
1. a kind of old halogen in salt pan proposes lithium method, which comprises the following steps:
(1) demagging is adsorbed
A) adsorb: the old halogen in salt pan enters old halogen conditioning tank from old halogen reservoir, and in old halogen conditioning tank, clear old halogen and washing are removed
The discharge liquor or brackish water or mixing of fresh water of magnesium, then it is pumped into adsorption tower, the old halogen in salt pan enters from adsorption tower top, from adsorption tower
Bottom outflow, from absorption tower bottom flow out liquid be known as adsorption tail liquid, be discharged into old halogen canal；Adsorbent in adsorption tower is inhaled
Attached saturation terminates absorption, arranges halogen operational sequence into compressed air；
B) compressed air arranges brine: after the adsorbent adsorption saturation in adsorption tower, upper space is still filled with brine, using pressure
Contracting air empties this part brine as far as possible, and discharge liquor returns to old halogen conditioning tank；
C) wash demagging: the saturation adsorption tower after row's halogen turns water washing operations, by fresh water or brackish water by saturation adsorption tower, to suction
The adsorbent of adsorption saturation is washed in attached tower, and discharge liquor is discharged into old halogen conditioning tank；
(2) Shift speed segmentally elutes de- lithium
A) one section of elution: will from one section of leacheate of following b) steps, by the saturation adsorption tower after washing, leacheate by
The top of the saturation adsorption tower enters, and bottom outflow, efflux is qualified lithium leacheate, into qualified lithium leacheate reservoir；
B) two sections of elution: will be entered from two sections of leacheates in step c) by the top of the saturation adsorption tower, bottom outflow, institute
Efflux is stated as one section of leacheate, it is spare to be discharged into one section of leacheate reservoir；
C) three sections of elution: the fresh water of the reverse osmosis output of fresh water or fresh water and part, as three sections of elution wash waters, by the saturation
The top of adsorption tower enters, and it is standby to be discharged into two sections of leacheate reservoirs as two sections of leacheates for bottom outflow, the efflux of this section
With；
It runs for the first time, is from c) step 3 section feeding, two sections at this time, one section are void towers, are completed to three sections of elution processing, efflux
Enter two sections, make b) step 2 section leacheate, is completed to two sections of elution processing, efflux is as a) step 1 section leacheate；
(3) depth demagging
A) a depth demagging: being adsorbed using single column, and depth demagging tower loads Cation adsorption resin, by lithium leacheate from
Leacheate reservoir is pumped into a depth demagging tower, enters from the top of tower, bottom outflow, this process efflux is a demagging
Lithium leacheate, the material liquid into a demagging lithium leacheate reservoir, as secondary deep demagging；
B) it secondary deep demagging: is adsorbed using single column, secondary deep demagging tower also loads Cation adsorption resin, by a demagging
Lithium leacheate is pumped into secondary deep demagging tower from a demagging lithium leacheate reservoir, enters from tower top, bottom outflow, this process
Efflux is secondary demagging lithium leacheate, into secondary demagging lithium leacheate reservoir, as reverse osmosis material liquid；
(4) secondary demagging lithium leacheate is imported into reverse osmosis unit by reverse osmosis process, and dope returns to old halogen field, penetrating fluid
It into vaporising device, is concentrated by evaporation, obtains high lithium mother liquor, be sent into lithium carbonate preparation section；
(5) lithium carbonate prepares workshop section
A) it filters refining step: high lithium mother liquor obtained by step (4) being pumped directly into flame filter press filtering and is desilted, filtrate is through precision
After filter further cleans, it is pumped into the high lithium solution head tank of purification；Will through the filtered saturation soda ash solution of microfroc filter,
It is delivered to head tank, the raw material as sinker reaction；
B) sinker process: reaction kettle is added with saturation soda ash solution in the high lithium mother liquor after secondary filter and is reacted, is generated
Lithium carbonate, after sedimentation separation, the solution of lithium carbonate containing enters centrifuge centrifugation, is emitted into old halogen pond after the acidified tune pH value of clear liquid
In further recycle lithium, filter cake is Crude lithium Carbonate, by second adverse current washing and centrifugal filtration after, into drying system；
C) dry, packaging.
2. the as described in claim a kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (1), it is described
Adsorption tower includes No. 1 tower, No. 2 towers, No. 3 towers, No. 4 towers, wherein No. 1 tower, No. 2 towers, No. 3 towers are sequentially connected in series, tower headed by No. 1 tower,
No. 3 towers are tailing column, and the old halogen in salt pan enters from No. 1 tower, that is, top Shou Ta, are flowed out from No. 3 tower, that is, tailing column bottoms, from tailing column bottom
The liquid of outflow is known as adsorption tail liquid, is discharged into old halogen canal；After operation 200-500 minutes, No. 1 tower adsorption saturation terminates absorption,
No. 1 tower switches, and arranges halogen operational sequence into compressed air；Hereafter, No. 2 towers become first tower, meanwhile, it is gone here and there behind No. 3 towers
Join No. 4 towers, No. 4 towers become tailing column, and adsorbed state is No. 2 towers, No. 3 towers, No. 4 tower series connection absorption, operating parameter and institute at this time
It states that No. 1 tower, No. 2 towers, No. 3 towers series connection adsorption operations parameters are identical, and then No. 2 towers are switched, arranges halogen into compressed air
Operational sequence；Such circulate operation is so far completed an operation and is followed until being returned to No. 1 tower, No. 2 towers, No. 3 tower series connection absorption
Ring.
3. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (1),
Sub-step c) in step (1), the fresh water or brackish water are with 300-1000m3The flow of/h passes through saturation adsorption tower, used time
It is 5-25 minutes.
4. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (2),
One section of leacheate is with 40-100m3The flow of/h by washing after saturation adsorption tower, from top enter to bottom flow out when
Between, it is 1.5-4.0h.
5. the as claimed in claim 3 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (2), one section
Leacheate is with 40-100m3The flow of/h enters to the time that bottom is flowed out by the saturation adsorption tower after washing, from top, is
1.5-4.0h。
6. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (2),
Two sections of leacheates are with 150-200m3The flow of/h is entered by the top of the saturation adsorption tower, and bottom outflow is 1- by the time
3h。
7. the as claimed in claim 3 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (2), two sections
Leacheate is with 150-200m3The flow of/h is entered by the top of the saturation adsorption tower, and bottom outflow is 1-3h by the time.
8. the as claimed in claim 4 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (2), two sections
Leacheate is with 150-200m3The flow of/h is entered by the top of the saturation adsorption tower, and bottom outflow is 1-3h by the time.
9. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step c) in step (2),
Fresh water is with 160-200m3The flow of/h is entered by the top of the saturation adsorption tower, and bottom outflow is 1.5- by the time
3.0h。
10. the as claimed in claim 3 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step c) in step (2) is light
Water is with 160-200m3The flow of/h is entered by the top of the saturation adsorption tower, and bottom outflow is 1.5-3.0h by the time.
11. the as claimed in claim 4 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step c) in step (2) is light
Water is with 160-200m3The flow of/h is entered by the top of the saturation adsorption tower, and bottom outflow is 1.5-3.0h by the time.
12. the as claimed in claim 6 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step c) in step (2) is light
Water is with 160-200m3The flow of/h is entered by the top of the saturation adsorption tower, and bottom outflow is 1.5-3.0h by the time.
13. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (3)
, in a depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 150-
300m3The flow of/h is pumped into a depth demagging tower, and lithium leacheate enters tower bottom outflow from tower top, and the total time is
120-180 minutes.
14. the as claimed in claim 3 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (3), one
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 150-300m3/h
Flow be pumped into a depth demagging tower, lithium leacheate enters tower bottom outflow from tower top, and the total time is 120-180 points
Clock.
15. the as claimed in claim 4 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (3), one
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 150-300m3/h
Flow be pumped into a depth demagging tower, lithium leacheate enters tower bottom outflow from tower top, and the total time is 120-180 points
Clock.
16. the as claimed in claim 6 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (3), one
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 150-300m3/h
Flow be pumped into a depth demagging tower, lithium leacheate enters tower bottom outflow from tower top, and the total time is 120-180 points
Clock.
17. the as claimed in claim 9 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (3), one
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 150-300m3/h
Flow be pumped into a depth demagging tower, lithium leacheate enters tower bottom outflow from tower top, and the total time is 120-180 points
Clock.
18. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (3),
In secondary deep demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 200-360m3/
The flow of h is pumped into secondary deep demagging tower, and lithium leacheate enters tower bottom outflow, total time 30-36h from tower top.
19. the as claimed in claim 3 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (3), two
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 200-360m3/h
Flow be pumped into secondary deep demagging tower, lithium leacheate enters tower bottom outflow, total time 30-36h from tower top.
20. the as claimed in claim 4 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (3), two
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 200-360m3/h
Flow be pumped into secondary deep demagging tower, lithium leacheate enters tower bottom outflow, total time 30-36h from tower top.
21. the as claimed in claim 6 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (3), two
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 200-360m3/h
Flow be pumped into secondary deep demagging tower, lithium leacheate enters tower bottom outflow, total time 30-36h from tower top.
22. the as claimed in claim 9 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (3), two
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 200-360m3/h
Flow be pumped into secondary deep demagging tower, lithium leacheate enters tower bottom outflow, total time 30-36h from tower top.
23. the as claimed in claim 13 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step b) in step (3), two
In secondary depth demagging tower, the loading of the Cation adsorption resin is 40.0-50.0 m3；Lithium leacheate is with 200-360m3/h
Flow be pumped into secondary deep demagging tower, lithium leacheate enters tower bottom outflow, total time 30-36h from tower top.
24. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium is female
The lithium ion content of liquid is 2-10g/L.
25. the as claimed in claim 3 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium mother liquor
Lithium ion content be 2-10g/L.
26. the as claimed in claim 4 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium mother liquor
Lithium ion content be 2-10g/L.
27. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium is female
The lithium ion content of liquid is 2-10g/L.
28. the as claimed in claim 3 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium mother liquor
Lithium ion content be 2-10g/L.
29. the as claimed in claim 4 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium mother liquor
Lithium ion content be 2-10g/L.
30. the as claimed in claim 6 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium mother liquor
Lithium ion content be 2-10g/L.
31. the as claimed in claim 9 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium mother liquor
Lithium ion content be 2-10g/L.
32. the as claimed in claim 13 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium mother liquor
Lithium ion content be 2-10g/L.
33. the as claimed in claim 18 kind of old halogen in salt pan proposes lithium method, which is characterized in that in step (4), the high lithium mother liquor
Lithium ion content be 2-10g/L.
34. the as claimed in claim 1 or 2 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (5)
, after the high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, it is heated to 70~90 DEG C.
35. the as claimed in claim 3 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (5), institute
It states after high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, is heated to 70~90 DEG C.
36. the as claimed in claim 4 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (5), institute
It states after high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, is heated to 70~90 DEG C.
37. the as claimed in claim 6 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (5), institute
It states after high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, is heated to 70~90 DEG C.
38. the as claimed in claim 9 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (5), institute
It states after high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, is heated to 70~90 DEG C.
39. the as claimed in claim 13 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (5),
After the high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, it is heated to 70~90 DEG C.
40. the as claimed in claim 18 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (5),
After the high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, it is heated to 70~90 DEG C.
41. the as claimed in claim 24 kind of old halogen in salt pan proposes lithium method, which is characterized in that the sub-step a) in step (5),
After the high lithium mother liquor is pumped into the high lithium mother liquor head tank of purification, it is heated to 70~90 DEG C.
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| CN108298570A (en) * | 2017-12-28 | 2018-07-20 | 核工业北京化工冶金研究院 | The method that absorption method brine proposes demagging in lithium leacheate |
| CN108396159A (en) * | 2018-03-19 | 2018-08-14 | 青海盐湖工业股份有限公司 | Brine refining device and Brine Purification Process in a kind of salt lake bittern magnesium technology |
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| CN106507816B (en) * | 2005-12-30 | 2010-09-08 | 核工业北京化工冶金研究院 | The method for extracting lithium from bittern |
| CN108298570A (en) * | 2017-12-28 | 2018-07-20 | 核工业北京化工冶金研究院 | The method that absorption method brine proposes demagging in lithium leacheate |
| CN108396159A (en) * | 2018-03-19 | 2018-08-14 | 青海盐湖工业股份有限公司 | Brine refining device and Brine Purification Process in a kind of salt lake bittern magnesium technology |
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