CN108314065A - Divide the full membrane separating method that salt produces lithium liquor by salt lake bittern multistage nanofiltration - Google Patents
Divide the full membrane separating method that salt produces lithium liquor by salt lake bittern multistage nanofiltration Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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Abstract
The invention discloses a kind of full membrane separating methods dividing salt production lithium liquor by salt lake bittern multistage nanofiltration, including：(1) salt lake bittern is pre-processed using micro-filtration purification system, removes suspended matter, colloid and other impurities therein, is then diluted with fresh water, obtained micro-filtration and pre-process brine；(2) obtained micro-filtration pretreatment brine is sent into nanofiltration point salt system, separation obtains the filtrate based on monovalent cation and the concentrate based on polyvalent cation；(3) filtrate in step (2) is sent into film concentration systems, is concentrated to give rich lithium concentrate；(4) the rich lithium concentrate for obtaining step (3) is sent into nanofiltration depth demagging system, and lithium liquor is obtained after NF membrane depth demagging.The process energy consumption is low, the rate of recovery is high, production cost is low, continuous controllable, the reliability height of technique, and the lithium liquor Mg/Li ratio produced is low, lithium concentration is high, stable quality, can be used for large-scale production.
Description
Technical field
The invention belongs to technical field of membrane separation, and in particular to a kind of to divide salt production to carry lithium mother by salt lake bittern multistage nanofiltration
The full membrane separation process of liquid.
Background technology
Lithium and its compound play in fields such as the energy, petrochemical industry, metallurgy, ceramics, medicine, aerospace, refrigeration
Extremely important effect is referred to as " energy metal of 21 century ".Salt lake bittern is an important sources of lithium, at present world's lithium
80% or more of salt total output comes from salt lake bittern.
Currently, the main method that salt lake bittern carries lithium has evaporative crystallization partition method, the precipitation method, calcining leaching method, You Jirong
Agent extraction, ion exchange adsorption, electroosmose process, Xu Shi methods and nano filtering process etc., post-processing step generally clean, concentration,
Precipitation etc..Carrying the concentration of lithium and Mg/Li ratio in pre-treating technology, product quality and the economic benefit, with brine of lithium has prodigious pass
System.Low lithium concentration and high Mg/Li ratio all can seriously limit the process combination mode that brine carries lithium, influence its feasibility and economic effect
Benefit.Nano filtering process can efficiently separate monovalent ion and multivalent ion, but conventional nanofiltration system is to the very high salt lake halogen of salt content
Water could be handled after diluting more times.
Application No. is 201310571755.2 Chinese patent applications to disclose through nanofiltration system separation magnesium ion and lithium
Ion, counter-infiltration system are enriched with lithium ion, and salt pan is concentrated by evaporation, and lithium concentration can be made to reach dense needed for prepared calcium carbonate lithium
Degree；However the series of the nanofiltration system of this application design is only level-one, separating magnesium and lithium ability is limited, at the brine of high Mg/Li ratio
Manage it is ineffective, have certain limitation；In addition, it is further dense to still need to time-consuming longer salt pan evaporation after reverse osmosis concentration
Contracting, just can make lithium concentration reach the requirement for producing lithium carbonate.Application No. is 201610751304.0 Chinese patent applications
Open indicate can concentrate lithium-containing solution using positive osmosis system, be enriched with lithium ion, however due to the magnesium of level-one nanofiltration system
Lithium concentration is limited in ion remaval effect and production water, still needs to that alkali depth demagging is added after positive osmosis concentration, and pass through high energy
The multiple-effect evaporation of consumption further concentrates refined lithium-containing solution, improves lithium concentration；And positive osmosis system uses bicarbonate
Ammonium salt solution fails to gather materials on the spot as liquid is drawn, and salt pan is made full use of to ted the salt of gained.
China's salt lake bittern is mostly sulfate type and chloride type, has lithium content height and high two of Mg/Li ratio significant special
Therefore how point cost-effectively utilizes salt lake bittern to prepare the lithium salts of high-purity, becomes China's saline lake lithium resource and develop and use
Key.
Invention content
In view of the above technical problems, salt is divided to produce lithium liquor by salt lake bittern multistage nanofiltration the present invention provides a kind of
Full membrane separation process makes full use of the respective advantage of microfiltration membranes, NF membrane, reverse osmosis membrane, forward osmosis membrane, according to brine water quality,
Reasonable disposition is carried out to the sum of series membrane module of nanofiltration system, magnesium ion can be effectively removed, solve Separation of Li and Mg problem in brine,
And nanofiltration filtrate is concentrated by energy consumption extremely low positive osmosis system, the lithium concentration in solution is improved, is carried
Lithium mother liquor.The process energy consumption is low, the rate of recovery is high, production cost is low, continuous controllable, the reliability height of technique, the lithium liquor produced
Mg/Li ratio is low, lithium concentration is high, stable quality, can be used for large-scale production.
The present invention is realized by following technical proposals.
It is a kind of to divide the full membrane separating method that salt produces lithium liquor by salt lake bittern multistage nanofiltration, include the following steps：
(1) salt lake bittern is pre-processed using micro-filtration purification system, removes suspended matter therein, colloid and other is miscellaneous
Then matter dilutes 2~5 times with fresh water, obtain micro-filtration and pre-process brine；
(2) the micro-filtration pretreatment brine obtained step (1) is sent into multistage nanofiltration point salt system, and separation micro-filtration pre-processes halogen
Polyvalent cation in water and part monovalent cation obtain filtrate based on monovalent cation and based on polyvalent cation
Concentrate；
(3) filtrate in step (2) is sent into film concentration systems, is concentrated to give rich lithium concentrate；
(4) the rich lithium concentrate for obtaining step (3) is sent into nanofiltration depth demagging system, after NF membrane depth demagging
To lithium liquor.
Further, in the step (1), the Mg/Li ratio of salt lake bittern is calculated as (10~1000) in mass ratio:1, lithium ion
Mass concentration be 0.1~5g/L, pH value be 5~7.5.
Further, in the step (1), the series of micro-filtration purification system is 1~2 grade, be 1~5 μm by filtering accuracy,
One or both of 0.45~1 μm or 0.1~0.45 μm is composed successively by pore size.
Further, the micro-filtration membrane material of the micro-filtration purification system is ceramics, polypropylene, makrolon, polyvinyl chloride, gathers
It is one or more in sulfone, Kynoar or polytetrafluoroethylene (PTFE).
Further, in the step (2), multistage nanofiltration divides the series of salt system to be 1~3 grade；First order nanofiltration divides salt system
System uses DT NF membranes, and the rejection to magnesium sulfate is 70~95%, and the rejection to sodium chloride is 1-5%, operating pressure
For 3~6MPa, the rate of recovery is 50~70%.
Further, the second level and third level nanofiltration divide salt system to use one kind in rolled film, tubular membrane or plate membrane,
It is 90~98% to the rejection of magnesium sulfate, and the rejection to sodium chloride is 5~10%, and operating pressure is 0.8~4MPa, is returned
Yield is 60~80%, and filter type is cross-flow filtration.
Further, nanofiltration divides salt system that internal circulation pattern, i.e., nanofiltrations at different levels is used to divide one in the concentrate of salt system
It is partly refluxed in the liquid pool of this grade of nanofiltration point salt system and is recycled, wherein primary concentration liquid cools down before reflux, promotes
The inorganic salt loading in part is precipitated, and reduces the salt content of concentrate, is sent into the liquid pool that first order nanofiltration divides salt system after filtering
In；Arrange outside another part primary concentration liquid otherwise utilized, remaining two level and three-level concentrate are back to the first order and the respectively
Two level nanofiltration divides in the liquid pool of salt system.
Further, the film concentration systems be by positive osmosis system, or positive osmosis system and counter-infiltration system combination system
System is constituted；Reverse osmosis filtrate and primary rich lithium concentrate can be obtained from counter-infiltration system, it is dense to can get rich lithium from positive osmosis system
Contracting liquid；Reverse osmosis filtrate flows back into the fresh water dilution system of micro-filtration purification system, and brine is pre-processed to prepare micro-filtration.
Further, the series of the nanofiltration depth demagging system is 1~2 grade, and using complete alternation pattern, i.e., concentrated waters at different levels are complete
Portion is back in the liquid pool of this grade of nanofiltration point salt system and is recycled；Use one in rolled film, tubular membrane or plate membrane
Kind, it is 90~99% to the rejection of magnesium sulfate, the rejection to sodium chloride is 5~10%, operating pressure is 0.8~
3MPa, the rate of recovery are 60~80%, and filter type is cross-flow filtration.
Further, the nanofiltration of the step (2) divides the nanofiltration depth demagging system of salt system and step (4) to use rolling
Monovalent ion is selected selectively to penetrate NF membrane in film, tubular membrane or plate membrane, nanofiltration membrane material is aromatic polyamides, gathers
It is one or more in piperazine amide, polyimides or sulfonated polysulfone.
It advantages of the present invention and has the beneficial effect that：
(1) present invention selects micro-filtration, nanofiltration, reverse osmosis and positive infiltration system using low consumption, efficient membrane separation process as core
System and it is high pressure resistant, dividing salt drop magnesium efficiency higher DT nanofiltration systems in high salt concentration, (DT nanofiltration systems contain suitable for high concentration
Brine, and need not big multiple dilution brine or do not dilute use in the case of brine).Different combinations can be carried out according to water quality and is matched
It sets, flexible design, the salt lake bittern water quality that can be handled is wide in range, and application is strong, can be to the salt of different lithium concentrations and Mg/Li ratio
Lake bittern water carries out the enrichment method of separating magnesium and lithium and lithium.
(2) full membrane separation process of the invention effectively prevents being concentrated by evaporation in production, precipitates the traditional handicrafts such as salt reduction
The deficiency big to equipment corrosion, environmental pollution is serious, operating cost is high etc. is ensureing the higher enrichment degree of lithium ion and is returning
While yield, production cost is reduced.
(3) full membrane separation process operation and maintenance of the invention are convenient, and membranous system is easy to configuration, cleaning, installation and transhipment, has
Conducive to popularization and application, large-scale production is carried out.
(4) full membrane separation process of the invention substantially effectively utilizes resource, wherein：Positive osmosis system is drawn
Liquid is taken, can be that salt lake bittern, the nanofiltration of removal mechanical admixture divide the primary concentration liquid arranged outside salt system or salt lake bittern to ted
The solution that the inorganic salts produced are prepared is used as and draws liquid；If it is the salt lake bittern for removing mechanical admixture to draw liquid, after use
Nanofiltration point salt system can be still sent into utilize again；Reverse osmosis filtrate is reflowable to arrive technique front end, the fresh water used as dilution,
It is effectively saved the extremely rare fresh water in area with high salt.Technology adaptation to local conditions, gathers materials on the spot, and has both saved production cost,
Carrying capacity of environment is dramatically reduced again, it is efficient, energy saving.
(5) nanofiltration of the invention divides salt system, film concentration systems, and drop magnesium is efficient, and cycles of concentration is big, with traditional handicraft phase
Than the Mg/Li ratio (counting in mass ratio) of brine can be greatly reduced, improve lithium concentration, avoid alkaline process demagging, removing impurity by means of precipitation
Etc. complicated processes, greatly reduce the loss of lithium resource.
(6) water-loop heat pump system of the invention will be turned by heat exchanger after the heat absorption in the primary concentration liquid of reflux
Full membrane separation process front end is moved on to, the temperature of brine is pre-processed for promoting micro-filtration, is conducive to the solubility for increasing inorganic salts, keeps away
Exempt from temperature it is relatively low when concentrate in inorganic salts supersaturation be precipitated the problem of.
Description of the drawings
Fig. 1 is illustrated according to a kind of method flow for the full membrane separation process producing lithium liquor by salt lake bittern of the present invention
Figure.
Fig. 2 is the technique of the 1 full membrane separation process that lithium liquor is produced by salt lake bittern according to an embodiment of the invention
Flow diagram.
Fig. 3 is the technique of the 2 full membrane separation process that lithium liquor is produced by salt lake bittern according to an embodiment of the invention
Flow diagram.
Fig. 4 is the technique of the 3 full membrane separation process that lithium liquor is produced by salt lake bittern according to an embodiment of the invention
Flow diagram.
Fig. 5 is the technique of the 4 full membrane separation process that lithium liquor is produced by salt lake bittern according to an embodiment of the invention
Flow diagram.
Specific implementation mode
With reference to embodiment, the invention will be described in further detail, but be not intended as to invention do any restrictions according to
According to.
Fig. 1 gives the flow diagram of the method for the present invention.The present invention divides salt production to carry lithium mother by salt lake bittern multistage nanofiltration
There are many embodiments for the full membrane separation process of liquid, include the following steps：
(1) salt lake bittern is pre-processed using micro-filtration purification system, removes suspended matter therein, colloid and other is miscellaneous
Then matter dilutes 2~5 times with fresh water, obtain micro-filtration and pre-process brine.
Wherein, the Mg/Li ratio of salt lake bittern is calculated as (10~1000) in mass ratio:1, the mass concentration of lithium ion is 0.1~
5g/L, pH value are 5~7.5.
The series of micro-filtration purification system is 1~2 grade, is 1~5 μm, 0.45~1 μm or 0.1~0.45 μm by filtering accuracy
One or both of be composed successively by pore size；The micro-filtration membrane material of micro-filtration purification system is ceramics, polypropylene, gathers
It is one or more in carbonic ester, polyvinyl chloride, polysulfones, Kynoar or polytetrafluoroethylene (PTFE).
(2) the micro-filtration pretreatment brine obtained step (1) is sent into multistage nanofiltration point salt system, and separation micro-filtration pre-processes halogen
Polyvalent cation in water and part monovalent cation obtain filtrate based on monovalent cation and based on polyvalent cation
Concentrate.
Wherein, nanofiltration divides the series of salt system to be 1~3 grade；First order nanofiltration divides salt system to use DT NF membranes, to sulphur
The rejection of sour magnesium is 70~95%, and the rejection to sodium chloride is 1~5%, and operating pressure is 3~6MPa, the rate of recovery 50
~70%；The second level and third level nanofiltration divide salt system using one kind in rolled film, tubular membrane or plate membrane, to sulfuric acid
The rejection of magnesium is 90~98%, and the rejection to sodium chloride is 5~10%, and operating pressure is 0.8~4MPa, the rate of recovery 60
~80%, filter type is cross-flow filtration.
Nanofiltration divides salt system that internal circulation pattern, i.e., nanofiltrations at different levels is used to divide the part reflux in the concentrate of salt system
To being recycled in the liquid pool of this grade of nanofiltration point salt system, wherein primary concentration liquid cools down before reflux, passes through coolant water temperature
Degree is realized for 5~10 DEG C of water-loop heat pump system, promotes the inorganic salt loading in part to be precipitated, reduces the salt content of concentrate, passes through
First order nanofiltration is sent into after filter to divide in the liquid pool of salt system；Water-loop heat pump system is using mechanical On Line Foul Removing Technology technology, in its heat
It is equipped with moveable nylon bruss on exchanger, removes the inorganic salts deposited on exchanger coil pipe；The heat of water-loop heat pump system simultaneously
Source is used to improve the temperature of micro-filtration pretreatment brine.Otherwise utilized, remaining two level and three is arranged outside another part primary concentration liquid
Grade concentrate is back to respectively in the liquid pool of the first order and second level nanofiltration point salt system.
Nanofiltration divides salt system selectively to penetrate NF membrane using monovalent ion, and nanofiltration membrane material is aromatic polyamides, poly- piperazine
It is one or more in carboxamide dihydrochloride, polyimides or sulfonated polysulfone.
(3) filtrate in step (2) is sent into film concentration systems, is concentrated to give rich lithium concentrate.
Wherein, film concentration systems are by positive osmosis system, or the combined system of positive osmosis system and counter-infiltration system is constituted；
Reverse osmosis filtrate and primary rich lithium concentrate can be obtained from counter-infiltration system, can get rich lithium concentrate from positive osmosis system；Instead
Infiltration filtrate flows back into the fresh water dilution system of micro-filtration purification system, and brine is pre-processed to prepare micro-filtration.
Positive osmosis system draw liquid be the salt lake bittern for removing mechanical admixture, outside nanofiltration point salt system row primary concentration
Liquid or salt lake bittern ted one or more be configured to solution in the sodium chloride, bischofite, magnesium sulfate produced；When
It is that will draw liquid when removing the salt lake bittern of mechanical admixture after positive osmosis system work and pre-process brine with micro-filtration to draw liquid
Merge, is sent into nanofiltration after mixing and divides salt system.
The kit form for the forward osmosis membrane that positive osmosis system uses is one kind in tablet, rolling or doughnut；Just ooze
The material of permeable membrane is one kind in Triafol T, polybenzimidazoles, polyacrylonitrile, polysulfones or polyether sulfone.
It when the operating pressure of counter-infiltration system is 4-6MPa, is concentrated using single-stage, filter type is cross-flow filtration, and salt is cut
Rate is stayed to reach 97-98%, the rate of recovery is 60~80%；It is aromatic polyamides, poly- piperazine acyl that the component of reverse osmosis membrane, which uses rolling, matter,
It is one or more in amine, polyimides or sulfonated polysulfone.
(4) the rich lithium concentrate for obtaining step (3) is sent into nanofiltration depth demagging system, after NF membrane depth demagging
To lithium liquor.
The series of nanofiltration depth demagging system is 1~2 grade, and using complete alternation pattern, i.e., concentrated waters at different levels are all back to this
It is recycled in the liquid pool of grade nanofiltration point salt system；Using one kind in rolled film, tubular membrane or plate membrane, to sulfuric acid
The rejection of magnesium is 90~99%, and the rejection to sodium chloride is 5~10%, and operating pressure is 0.8~3MPa, the rate of recovery 60
~80%, filter type is cross-flow filtration；NF membrane is selectively penetrated using monovalent ion, nanofiltration membrane material is fragrant polyamides
It is one or more in amine, polypiperazine-amide, polyimides or sulfonated polysulfone.
The mass concentration of lithium ion is 20~40g/L in the lithium liquor of acquisition, and Mg/Li ratio (counting in mass ratio) is less than
0.2。
It is further illustrated the present invention with reference to specific embodiment.
Embodiment 1：
As shown in Fig. 2, the present embodiment selects three-level grade nanofiltration to divide salt system, just infiltration and counter-infiltration system and nanofiltration
Depth demagging system.Include the following steps：
(1) to utilize micro-filtration purification system be 115.10g/L to the mass concentration of pH=5, magnesium ion, the quality of lithium ion is dense
It spends for 0.384g/L, Mg/Li ratio (counting in mass ratio) 300：1 salt lake bittern is pre-processed, and suspended matter therein, glue are removed
Then body and other impurities dilute 2.5 times with fresh water, obtain micro-filtration and pre-process brine.
Wherein, micro-filtration purification system is composed of successively two microfiltration systems that filtering accuracy is 3 μm and 0.22 μm, micro-
The material of filter membrane is followed successively by makrolon and polysulfones.
(2) being sent into the micro-filtration pretreatment brine that step (1) obtains, there is three-level nanofiltration point salt system to handle, by two
Valence magnesium ion is detached with monovalence lithium ion, obtains the more higher concentrate of filtrate and magnesium ion content of lithium ion content.
Three-level nanofiltration divides salt system all to use monovalent ion selectively transmission, the NF membrane of multivalent ion preferential rejection, choosing
Select aromatic polyamide nanofiltration membrane.In the present embodiment, first order nanofiltration divides salt system to use DT NF membranes, is cut to magnesium sulfate
It is 70% to stay rate, and the rejection to sodium chloride is 3%, operating pressure 5MPa, the rate of recovery 70%；The second level and the third level receive
Filter divides salt system to use rolling NF membrane, and the rejection to magnesium sulfate is 90%, and the rejection to sodium chloride is 7%, operation
Pressure is respectively 2MPa and 1.5MPa, the rate of recovery 80%, by the way of cross-flow filtration.
Corresponding filtrate and concentrate can be generated per level-one nanofiltration point salt system, level-one filtrate and two level filtrate are all sent into
Next stage nanofiltration divides in the liquid pool of salt system, and the part in concentrates at different levels is back to the stoste of this grade of nanofiltration point salt system
It is recycled in pond.Meanwhile being arranged outside another part primary concentration liquid, remaining two level, three-level concentrate are back to first respectively
Grade, second level nanofiltration divide in the liquid pool of salt system.The Mg/Li ratio (counting in mass ratio) of three-level filtrate reaches 1.1:1, lithium ion
Concentration reaches 0.321g/L.
The water-loop heat pump system that primary concentration liquid is 5 DEG C by cooling water temperature before reflux carries out cooling processing, makes sulphur
The inorganic salt loading such as sour potassium, sodium sulphate is precipitated, and reduces the salt content of concentrate, is sent into first order nanofiltration after filtering and divides salt system
Liquid pool in.
Water-loop heat pump system is equipped with moveable nylon bruss on its heat exchanger, is gone using mechanical On Line Foul Removing Technology technology
Except the inorganic salts deposited on exchanger coil pipe；The heat source of water-loop heat pump system can be used for improving the temperature of micro-filtration pretreatment brine simultaneously
Degree.
(3) the three-level filtrate in step (2) is sent into counter-infiltration system to concentrate, obtains reverse osmosis filtrate and primary is rich
Lithium concentrate；Then the rich lithium concentrate of the primary of acquisition is re-fed into positive osmosis system, carries out concentration, obtain rich lithium concentration
Liquid.
The operating pressure of counter-infiltration system is 4MPa, and the rejection of salt selects rolling reverse osmosis in the present embodiment up to 97%
Permeable membrane, matter are aromatic polyamides.The fresh water dilution system that the reverse osmosis filtrate of gained is flowed back into micro-filtration purification system, to prepare
Micro-filtration pre-processes brine.The forward osmosis membrane kit form that positive osmosis system uses is TFC plate membranes, and the material of forward osmosis membrane is poly-
Sulfone and polyether sulfone；It is the salt lake bittern for removing mechanical admixture to draw liquid.Liquid and micro-filtration will be drawn after positive osmosis system work
It pre-processes brine to merge, is sent into nanofiltration after mixing and divides salt system.
(4) the rich lithium concentrate for obtaining step (3) is sent into level-one nanofiltration depth demagging system, through NF membrane depth demagging
After obtain lithium liquor.
Level-one nanofiltration depth demagging system uses complete alternation pattern, i.e. level-one concentrated water to be all back to nanofiltration depth demagging system
It is recycled in the liquid pool of system；Monovalent ion is selected selectively to penetrate, the NF membrane of multivalent ion preferential rejection.In this implementation
In example, it is aromatic polyamides that level-one nanofiltration depth demagging system, which uses rolling NF membrane, nanofiltration membrane material, is cut to magnesium sulfate
It is 90% to stay rate, and the rejection to sodium chloride is 8%, operating pressure 2.5MPa, the rate of recovery 75%, using cross-flow filtration
Mode.
The mass concentration of magnesium ion is 30.448g/L in lithium liquor in the present embodiment, the mass concentration of lithium ion is
29.890g/L, Mg/Li ratio (in mass ratio count) are up to 0.12：1.Lithium concentration is 77.8 times of salt lake bittern.
The ingredient for carrying each stage brine during lithium in the present embodiment using salt lake bittern is shown in Table 1：
The component list (g/L) of each stage brine in 1 embodiment 1 of table
| Type | Mg2+ | Li+ | Mg2+/Li+ |
| Salt lake bittern | 115.10 | 0.384 | 300:1 |
| Micro-filtration pre-processes brine | 46.04 | 0.154 | 300:1 |
| Level-one filtrate | 19.73 | 0.193 | 102:1 |
| Primary concentration liquid | 107.43 | 0.063 | 1249:1 |
| Two level filtrate | 2.865 | 0.248 | 11.6:1 |
| Three-level filtrate | 0.361 | 0.321 | 1.1:1 |
| Primary richness lithium concentrate | 2.694 | 2.395 | 1.1:1 |
| Rich lithium concentrate | 25.863 | 22.992 | 1.1:1 |
| Lithium liquor | 30.448 | 29.890 | 0.12:1 |
| Level-one concentrated water | 93.107 | 2.293 | 40.6:1 |
Embodiment 2：
As shown in figure 3, the present embodiment selects two-stage nanofiltration to divide salt system, the nanofiltration than embodiment 1 divides salt system few level-one,
In addition to following differences, other parts are the same as embodiment 1.In the present embodiment：
(1) salt lake bittern pH is 6.4, the mass concentration of magnesium ion is 51.75g/L, the mass concentration of lithium ion is
0.535g/L, Mg/Li ratio (counting in mass ratio) 100：1, salt lake bittern dilutes 5 times, and micro-filtration purification system is 1 μm by filtering accuracy
Two microfiltration systems with 0.1 μm are composed successively, and the material of microfiltration membranes is followed successively by polypropylene and Kynoar.
(2) the present embodiment selects two-stage nanofiltration to divide salt system, and first order nanofiltration divides salt system to use DT NF membranes, to sulphur
The rejection of sour magnesium is 95%, and the rejection to sodium chloride is 5%, operating pressure 3MPa, the rate of recovery 65%；It receives the second level
Filter divides salt system to use tubular nanofiltration membrane, and the rejection to magnesium sulfate is 98%, and the rejection to sodium chloride is 10%, operation
Pressure is 4MPa, the rate of recovery 75%.Nanofiltration membrane material is polypiperazine-amide, and two level filtrate Mg/Li ratio (counting in mass ratio) reaches
0.53:1, lithium concentration reaches 0.188g/L.
(3) operating pressure of counter-infiltration system is 4.5MPa in the present embodiment, and it is poly- piperazine to select coiled reverse osmosis membrane, matter
Amide.Forward osmosis membrane is rolled film, and the material of forward osmosis membrane is Triafol T, and the water chlorine produced is tedded using salt lake bittern
The solution that magnesite compound concentration is 4mol/L, which is used as, draws liquid.
(4) it is poly- piperazine acyl that level-one nanofiltration depth demagging system, which uses tubular nanofiltration membrane, nanofiltration membrane material, in the present embodiment
Amine, the rejection to magnesium sulfate are 99%, and the rejection to sodium chloride is 10%, operating pressure 3MPa, and the rate of recovery is
60%.
The ingredient for carrying each stage brine during lithium in the present embodiment using salt lake bittern is shown in Table 2；In lithium liquor lithium from
The mass concentration of son is 16.233g/L, Mg/Li ratio (in mass ratio count) is up to 0.53：1, the mass concentration of lithium ion is salt lake bittern
30.34 times.
The component list (g/L) of each stage brine in 2 embodiment 2 of table
| Type | Mg2+ | Li+ | Mg2+/Li+ |
| Salt lake bittern | 51.75 | 0.535 | 100:1 |
| Micro-filtration pre-processes brine | 10.35 | 0.107 | 100:1 |
| Level-one filtrate | 1.479 | 0.139 | 10.6:1 |
| Primary concentration liquid | 28.093 | 0.048 | 585.3:1 |
| Two level filtrate | 0.099 | 0.188 | 0.53:1 |
| Primary richness lithium concentrate | 0.961 | 1.824 | 0.53:1 |
| Rich lithium concentrate | 8.553 | 16.233 | 0.53:1 |
| Lithium liquor | 1.426 | 20.129 | 0.071:1 |
Embodiment 3：
As shown in figure 4, the present embodiment selects two-stage nanofiltration depth demagging system, than the nanofiltration depth demagging system of embodiment 1
It unites more level-ones, in addition to following differences, other parts are the same as embodiment 1.
(1) in the present embodiment, salt lake bittern pH is 5.7, the mass concentration of magnesium ion is 101.18g/L, lithium ion
Mass concentration is 0.102g/L, dilutes 2 times, two microfiltration systems that micro-filtration purification system is 1 μm and 0.22 μm by filtering accuracy
It is composed successively, the material of microfiltration membranes is followed successively by polypropylene and polytetrafluoroethylene (PTFE).
(2) in the present embodiment, first order nanofiltration divides salt system using DT NF membranes, and the rejection to magnesium sulfate is
95%, the rejection to sodium chloride is 1%, and operating pressure 6MPa, the rate of recovery 55%, the second level and third level nanofiltration divide salt
It is aromatic polyamides that system, which uses board-like NF membrane, nanofiltration membrane material,；It is 95% to the rejection of magnesium sulfate, to sodium chloride
Rejection is 5%, and operating pressure is respectively 2MPa and 1.5MPa, the rate of recovery 60%.Three-level filtrate Mg/Li ratio is counted in mass ratio
Reach 5.5:1, lithium concentration reaches 0.118g/L.
(3) operating pressure of counter-infiltration system is 5MPa in the present embodiment, and up to 98%, positive osmosis system makes the rejection of salt
It is the primary concentration liquid arranged outside nanofiltration point salt system to draw liquid.Positive osmosis system uses doughnut forward osmosis membrane；Just ooze
The material of permeable membrane is polybenzimidazoles.
(4) in the present embodiment, two-stage nanofiltration depth demagging system all uses complete alternation pattern, the first order and second level nanofiltration
Depth demagging system uses rolling NF membrane, and the rejection to magnesium sulfate is 95%, and the rejection to sodium chloride is 5%,
Operating pressure is respectively 2.5MPa and 1.5MPa, the rate of recovery 80%.
The ingredient for carrying each stage brine during lithium in the present embodiment using salt lake bittern is shown in Table 3；In lithium liquor lithium from
A concentration of 17.701g/L of son, lithium ion mass concentration are 173.5 times of salt lake bittern, Mg/Li ratio (counting in mass ratio) is by 1000：
1 is down to 0.06：1.
The component list (g/L) of each stage brine in 3 embodiment 3 of table
| Type | Mg2+ | Li+ | Mg2+/Li+ |
| Salt lake bittern | 101.18 | 0.102 | 1000:1 |
| Micro-filtration pre-processes brine | 50.59 | 0.051 | 1000:1 |
| Level-one filtrate | 27.591 | 0.066 | 418:1 |
| Primary concentration liquid | 78.698 | 0.033 | 2385:1 |
| Two level filtrate | 4.245 | 0.088 | 48:1 |
| Three-level filtrate | 0.654 | 0.118 | 5.5:1 |
| Primary richness lithium concentrate | 6.961 | 1.256 | 5.5:1 |
| Rich lithium concentrate | 68.217 | 12.302 | 5.5:1 |
| Level-one produces water | 8.527 | 14.753 | 0.578:1 |
| Lithium liquor | 1.065 | 17.701 | 0.06:1 |
Embodiment 4：
As shown in figure 5, the present embodiment selects level-one nanofiltration to divide salt system, only with positive osmosis system and level-one nanofiltration depth
Demagging system.In the present embodiment：
(1) utilize micro-filtration purification system to pH=7.5, lithium ion mass concentration be 2.390g/L, Mg/Li ratio (in mass ratio
Meter) up to 10：1 salt lake bittern is pre-processed, and then dilutes 2 times with fresh water, is obtained micro-filtration and is pre-processed brine.
Micro-filtration purification system is composed of successively two microfiltration systems that filtering accuracy is 0.45 μm and 0.1 μm, micro-filtration
The material of film is followed successively by polyvinyl chloride and ceramics.
(2) micro-filtration that step (1) obtains pretreatment brine level-one nanofiltration point salt system is sent into handle, obtain lithium from
The more level-one filtrate of sub- content and the higher primary concentration liquid of magnesium ion content.
Level-one nanofiltration divides salt system to use monovalent ion selectively transmission, the NF membrane of multivalent ion preferential rejection.
In the present embodiment, it is polyimides and sulfonation that level-one nanofiltration, which divides salt system to use DT NF membranes, nanofiltration membrane material,
Polysulfones；It is 85% to the rejection of magnesium sulfate, and the rejection to sodium chloride is 3%, operating pressure 5MPa, and the rate of recovery is
70%.DT nanofiltrations Mg/Li ratio (counting in mass ratio) reaches 0.75:1, lithium concentration reaches 2.436g/L.
A part in primary concentration liquid is back in the liquid pool of nanofiltration point salt system and is recycled, meanwhile, another portion
Divide outside primary concentration liquid and arranges.
Primary concentration liquid is cooled down before reflux by water-loop heat pump system, actual conditions and operation and water-loop heat pump system with
Embodiment 1 is identical.
(3) the level-one filtrate in step (2) is sent into positive osmosis system, carries out concentration, obtains rich lithium concentrate.
The forward osmosis membrane that the positive osmosis system uses is CTA plate membranes, and it is the salt lake halogen for removing mechanical admixture to draw liquid
Water teds the solution for a concentration of 4mol/L that the sodium chloride produced and magnesium sulfate are configured to.It will after positive osmosis system work
It draws liquid with micro-filtration pretreatment brine to merge, is sent into nanofiltration after mixing and divides salt system.
(4) the rich lithium concentrate for obtaining step (3) is sent into level-one nanofiltration depth demagging system, through NF membrane depth demagging
After obtain lithium liquor.
The level-one nanofiltration depth demagging system uses complete alternation pattern；Select monovalent ion selectively penetrate, multivalence from
The NF membrane of sub- preferential rejection.In the present embodiment, level-one nanofiltration depth demagging system uses rolling NF membrane, to magnesium sulfate
Rejection be 98%, be 9% to the rejection of sodium chloride, operating pressure 0.8MPa, the rate of recovery 70%, using cross-flow
The mode of filter.
The ingredient for carrying each stage brine during lithium in the present embodiment using salt lake bittern is shown in Table 3；Lithium in lithium liquor
A concentration of 22.922g/L of mass of ion, lithium ion mass concentration be 9.59 times of salt lake bittern, Mg/Li ratio (counting in mass ratio) by
10：1 is down to 0.032：1.
The component list (g/L) of each stage brine in 4 embodiment 4 of table
| Type | Mg2+ | Li+ | Mg2+/Li+ |
| Salt lake bittern | 24.62 | 2.390 | 10:1 |
| Micro-filtration pre-processes brine | 12.31 | 1.195 | 10:1 |
| Level-one filtrate | 0.879 | 1.554 | 0.57:1 |
| Primary concentration liquid | 38.982 | 0.357 | 109:1 |
| Rich lithium concentrate | 10.988 | 19.425 | 0.57:1 |
| Lithium liquor | 0.733 | 22.922 | 0.032:1 |
From above-described embodiment as can be seen that dividing salt to carry out salt lake bittern by multistage nanofiltration using the present invention produces lithium liquor
The lithium liquor produced of full membrane separating method：For low lithium high-magnesium brine, lithium concentration is increased to from 0.102g/L
17.701g/L, 173.5 times are improved, Mg/Li ratio is counted in mass ratio by 1000:1 drops to 0.06:1；For the lower halogen of Mg/Li ratio
Water, lithium concentration are increased to 22.922g/L from 2.390g/L, improve 9.59 times, and Mg/Li ratio is counted in mass ratio by 10:1 drops to
0.032:1；It is processed suitable for further lithium product.It can thus be seen that the lithium liquor prepared by the present invention not only has
Lower Mg/Li ratio is provided simultaneously with higher lithium concentration, is that low energy consumption, the rate of recovery is high, production cost is low, technique connects for one kind
Continuous full membrane separating method controllable, reliability is high.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.
Claims (10)
1. it is a kind of by salt lake bittern multistage nanofiltration divide salt produce lithium liquor full membrane separating method, which is characterized in that including with
Lower step：
(1) salt lake bittern is pre-processed using micro-filtration purification system, removes suspended matter, colloid and other impurities therein,
Then 2~5 times are diluted with fresh water, obtains micro-filtration and pre-processes brine；
(2) the micro-filtration pretreatment brine obtained step (1) is sent into multistage nanofiltration point salt system, and separation micro-filtration pre-processes in brine
Polyvalent cation and part monovalent cation, obtain filtrate based on monovalent cation and dense based on polyvalent cation
Contracting liquid；
(3) filtrate in step (2) is sent into film concentration systems, is concentrated to give rich lithium concentrate；
(4) the rich lithium concentrate for obtaining step (3) is sent into nanofiltration depth demagging system, is carried after NF membrane depth demagging
Lithium mother liquor.
2. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 1
Method, which is characterized in that in the step (1), the Mg/Li ratio of salt lake bittern is calculated as (10~1000) in mass ratio:1, lithium ion
Mass concentration is 0.1~5g/L, and pH value is 5~7.5.
3. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 1
Method, which is characterized in that in the step (1), the series of micro-filtration purification system is 1~2 grade, be 1~5 μm by filtering accuracy,
One or both of 0.45~1 μm or 0.1~0.45 μm is composed successively by pore size.
4. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 3
Method, which is characterized in that the micro-filtration membrane material of the micro-filtration purification system is ceramics, polypropylene, makrolon, polyvinyl chloride, gathers
It is one or more in sulfone, Kynoar or polytetrafluoroethylene (PTFE).
5. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 1
Method, which is characterized in that in the step (2), multistage nanofiltration divides the series of salt system to be 1~3 grade；First order nanofiltration divides salt system
It is 70~95%% to the magnesium sulfate rejection rate in high bittern water using DT NF membranes, the rejection to sodium chloride is 1~
5%, operating pressure is 3~6MPa, and the rate of recovery is 50~70%.
6. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 5
Method, which is characterized in that the second level and third level nanofiltration divide salt system to use one kind in rolled film, tubular membrane or plate membrane,
It is 90~98% to the rejection of magnesium sulfate, and the rejection to sodium chloride is 5~10%, and operating pressure is 0.8~4MPa, is returned
Yield is 60~80%, and filter type is cross-flow filtration.
7. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 6
Method, which is characterized in that nanofiltration divides salt system that internal circulation pattern, i.e., nanofiltrations at different levels is used to divide one in the concentrate of salt system
Divide to be back in the liquid pool of this grade of nanofiltration point salt system and be recycled, wherein primary concentration liquid cools down before reflux, promotes portion
Divide inorganic salt loading to be precipitated, reduce the salt content of concentrate, is sent into first order nanofiltration after filtering and divides in the liquid pool of salt system；
Arrange outside another part primary concentration liquid otherwise utilized, remaining two level and three-level concentrate are back to the first order and the second level respectively
Nanofiltration divides in the liquid pool of salt system.
8. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 1
Method, which is characterized in that the film concentration systems be by positive osmosis system, or positive osmosis system and counter-infiltration system combined system
It constitutes；Reverse osmosis filtrate and primary rich lithium concentrate can be obtained from counter-infiltration system, can get rich lithium concentration from positive osmosis system
Liquid；Reverse osmosis filtrate flows back into the fresh water dilution system of micro-filtration purification system, and brine is pre-processed to prepare micro-filtration.
9. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 1
Method, which is characterized in that the series of the nanofiltration depth demagging system is 1~2 grade, and using complete alternation pattern, i.e., concentrated waters at different levels are complete
Portion is back in the liquid pool of this grade of nanofiltration point salt system and is recycled；Use one in rolled film, tubular membrane or plate membrane
Kind, it is 90~99% to the rejection of magnesium sulfate, the rejection to sodium chloride is 5~10%, operating pressure is 0.8~
3MPa, the rate of recovery are 60~80%, and filter type is cross-flow filtration.
10. a kind of full UF membrane side dividing salt production lithium liquor by salt lake bittern multistage nanofiltration according to claim 1
Method, which is characterized in that the nanofiltration of the step (2) divide the nanofiltration depth demagging system of salt system and step (4) using rolled film,
Monovalent ion is selected selectively to penetrate NF membrane in tubular membrane or plate membrane, nanofiltration membrane material is aromatic polyamides, poly- piperazine
It is one or more in carboxamide dihydrochloride, polyimides or sulfonated polysulfone.
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