CN114870633B - Process for enriching lithium in salt lake brine - Google Patents
Process for enriching lithium in salt lake brine Download PDFInfo
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- CN114870633B CN114870633B CN202210536999.6A CN202210536999A CN114870633B CN 114870633 B CN114870633 B CN 114870633B CN 202210536999 A CN202210536999 A CN 202210536999A CN 114870633 B CN114870633 B CN 114870633B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention belongs to the technical field of solution purification and separation, and discloses a process for enriching lithium in salt lake brine. After pretreatment, the salt lake brine respectively passes through an adsorption device, an ultrafiltration device, a primary nanofiltration device, a reverse osmosis device I, a secondary nanofiltration device and an electrodialysis device to obtain a solution which can be directly used for preparing high-purity lithium. In order to reduce the pressure difference between two sides of the reverse osmosis membrane and improve the recovery rate of lithium ions, the electrodialysis produced water is sent to a reverse osmosis device I and is mixed with the reverse osmosis produced water I to be used as the rear-end outlet water of the reverse osmosis device I; and (3) setting an independent reverse osmosis device II to concentrate the water discharged from the rear end of the reverse osmosis device I, mixing the reverse osmosis concentrated water II with the secondary nanofiltration produced water, and feeding the mixture into the electrodialysis device. The enrichment process provided by the invention has the advantages of low energy consumption and high lithium recovery rate.
Description
Technical Field
The invention belongs to the technical field of solution purification and separation, and particularly relates to separation and recovery of magnesium and lithium in salt lake brine.
Background
The lithium ion battery has the advantages of low cost, long service life and the like, and gradually replaces a chemical battery to become a pet of an energy storage device. With the increase of new energy automobile production and sales, the demand of lithium ion batteries also increases, and new energy automobiles will become the main field of the future increase of lithium consumption, so the battery grade lithium carbonate is called as "21 st century energy new and expensive". Lithium ions exist in nature mainly as solid mineral resources (spodumene, lepidolite and the like) and liquid mineral resources (salt lake brine, seawater, oil field water and the like). The lithium resource reserve of the salt lake brine accounts for about 70-80% of the total amount of the lithium resource. The most remarkable characteristic of the salt lake brine in China is that the magnesium-lithium ratio is higher. The chemical properties of magnesium ions and lithium ions are extremely similar, and the existence of a large amount of magnesium ions increases the difficulty of extracting the lithium ions. At present, in the existing membrane separation technology, although magnesium and lithium ions are separated to a certain degree, and lithium ion enrichment is realized, in the enrichment process, due to the increase of osmotic pressure of each membrane stage, the ion enrichment efficiency and the process cost are increased.
Disclosure of Invention
Aiming at the problems in the prior art, the invention mainly aims to provide a process for separating magnesium and lithium from salt lake brine, and the process has the advantages of low energy consumption and low cost.
In order to achieve the above object, the present invention provides the following specific technical solutions.
A process for enriching lithium in salt lake brine comprises the following steps:
filtering the salt lake brine to obtain pretreated salt lake brine;
after the pretreated salt lake brine passes through an adsorption device, resolving to obtain resolving liquid;
after the analysis solution passes through an ultrafiltration device, ultrafiltration water is obtained;
the ultrafiltration water enters a primary nanofiltration device to obtain primary nanofiltration water and primary nanofiltration concentrated water, and the primary nanofiltration concentrated water returns to the adsorption device;
the first-stage nanofiltration produced water enters a reverse osmosis device I to obtain reverse osmosis produced water I and reverse osmosis concentrated water I;
the reverse osmosis concentrated water I enters a secondary nanofiltration device to obtain secondary nanofiltration concentrated water and secondary nanofiltration produced water; returning the secondary nanofiltration concentrated water to the ultrafiltration device;
the water produced by the second-stage nanofiltration enters an electrodialysis device to obtain electrodialysis concentrated water and electrodialysis water; the electrodialysis concentrated water enters the subsequent process of recovering lithium;
conveying the electrodialysis produced water to a reverse osmosis device I, and mixing the electrodialysis produced water with the reverse osmosis produced water I to obtain rear-end effluent of the reverse osmosis device I;
the water discharged from the rear end of the reverse osmosis device I enters a reverse osmosis device II for concentration to obtain reverse osmosis produced water II and reverse osmosis concentrated water II;
and mixing the reverse osmosis concentrated water II and the second-stage nanofiltration produced water, and feeding the mixture into an electrodialysis device.
Furthermore, the first-stage nanofiltration device and the second-stage nanofiltration device adopt monovalent or divalent ion selective nanofiltration membranes. By selective nanofiltration membrane to Li in the desorption solution + With Ca 2+、 Mg 2+ The divalent ions are subjected to preliminary separation to ensure that Li of the nanofiltration water production + Further enriching Ca in the solution 2+ 、Mg 2+ Divalent ions with Li + And (4) effectively separating.
The concentrated water of the first-stage nanofiltration still contains high-concentration Li + And the lithium ions are returned to the adsorption device for repeated recovery, so that the recovery utilization rate of the lithium ions is greatly improved.
Furthermore, the monovalent or divalent ion selective nanofiltration membrane is of a two-stage structure. The content of lithium ions in the water produced by the first-stage nanofiltration is not obviously changed, but the content of magnesium ions can be reduced by 90 percent. The removal rate of magnesium ions in the water produced by the secondary nanofiltration is more than 95 percent.
And (4) enabling the reverse osmosis concentrated water I to enter a secondary nanofiltration device for secondary magnesium ion and lithium ion separation. And the secondary nanofiltration produced water enters an electrodialysis device, and lithium ions in the nanofiltration produced water are further concentrated and enriched through electrodialysis. The content of salt and lithium ions in the electrodialysis water is high, and the content of magnesium ions is low.
Along with the concentration of the reverse osmosis membrane on the inlet water, the salt content in the concentrated water gradually rises, so that the osmotic pressure is increased. In order to ensure the concentration effect of the reverse osmosis device, the pressure of the reverse osmosis concentrated water side needs to be increased.
And further, returning electrodialysis produced water to a water production end of the reverse osmosis device I, mixing the electrodialysis produced water with the reverse osmosis produced water I, and then feeding the electrodialysis produced water into the reverse osmosis device II for treatment.
Further, the reverse osmosis device I is of a one-stage multi-section structure or a multi-stage structure: when the reverse osmosis device I is of a first-stage multi-section structure, the electrodialysis water production is conveyed to the water production end of the last section; when the reverse osmosis device I is of an n-stage structure, wherein n is more than or equal to 2, electrodialysis produced water is conveyed to a water production end of the last section of the n-th stage reverse osmosis, and produced water before the n-1 th stage reverse osmosis returns to a desorption liquid tank.
And the electrodialysis produced water is low-concentration salt solution, is conveyed to the reverse osmosis device I and is mixed with the reverse osmosis produced water I to be used as the rear-end effluent of the reverse osmosis device I, so that the osmotic pressure on two sides of the reverse osmosis membrane and the transmembrane pressure difference on two sides of the membrane are reduced. Meanwhile, the water discharged from the rear end of the reverse osmosis device I is treated by the independent reverse osmosis device II without passing through a secondary nanofiltration device, so that the loss of lithium ions can be reduced.
In order to ensure that the electrodialysis device has better salt transfer efficiency, the salt content in the electrodialysis production water can be improved. The electrodialysis water production with higher salt content returns to the water production end of the high-power concentration section of the reverse osmosis device I, so that the pressure difference on two sides of the reverse osmosis membrane can be further reduced, and the problem of pollution and blockage of the reverse osmosis membrane is solved. And moreover, concentrated water obtained by concentrating the rear-end effluent of the reverse osmosis device I through the reverse osmosis device II directly returns to the electrodialysis device for concentration, and Li ions are not lost. And sending the reverse osmosis water II into a desorption liquid tank.
Furthermore, the reverse osmosis device I and the reverse osmosis device II both adopt brackish water membranes as reverse osmosis membranes.
Further, the electrodialysis process may employ one-stage or multi-stage treatment processes.
Compared with the prior art, the technical scheme of the invention has the following obvious beneficial effects.
(1) The separation of magnesium and lithium and the high-efficiency enrichment of lithium in the salt lake brine are realized, and the method is very suitable for the salt lake brine with high magnesium content.
(2) The water produced in the nanofiltration, reverse osmosis and electrodialysis processes is recycled and utilized, and the energy consumption of the system, the lithium resource waste and the wastewater discharge are reduced.
(3) The electrodialysis water production enters the reverse osmosis water production end, so that the osmotic pressure on two sides of the reverse osmosis membrane is reduced, the reverse osmosis concentration effect is improved, and membrane fouling and blocking are reduced.
(4) The magnesium content in the electrodialysis water production and the reverse osmosis water production is low, and the electrodialysis water production and the reverse osmosis water production are concentrated by a single reverse osmosis device and then directly enter the electrodialysis device for secondary concentration, so that the loss of lithium ions is reduced.
Drawings
FIG. 1 is a process flow diagram of a portion of an embodiment.
Detailed Description
To better illustrate the objects, technical solutions and advantages of the present invention, the following examples are provided for further illustration. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention. In the examples, the methods used were conventional methods unless otherwise specified, and the equipment used was commercially available.
After the salt lake brine is filtered, adsorbed and analyzed, the concentration of lithium ions in the analysis solution is 800 mg/L, the concentration of magnesium ions is 400 mg/L, the mass ratio of the magnesium ions to the lithium ions is 1. The amount of the liquid supplied in this example was 250m 3 /h。
The recovery rate of lithium ions at each stage in the examples was calculated as follows: recovery rate of lithium ions = (water production amount × lithium ion concentration)/(water intake amount × lithium ion concentration).
And (3) ultrafiltration:
and (4) feeding the adsorption and desorption solution into an ultrafiltration device to remove impurities, and obtaining ultrafiltration water. The concentrations of lithium ions and magnesium ions in the ultrafiltration water are almost unchanged, and the amount of the ultrafiltration water is about 237.5 m 3 /h。
Primary nanofiltration:
the ultrafiltration water is processed by a first-stage nanofiltration device to obtain first-stage nanofiltration water and first-stage nanofiltration concentrated water.
The nanofiltration device adopts monovalent ion selective nanofiltration membranes, the primary nanofiltration device consists of 2 sets of nanofiltration membrane equipment, and each set of nanofiltration membrane equipment is formed by connecting two-section type structures in series. The design pressure of the nanofiltration membrane is less than or equal to 4.0MPa, the design temperature is 10-40 ℃, and the design pH is = 2-11.
The concentration of lithium ions in the first-stage nanofiltration produced water is 815 mg/L, the concentration of magnesium ions is reduced to 90 mg/L, and the mass ratio of the magnesium ions to the lithium ions is 1; the water yield of the first-stage nanofiltration is about 208.24 m 3 The salt content is 6872mg/L.
The concentrated water amount of the first-stage nanofiltration is about 36.75 m 3 The salt content is 21000 mg/L, the lithium ion content is about 1418 mg/L, and the lithium ion is directly returned to the adsorption device to increase the recovery of the lithium ions. After passing through a primary nanofiltration deviceThe recovery rate of lithium ions was about 85%.
Reverse osmosis:
and the water produced by the first-stage nanofiltration enters a reverse osmosis device I for concentration.
The reverse osmosis device I is composed of 2 sets of reverse osmosis membrane equipment, each set of reverse osmosis equipment adopts a three-section design, and each section of reverse osmosis unit comprises different numbers of reverse osmosis membranes; the design pressure is less than or equal to 4.0MPa, the design temperature is 10 to 40 ℃, and the design pH value is 2 to 11. The first-stage nanofiltration water product passes through a first set of reverse osmosis membrane equipment and is concentrated by the reverse osmosis units in each section in sequence to obtain first-stage reverse osmosis concentrated water and first-stage reverse osmosis water product. And conveying the first-stage reverse osmosis produced water to a desorption liquid tank. The first-stage reverse osmosis concentrated water enters a second set of reverse osmosis membrane equipment and is concentrated through each section of reverse osmosis unit in sequence to obtain reverse osmosis concentrated water I and reverse osmosis produced water I. The quantity of the reverse osmosis concentrated water I is about 49.98 m 3 The concentration of lithium ions is 3303.2 mg/L, the concentration of magnesium ions is 364.5mg/L, the mass ratio of the magnesium ions to the lithium ions is 1; the quantity of reverse osmosis produced water I is about 33.32 m 3 And the lithium ion content is about 39.96 mg/L and the magnesium ion content is about 4.41 mg/L, and the lithium ion content and the magnesium ion content are returned to the adsorption device to be used as the eluting water, so that the utilization rate of reverse osmosis water production is improved.
And (3) secondary nanofiltration:
and (4) enabling the reverse osmosis concentrated water I to enter a secondary nanofiltration device for secondary magnesium-lithium separation. The secondary nanofiltration device adopts monovalent ion selective nanofiltration membranes and consists of 2 sets of nanofiltration membrane equipment, and each set of nanofiltration membrane equipment is formed by connecting two-section type structures in series. The design pressure of the nanofiltration membrane is less than or equal to 4.0MPa, the design temperature is 10-40 ℃, and the design pH value is 2-11.
And (4) passing the reverse osmosis concentrated water I through a secondary nanofiltration device to obtain secondary nanofiltration concentrated water and secondary nanofiltration produced water. The water yield of the secondary nanofiltration is about 42.48 m 3 H, the concentration of lithium ions is 3138.3 mg/L, the concentration of magnesium ions is 72.90 mg/L, the mass ratio of the magnesium ions to the ions is 1; the salt content of the secondary nanofiltration concentrated water is about 138 mg/L, wherein the lithium ion content is about 22.66 mg/L, the magnesium ion concentration is about 0.61mg/L, and the secondary nanofiltration concentrated water directly returns to the primary nanofiltration device to reduceLithium ion loss and waste water discharge. The whole secondary nanofiltration device ensures that the recovery rate of lithium ions in the secondary nanofiltration produced water can reach 85 percent.
Electrodialysis:
and (3) adopting a homogeneous phase ion exchange membrane as an ion selection membrane of the electrodialysis device, and concentrating the secondary nanofiltration water and the reverse osmosis concentrated water II through the electrodialysis device to obtain electrodialysis concentrated water and electrodialysis water. The amount of electrodialysis concentrated water is about 5.52 m 3 H, the concentration of lithium ions is 15.77g/L, and the concentration of magnesium ions is about 0.34 g/L; the mass ratio of magnesium ions to lithium ions is 0.022, and the salt content is about 104g/L. The lithium ion concentration in the electrodialysis concentrated water reaches the lithium ion concentration required by preparing high-purity lithium, and the electrodialysis concentrated water can be used for the subsequent process step of preparing lithium salt.
Introducing electrodialysis water production into a water production end of the last section of a second set of reverse osmosis membrane equipment of the reverse osmosis device I by using a circulating water pump, and mixing the electrodialysis water production with the reverse osmosis water production I to obtain water discharged from the rear end of the reverse osmosis device I; the rear end effluent directly enters a reverse osmosis device II for concentration to obtain reverse osmosis produced water II and reverse osmosis concentrated water II, or the rear end effluent of the reverse osmosis device I is conveyed to an intermediate water tank for storage. The water discharged from the rear end of the reverse osmosis device I stored in the intermediate water tank enters a reverse osmosis device II for concentration to obtain reverse osmosis produced water II and reverse osmosis concentrated water II; or the rear end outlet water of the reverse osmosis device I stored in the intermediate water tank is further mixed with the electrodialysis water production water and the reverse osmosis water production water I to be used as the rear end outlet water of the reverse osmosis device I.
And conveying the reverse osmosis produced water II to a desorption liquid tank. And after the reverse osmosis concentrated water II is mixed with the second-stage nanofiltration produced water, the mixture enters an electrodialysis device for concentration.
By improving the salt content of the water production side of the reverse osmosis membrane and reducing the transmembrane pressure difference of the two sides of the reverse osmosis membrane, the problems of easy pollution and blockage of the membrane, low water production rate, poor concentration effect and the like are solved.
The water yield of electrodialysis is about 64.21 m 3 And h, conveying the water to a reverse osmosis device I, mixing the water with reverse osmosis produced water I, and taking the water as the water outlet at the rear end of the reverse osmosis device I to reduce the differential pressure of a reverse osmosis membrane. The quantity of reverse osmosis produced water I is about 97.53 m 3 /h，The salt content gradually decreased to 4653mg/L, wherein the lithium ion content was about 759.7mg/L and the magnesium ion content was about 21.62 mg/L.
The quantity of the reverse osmosis concentrated water II is about 24.38 m 3 The salt content increased to 18.3g/L, the lithium ion content was about 2970.8 mg/L and the magnesium ion concentration was about 84.68 mg/L. The reverse osmosis concentrated water II is mixed with the second-stage nanofiltration produced water and then returns to the electrodialysis device for treatment, so that the water inflow of the electrodialysis device is increased to 66.86m 3 The concentration of lithium ions in the feed water is about 1133.21 mg/L, the concentration of magnesium ions is about 30.56 mg/L, and the salt content is about 22.23 g/L. The quantity of reverse osmosis produced water II is about 73.15 m 3 H, the lithium ion content is about 22.66 mg/L, the magnesium ion content is about 0.61mg/L, and the solution is conveyed to a solution tank to be used as preparation water of rinsing water and solution.
And the reverse osmosis device II adopts a salt water membrane as a reverse osmosis membrane.
The scheme of the embodiment realizes the separation of magnesium and lithium and the high-efficiency enrichment of lithium in the salt lake brine, and the finally obtained electrodialysis concentrated water has higher lithium ion concentration, so that the electrodialysis concentrated water can be directly used for preparing high-purity lithium. The yield of lithium ions in the whole magnesium-lithium separation process is more than 68 percent. In the process of treating the salt lake brine, water in all stages is completely utilized, external drainage is not carried out, and the recovery rate of lithium ions is very high and basically can be considered to be 99%.
In other embodiments of the invention, the reverse osmosis device I is a one-stage three-section type, and the electrodialysis water production is introduced into a three-section water production end by utilizing a circulating water pump.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (10)
1. A process for enriching lithium in salt lake brine is characterized by comprising the following steps:
filtering the salt lake brine to obtain pretreated salt lake brine;
after the pretreated salt lake brine passes through an adsorption device, resolving to obtain resolving liquid;
after the analysis solution passes through an ultrafiltration device, ultrafiltration water is obtained;
the ultrafiltration water enters a primary nanofiltration device to obtain primary nanofiltration water and primary nanofiltration concentrated water, and the primary nanofiltration concentrated water returns to the adsorption device;
the first-stage nanofiltration produced water enters a reverse osmosis device I to obtain reverse osmosis produced water I and reverse osmosis concentrated water I;
the reverse osmosis concentrated water I enters a secondary nanofiltration device to obtain secondary nanofiltration concentrated water and secondary nanofiltration produced water; returning the secondary nanofiltration concentrated water to the ultrafiltration device;
the water produced by the secondary nanofiltration enters an electrodialysis device to obtain electrodialysis concentrated water and electrodialysis water; the electrodialysis concentrated water enters the subsequent process of recovering lithium;
conveying the electrodialysis produced water to a reverse osmosis device I, and mixing the electrodialysis produced water with the reverse osmosis produced water I to obtain rear-end outlet water of the reverse osmosis device I;
the water discharged from the rear end of the reverse osmosis device I enters a reverse osmosis device II for concentration to obtain reverse osmosis produced water II and reverse osmosis concentrated water II;
and mixing the reverse osmosis concentrated water II and the second-stage nanofiltration produced water, and feeding the mixture into an electrodialysis device.
2. The beneficiation process according to claim 1, wherein the primary and secondary nanofiltration devices employ monovalent or divalent ion selective nanofiltration membranes.
3. The concentration process according to claim 2, wherein the monovalent or divalent ion selective nanofiltration membrane has a two-stage or multi-stage structure.
4. The beneficiation process of claim 1, wherein the first stage nanofiltration concentrated water is returned to the adsorption device.
5. The beneficiation process of claim 1, wherein the reverse osmosis unit i is a one-stage multi-stage reverse osmosis unit or a multi-stage reverse osmosis unit.
6. The concentration process according to claim 5, wherein when the reverse osmosis device I is in a one-stage multi-stage structure, the electrodialytic produced water is conveyed to the water production end of the last stage; when the reverse osmosis device I is of an n-stage structure, wherein n is more than or equal to 2, electrodialysis produced water is conveyed to a water production end of the last section of the n-th stage reverse osmosis, and produced water before the n-1 th stage reverse osmosis returns to a desorption liquid tank.
7. The beneficiation process according to claim 1, wherein the reverse osmosis produced water ii is sent to a solution tank.
8. The enrichment process according to claim 1, wherein the reverse osmosis device I and the reverse osmosis device II both adopt a brackish water membrane as the reverse osmosis membrane; the electrodialysis process adopts a one-stage or multi-stage treatment process.
9. The beneficiation process according to claim 1, wherein an intermediate water tank is provided for storing the rear end effluent of the reverse osmosis unit I.
10. The beneficiation process according to claim 9, wherein the back end effluent stored in the intermediate water tank is delivered to a reverse osmosis unit ii as the feed water, or is mixed with the electrodialysis product water as the back end effluent of the reverse osmosis unit i.
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