CN111729350B - Equipment for extracting lithium from brine by adsorption method - Google Patents
Equipment for extracting lithium from brine by adsorption method Download PDFInfo
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- CN111729350B CN111729350B CN202010645609.XA CN202010645609A CN111729350B CN 111729350 B CN111729350 B CN 111729350B CN 202010645609 A CN202010645609 A CN 202010645609A CN 111729350 B CN111729350 B CN 111729350B
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- brine
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- 239000012267 brine Substances 0.000 title claims abstract description 132
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 132
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 63
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 177
- 238000005406 washing Methods 0.000 claims abstract description 163
- 238000003795 desorption Methods 0.000 claims abstract description 122
- 239000003463 adsorbent Substances 0.000 claims abstract description 91
- 230000007246 mechanism Effects 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 230000005540 biological transmission Effects 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims description 112
- 239000000243 solution Substances 0.000 claims description 47
- 238000000429 assembly Methods 0.000 claims description 19
- 230000000712 assembly Effects 0.000 claims description 19
- 238000011084 recovery Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 abstract description 12
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 abstract description 9
- 238000011033 desalting Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract description 3
- 239000004744 fabric Substances 0.000 description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- 229910003002 lithium salt Inorganic materials 0.000 description 16
- 159000000002 lithium salts Chemical class 0.000 description 16
- 238000000926 separation method Methods 0.000 description 11
- 238000009826 distribution Methods 0.000 description 9
- 238000010828 elution Methods 0.000 description 9
- 238000000605 extraction Methods 0.000 description 7
- 239000006148 magnetic separator Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WKPSFPXMYGFAQW-UHFFFAOYSA-N iron;hydrate Chemical compound O.[Fe] WKPSFPXMYGFAQW-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/02—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/04—Filters with filtering elements which move during the filtering operation with filtering bands or the like supported on cylinders which are impervious for filtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/58—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/58—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element
- B01D33/60—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for washing
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention provides equipment for extracting lithium from brine by an adsorption method, and belongs to the technical field of adsorption lithium extracting equipment. The brine-stripping device comprises a belt vacuum filter, wherein the belt vacuum filter is connected with a solid-liquid mixing mechanism for mixing brine and an adsorbent, a raw material brine area, a salt-washing area and a desorption area which are connected with each other are sequentially arranged on the belt vacuum filter along the transmission direction of the belt vacuum filter, the solid-liquid mixing mechanism is connected with the raw material brine area, and a first liquid conveying mechanism for conveying salt-washing liquid and a second liquid conveying mechanism for conveying desorption liquid are respectively connected with the salt-washing area and the desorption area. Compared with the existing adsorption tower for adsorption, the invention has low investment cost, greatly reduces the investment and production cost of the subsequent desalting and purifying process, and finally can stably obtain the battery-grade lithium carbonate or lithium hydroxide.
Description
Technical Field
The invention belongs to the technical field of adsorption lithium extraction equipment, and relates to equipment for extracting lithium from brine by an adsorption method.
Background
The use form of the adsorbent is the key of the water treatment technology of the adsorption method. Because of the defects of difficult solid-liquid separation, difficult recovery and the like of the powder adsorbent, the water treatment adsorption method after the 90 th century adopts a process of combining a particle adsorbent with an adsorption tower.
The water treatment adsorbent is mainly divided into two major categories of organic and inorganic, the organic adsorbent with the diameter of about 1-2mm forms a mature market, and the organic adsorbent is filled in an adsorption tower and is widely applied to various fields of water treatment. Inorganic adsorbents represented by iron-based, aluminum-based, manganese-based and the like, particularly, adsorbents of hydroxy iron, aluminum, manganese and the like which cannot be formed by calcination, have no mature and complete solution in the granulating process, the inorganic adsorbents after granulation are easy to crush, and the activity of the granular adsorbents is far lower than that of powder.
The adsorption method brine lithium extraction technology has wide adaptability to different salt lakes, and can treat low-lithium-content brine. The technology of extracting lithium from brine by an adsorption method has been realized in the large-scale industrialization of Argentina salt lake and Qinghai salt lake in China. Meanwhile, great research and attention is paid to the technology of extracting lithium from brine by an adsorption method, and the technology relates to a plurality of fields of adsorbent synthesis, different lithium extraction efficiencies of brine, adsorption reaction mechanisms and the like.
Numerous studies and practices have shown that the most efficient adsorbents for extracting lithium from brine are oxides or hydroxides of aluminum, manganese, titanium, etc. The above-mentioned metal oxide or hydroxide sorbent granulation technique is consistently a water treatment industry challenge. However, the current industrial production line for extracting lithium from brine still inherits the technical route of the traditional water treatment adsorption method, and adopts a process of combining a particle adsorbent with an adsorption tower.
Because of the characteristics of brine extraction lithium adsorbents, research and patents have proposed using powder adsorbents for brine extraction of lithium. In order to realize recovery of the powder adsorbent, solid-liquid separation of the adsorbent and water by using a plate-and-frame filter press, a centrifuge and a ceramic membrane has been studied; there are also studies and patents to carry the adsorbent with magnetism, and then to realize solid-liquid separation by using a magnetic separator.
The technical route of combining the granular adsorbent with the adsorption tower is used for extracting lithium from brine, and has some problems: 1) The production stage needs to construct a large amount of adsorption towers filled with the adsorbent, and the investment cost is high; 2) Magnesium to lithium ratio greater than 3:1, salt to lithium ratio TDS: a desorption liquid with Li greater than 30:1; 3) The recovery rate of lithium in the adsorption section is generally less than 60%, and if the high recovery rate of lithium is to be realized, multiple towers are required to be connected in series and the function is required to be converted, so that the difficulty of industrial continuous production is greatly improved.
The brine lithium extraction process of a powder adsorbent combined plate-and-frame filter press, a centrifuge, precise filtration or a ceramic membrane is currently in a laboratory or pilot-scale stage, and related documents and patents only focus on solid-liquid separation of the powder adsorbent and brine, and lack knowledge and focus on the washing process of the adsorbent in the process of extracting the brine lithium, so that the process cannot obtain low-salt lithium ratio desorption liquid.
The total salinity of brine can reach hundreds of grams per liter, and the lithium content is only tens to hundreds of milligrams per liter. The applicant finds that how to furthest reduce the salt-lithium ratio in desorption liquid is the key for extracting lithium from brine by an adsorption method in the process of extracting lithium from brine by using the adsorption method through a large number of research experiments.
Disclosure of Invention
The invention aims to solve the problems and provide equipment for extracting lithium from brine by an adsorption method.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the utility model provides a device for absorption method brine draws lithium, includes belt vacuum filter, belt vacuum filter be connected with be used for with brine and adsorbent mixed solid-liquid mixing mechanism, belt vacuum filter is last and be equipped with interconnect's raw materials brine area, salt washing district and desorption district in proper order along belt vacuum filter's transmission direction, solid-liquid mixing mechanism connects raw materials brine area, carries the first liquid conveying mechanism of salt washing liquid and carries the second liquid conveying mechanism of desorption liquid to connect salt washing district and desorption district respectively.
In the above-mentioned equipment for extracting lithium from brine by adsorption, the first liquid conveying mechanism comprises at least two mutually independent salt-washing liquid circulating components which are sequentially connected, and the different salt-washing liquid circulating components are connected one by one from one side close to the desorption area to the other side.
In the device for extracting lithium from brine by the adsorption method, the discharge port of the brine-washing circulating assembly closest to the raw brine area is connected with the tail part of the belt vacuum filter, a brine-washing conveyor is arranged above the brine-washing circulating assembly closest to the desorption area, and the discharge port of the brine-washing circulating assembly on one side, close to the desorption area, of each two adjacent brine-washing circulating assemblies is positioned above the belt vacuum filter and corresponds to the feed port of the other brine-washing circulating assembly.
In the above-mentioned equipment for extracting lithium from brine by adsorption, the salt-washing liquid circulation assembly comprises a salt-washing liquid vacuum box connected with the belt vacuum filter and a salt-washing liquid conveying assembly connected with the salt-washing liquid vacuum box, wherein the discharge port of the salt-washing liquid conveying assembly on the salt-washing liquid circulation assembly on one side, close to the desorption area, of every two adjacent salt-washing liquid circulation assemblies is positioned above the belt vacuum filter and corresponds to the salt-washing liquid vacuum box on the other salt-washing liquid circulation assembly.
In the above-mentioned equipment for extracting lithium from brine by adsorption, the second liquid conveying mechanism comprises at least two mutually independent and sequentially connected desorption liquid circulation components, and the different desorption liquid circulation components are connected one by one from one side far away from the salt washing area to the other side.
In the above-mentioned equipment for extracting lithium from brine by adsorption method, the discharge port of the desorption solution circulation assembly closest to the salt washing area is connected with the subsequent finishing working section, the feed port of the desorption solution circulation assembly farthest from the salt washing area is connected with the desorption solution conveyor above the belt vacuum filter, and the discharge port of the desorption solution circulation assembly on one side of each adjacent two desorption solution circulation assemblies far from the salt washing area is positioned above the belt vacuum filter and corresponds to the feed port of the other desorption solution circulation assembly.
In the above-mentioned equipment for extracting lithium from brine by adsorption, the desorption liquid circulation assembly comprises a desorption liquid vacuum box connected with the belt vacuum filter and a desorption liquid conveying assembly connected with the desorption liquid vacuum box, and the desorption liquid conveying assembly on the desorption liquid circulation assembly on one side far away from the salt washing area in every two adjacent desorption liquid circulation assemblies is positioned above the belt vacuum filter and corresponds to the desorption liquid vacuum box on the other desorption liquid circulation assembly.
In the above-mentioned equipment for extracting lithium from brine by adsorption, the device further comprises a salt-washing and water-returning area connected with the desorption area, wherein the discharge port of the first liquid conveying mechanism is connected with the salt-washing and water-returning area.
In the above-mentioned equipment for extracting lithium from brine by adsorption, the device further comprises a salt-washing and water-returning area connected with the desorption area, wherein a discharge port of a salt-washing liquid circulating assembly nearest to the raw brine area is connected with the salt-washing and water-returning area, and the salt-washing and water-returning area is connected with the solid-liquid mixing mechanism through a conveying belt.
In the device for extracting lithium from brine by an adsorption method, the brine washing and returning area comprises a brine washing and returning vacuum box connected with a belt type vacuum filter, the brine washing and returning vacuum box is connected with a brine washing and recovering solid-liquid separator through a brine washing and returning conveying assembly, and the raw brine area is connected with the raw brine solid-liquid separator through a raw brine conveying assembly.
Compared with the prior art, the invention has the advantages that:
1. compared with the existing adsorption tower for adsorption, the invention has low investment cost and can reduce the investment cost by about 80 percent.
2. According to the invention, the desorption liquid with the magnesium-lithium ratio smaller than 1:1 and the salt-lithium ratio (TDS/Li) smaller than 10:1 can be obtained, so that the investment and production cost of the subsequent desalting and purifying process are greatly reduced, and finally, the battery grade lithium carbonate or lithium hydroxide can be stably obtained.
3. The loss of the adsorbent is small, and the leakage rate of the adsorbent in a single adsorption and desorption cycle is less than 0.01%.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic view of a partial structure of the present invention;
fig. 3 is a partial structural schematic of the present invention.
In the figure: the solid-liquid mixing mechanism 1, the mixing tank 1a, the raw material brine area 2, the salt washing area 3, the desorption area 4, the first liquid conveying mechanism 5, the second liquid conveying mechanism 6, the salt washing liquid circulating assembly 7, the salt washing liquid collecting tank 7a, the salt washing liquid vacuum box 8, the salt washing liquid conveying assembly 9, the desorption liquid circulating assembly 10, the desorption liquid vacuum box 11, the desorption liquid conveying assembly 11a, the salt washing backwater area 12, the conveying belt 13, the salt washing backwater vacuum box 14, the salt washing backwater conveying assembly 15, the salt washing recovery solid-liquid separator 16, the raw material brine conveying assembly 17, the raw material brine solid-liquid separator 18, the belt type vacuum filter 100, the frame 101, the filter cloth 102 and the scraper 103.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
As shown in fig. 1-3, an apparatus for extracting lithium from brine by an adsorption method comprises a belt vacuum filter 100, wherein the belt vacuum filter 100 is connected with a solid-liquid mixing mechanism 1 for mixing brine and an adsorbent, a raw material brine zone 2, a salt washing zone 3 and a desorption zone 4 which are connected with each other are sequentially arranged on the belt vacuum filter 100 along the transmission direction of the belt vacuum filter 100, the solid-liquid mixing mechanism 1 is connected with the raw material brine zone 2, and a first liquid conveying mechanism 5 for conveying salt washing liquid and a second liquid conveying mechanism 6 for conveying desorption liquid are respectively connected with the salt washing zone 3 and the desorption zone 4.
In this embodiment, the raw brine zone 2, the salt-washing zone 3 and the desorption zone 4 are connected to each other in the belt vacuum filter 100, and these zones are set so as to be divided according to the areas where the materials or liquids of the solid-liquid mixing mechanism 1, the first liquid transporting mechanism 5 and the second liquid transporting mechanism 6 contact the belt vacuum filter 100. The belt vacuum filter 100 is a prior art, and can be a commercially available product, specifically, the belt vacuum filter 100 comprises a frame 101 and a filter cloth 102 on the frame 101, the filter cloth 102 is connected end to form a ring shape, and a motor on the frame 101 is driven by a tensioning wheel and other components to circularly rotate in the circumferential direction.
The filter cloth 102 is used for solid-liquid separation, i.e. separating the adsorbent from the liquid, the filter cloth 102 preferably adopts a filter cloth with large ventilation capacity, and the ventilation capacity of the filter cloth is more than 500L/m 2 S to ensure the separation capacity of brine from the adsorbent, the retention rate of the adsorbent is more than 90%.
The solid-liquid mixing mechanism 1 mixes the adsorbent with the brine, lithium-containing salt and other salts in the brine are adsorbed by the adsorbent, the solid-liquid mixing mechanism 1 conveys the mixture to the raw material brine area 2, solid-liquid separation is realized between the adsorbent and the brine in the raw material brine area 2, the brine permeates the filter cloth 102, and the adsorbent is positioned on the filter cloth 102.
The solid-liquid mixing mechanism 1 comprises a mixing tank 1a, wherein a stirring paddle is arranged in the mixing tank 1a and used for stirring the adsorbent and brine, the mixing tank 1a can be directly arranged above the raw material brine area 2, so that the adsorbent and brine mixture can be directly sprinkled on the filter cloth 102 of the raw material brine area 2, or the mixing tank 1a is connected through a conveying pump, so that the adsorbent and brine mixture is input to the filter cloth 102 of the raw material brine area 2. Brine is pumped into the mixing tank 1a, and the adsorbent can be added directly into the mixing tank 1a or through a conveyer belt into the mixing tank 1 a.
The salt washing liquid adopts fresh water and is pumped to the position above the salt washing area 3 through a conveying pump, namely, the first liquid conveying mechanism 5 can be a conveying pump for conveying fresh water.
As a preferred solution, as shown in connection with fig. 3, the first liquid transfer means 5 comprise at least two mutually independent and sequentially connected brine-circulating assemblies 7, the different brine-circulating assemblies 7 being connected one by one from one side close to the desorption zone 4 to the other. That is, the salt wash circulation assemblies 7 are implemented in series with each other.
The discharging port of the salt washing liquid circulating assembly 7 closest to the raw material brine area 2 is connected with the tail part of the belt type vacuum filter 100, wherein the tail part refers to the tail end of the filter cloth 102, and the discharged water of the salt washing liquid circulating assembly 7 closest to the raw material brine area 2 returns to the tail end of the filter cloth 102, so that the salt content of the adsorbent on the filter cloth 102 is increased.
A salt-washing liquid conveyer is arranged above the salt-washing liquid circulating assembly 7 closest to the desorption zone 4, and the salt-washing liquid conveyer is a spray head connected with a conveying pump or a pipeline and the like and is used for directly spraying fresh water on the adsorbent of the filter cloth 102 so as to separate salt in the adsorbent.
In this embodiment, the multiple salt-washing liquid circulating assemblies 7 are connected in series, which actually has the effect of gradient elution, and also accords with the principle of a small number of times in chemistry, so that the impurity salt in the adsorbent is eluted in advance.
The discharge port of the salt washing liquid circulating assembly 7 on the side close to the desorption zone 4 in each adjacent two salt washing liquid circulating assemblies 7 is positioned above the belt type vacuum filter 100 and corresponds to the feed port of the other salt washing liquid circulating assembly 7. With the structure, the salt concentration in the salt washing liquid from the salt washing liquid circulation assembly 7 close to the desorption zone 4 to the salt washing liquid from the salt washing liquid circulation assembly 7 far from the desorption zone 4 is sequentially increased, so that the gradient elution of increasing type is realized, and the eluting efficiency is improved.
The applicant found that the more difficult the lithium salt adsorbed by the adsorbent is to desorb when the salt concentration in the salt wash is higher, the less easily the lithium is eluted when the salt-to-lithium ratio (ratio of normal salt to lithium-containing salt) in the adsorbent is higher. In view of the simultaneous achievement of washing and desalting and reduction of elution of lithium salt, the present invention creatively proposes a gradient elution structure. The principle of the gradient elution structure is as follows: the salt content of the salt washing liquid discharged from the discharge port of the salt washing liquid circulation assembly 7 gradually increases from the direction close to the desorption zone 4 to the direction close to the raw material brine zone 2, namely, the salt washing liquid closest to the desorption zone 4 is pure water, and the salt washing liquid closest to the raw material brine zone 2 contains part of desorbed lithium salt and other eluted mixed salt. The advantage is that the salt content of the salt washing liquid along the transmission direction of the filter cloth 102 is gradually decreased, the salt is gradually eluted, and the probability of synchronously eluting the lithium salt in the eluting process is greatly reduced, so that the lithium salt is prevented from being eluted in advance, and other impurity salts are better eluted.
In this embodiment, a structure is also provided for re-adsorbing and recovering lithium salt coming out of the discharge port of the brine-washing liquid circulation assembly 7 closest to the raw brine area 2. That is, the device also comprises a salt-washing and water-returning area 12 connected with the desorption area 4, and the discharge port of the first liquid conveying mechanism 5 is connected with the salt-washing and water-returning area 12. Specifically, the discharge port of the brine-washing circulation assembly 7 closest to the raw brine area 2 is connected with a brine-washing return area 12. Since the salt-washing and water-returning region 12 is connected behind the desorption region 4, the lithium salt in the adsorbent reaching the salt-washing and water-returning region 12 is desorbed, or the content of the lithium salt in the adsorbent is extremely low, the lithium salt contained in the backwater of the discharge port of the salt-washing liquid circulation assembly 7 can be adsorbed by the adsorbent again, so that the waste of the lithium salt is avoided.
The specific structure of the gradient salt washing is as follows: the salt washing liquid circulation assembly 7 comprises a salt washing liquid vacuum box 8 connected with the belt type vacuum filter 100 and a salt washing liquid conveying assembly 9 connected with the salt washing liquid vacuum box 8, wherein a discharge hole of the salt washing liquid conveying assembly 9 on the salt washing liquid circulation assembly 7 on one side, close to the desorption area 4, of every two adjacent salt washing liquid circulation assemblies 7 is positioned above the belt type vacuum filter 100 and corresponds to the salt washing liquid vacuum box 8 on the other salt washing liquid circulation assembly 7.
The salt washing liquid circulation assembly 7 comprises a salt washing liquid collection tank 7a connected with a salt washing liquid vacuum box 8, the salt washing liquid collection tank 7a is connected with a vacuum pump and a conveying pump, salt washing liquid is transferred through the conveying pump, the salt washing liquid reaches the upper portion of the filter cloth 102, the adsorbent on the filter cloth is leached, vacuum is generated through the vacuum pump, and liquid on the filter cloth 102 is sucked into the salt washing liquid collection tank 7 a. The brine washing water closest to the brine washing circulation assembly 7 of the raw brine area 2 is pumped to the upper part of the brine washing and returning area 12 by a conveying pump, and the adsorbent is leached.
A water distribution structure is arranged above the salt-washing liquid vacuum box 8, the water distribution structure can be a pipe or a plurality of pipes are arranged at intervals along the axial direction of the belt type vacuum filter 100, the water distribution structure is connected with a salt-washing liquid water inlet, wherein the water distribution structure closest to the desorption area 4 is directly connected with a salt-washing liquid conveyor, the salt-washing liquid circulating assembly 7 closest to the raw material brine area 2 is not connected with the water distribution structure, and the outlets of the rest salt-washing liquid circulating assemblies 7 are all connected with one water distribution structure.
The second liquid conveying mechanism 6 comprises at least two mutually independent and sequentially connected desorption liquid circulation assemblies 10, and the different desorption liquid circulation assemblies 10 are connected one by one from one side far away from the salt washing area 3 to the other side.
It will be appreciated that the desorber circulation assembly 10 may be configured in the same manner as the brine circulation assembly 7 and functions to deliver a liquid through which the adsorbent on the filter cloth 102 is rinsed to elute the lithium salt from the adsorbent.
In this embodiment, the desorption solution circulation modules 10 are also connected in series, and the gradient elution effect is achieved. The discharge port of the desorption solution circulation assembly 10 closest to the salt washing zone 3 is connected with a subsequent finishing working section, which is a subsequent working section such as filtration, concentration and the like, but the finishing working section is the prior art, and does not belong to the structure of the invention and is not the technical problem to be solved by the invention.
The feeding port of the desorption solution circulation assembly 10 farthest from the salt washing area 3 is connected with a desorption solution conveyor above the belt vacuum filter 100, the desorption solution conveyor can be a conveying pump for directly conveying pure water, and the discharging port of the desorption solution circulation assembly 10, which is far away from one side of the salt washing area 3, in every two adjacent desorption solution circulation assemblies 10 is located above the belt vacuum filter 100 and corresponds to the feeding port of the other desorption solution circulation assembly 10.
Along the transmission direction of the filter cloth 102 of the vacuum filter 100, the lithium content in the desorption liquid gradually decreases, and finally, pure water is used for desorbing the adsorbent, so that the lithium in the adsorbent can be fully eluted.
The desorption solution circulation assembly 10 comprises a desorption solution vacuum box 11 connected with the belt vacuum filter 100 and a desorption solution conveying assembly 11a connected with the desorption solution vacuum box 11, wherein the desorption solution conveying assembly on the desorption solution circulation assembly 10 on one side far away from the salt washing area 3 in each two adjacent desorption solution circulation assemblies 10 is positioned above the belt vacuum filter 100 and corresponds to the desorption solution vacuum box 11 on the other desorption solution circulation assembly 10. The desorption liquid conveying assembly 11a comprises a collection tank and a conveying pump which are connected with the desorption liquid vacuum box 11, and an outlet of the conveying pump of one desorption liquid circulating assembly 10 connected with a pipeline corresponds to the desorption liquid vacuum box 11 on the other adjacent desorption liquid circulating assembly 10.
Similarly, a water distribution structure is also arranged above each desorption solution vacuum box 11, and the water distribution structure can be a pipeline provided with a plurality of openings or spray heads and the like, and the water distribution structure forms desorption solution into a spray shape to spray the adsorbent on the filter cloth 102, so that lithium salt is washed out of the adsorbent. This elution mode has a great advantage: because the lithium content in the adsorbent on the filter cloth 102 of the belt vacuum filter 100 is more and less and is less likely to be desorbed, after the desorption solution circulation assembly 10 of the embodiment is in a series structure, the lithium content in the desorption solution is smaller along with the transmission direction of the filter cloth 102, that is, along with the transmission direction of the filter cloth 102, the lithium content in the desorption solution from different desorption solution circulation assemblies 10 and the lithium content in the adsorbent on the filter cloth 102 show a positive correlation relationship, and finally, pure water is used as the desorption solution to directly desorb and elute the adsorbent with the least lithium content, thereby achieving the effect of complete elution.
The brine of the brine-washing circulation assembly 7 closest to the raw brine area 2 may be directly applied to the brine field. However, the salt content of brine in the salt field is reduced by such treatment, and the brine also contains a certain amount of lithium, so that the lithium is directly discharged into the salt field to cause incomplete adsorption, and the extraction rate of the lithium is affected. Therefore, as a preferable scheme, a salt-washing and water-returning area 12 is arranged behind the desorption area 4, a discharge hole of the salt-washing liquid circulation assembly 7 closest to the raw brine area 2 is connected with the salt-washing and water-returning area 12, and the adsorbent on the salt-washing and water-returning area 12 is leached by the water discharged from the salt-washing liquid circulation assembly 7.
The salt-washing and water-returning area 12 is connected with the solid-liquid mixing mechanism 1 through a conveying belt 13. Specifically, a scraper 103 is arranged at a position on the frame 101 corresponding to the tail of the filter cloth 102, the scraper 103 scrapes off the adsorbent on the filter cloth 102 and then falls on the conveyer belt 13, the conveyer belt 13 is connected with the mixing tank 1a, the adsorbent returns to the mixing tank 1a again to be mixed with brine, lithium salt in the brine is adsorbed, and the adsorbent completes the cycle of adsorption-desorption-re-adsorption.
The salt-washing backwater area 12 comprises a salt-washing backwater vacuum box 14 connected with a belt type vacuum filter 100, the salt-washing backwater vacuum box 14 is connected with a salt-washing recovery solid-liquid separator 16 through a salt-washing backwater conveying assembly 15, and the raw material brine area 2 is connected with a raw material brine solid-liquid separator 18 through a raw material brine conveying assembly 17.
In this embodiment, the solid-liquid separator 16 is one or more of a cloth bag filter, a compact filter, a magnetic separator, a tripodia centrifuge, and a disc separator. When the adsorbent is a magnetic adsorbent, a magnetic separator can be selected, and when the adsorbent is a non-magnetic adsorbent, other solid-liquid separation equipment except the magnetic separator is selected.
The working process of the invention is as follows:
the adsorbent is put into a mixing tank 1a, brine in a salt field is pumped into the mixing tank, the solid-liquid ratio is 1:10-200, and the salt in the brine is adsorbed by the adsorbent under the stirring state according to the selection of the vacuum filter 100 and the salt content of the brine.
The mixture of the adsorbent and the brine is put into a raw brine area 2 from a mixing tank, the brine permeates a filter cloth 102 under the vacuum action of a belt vacuum filter 100, the adsorbent is isolated on the filter cloth 102, the adsorbent reaches a salt washing area 3 along with the transmission of the filter cloth 102, the adsorbent on the filter cloth is eluted by salt washing liquid above the salt washing area 3, the mixed salt in the adsorbent is eluted, the salt washing liquid after the elution treatment returns to a salt washing backwater area 12, and the adsorbent in the salt washing backwater area 12 is eluted, so that the adsorbent adsorbs the filtered adsorbent and lithium salt in the salt washing liquid.
After the adsorbent passing through the salt washing area 3 enters the desorption area 4, the lithium salt in the adsorbent is sucked out after leaching through desorption liquid, and the liquid containing the lithium salt is obtained after being collected through the desorption liquid circulation assembly 10 and can enter the next working procedure for treatment.
The applicant finds through a large number of experiments that for different brine separations, the minimum ventilation of the filter cloth should not be lower than 500L/m < 2 >. S to meet the ideal processing capacity of the belt vacuum filter, and the leakage of the adsorbents under different use conditions is different to a certain extent, but is generally smaller than 10%. At this time, the content of the adsorbent in brine, salt washing liquid and desorption liquid which pass through the filter cloth of the belt type vacuum filter is generally lower than 1%.
The brine with the solid content lower than 1 percent, the salt washing liquid and the desorption liquid are subjected to secondary treatment by a magnetic separator, precise filtering equipment or a ceramic membrane for solid-liquid separation, and then are discharged to a salt pan or enter a post-system for treatment. If the adsorbent contains magnetic substances, the magnetic separator can be used for recycling, and if the adsorbent does not contain magnetic substances, the precise filter equipment or the ceramic membrane can be used for recycling.
The adsorbent filtered by the belt type vacuum filter is subjected to secondary trapping by the magnetic separator, the precise filtering equipment and the ceramic membrane, and then back-flushing is carried out to a water feeding mouth corresponding to the belt type vacuum filter, and further the adsorbent is returned to the adsorption and desorption main body for circulation. The trapping rate of the belt filter to the adsorbent is more than 90%, and the trapping rate of the rear-stage solid-liquid separation equipment to the adsorbent is more than 99.9%, so that the leakage rate of the adsorbent in a single adsorption and desorption cycle is less than 0.01%.
The belt type vacuum filter provided by the invention can realize the rapid washing of the adsorbent with small water quantity, the desorption and regeneration of the adsorbent and the recovery of the washed salt lost lithium. According to the invention, the desorption liquid with the magnesium-lithium ratio smaller than 1:1 and the salt-lithium ratio (TDS/Li) smaller than 10:1 can be obtained, so that the investment and production cost of the subsequent desalting and purifying process are greatly reduced, and finally, the battery grade lithium carbonate or lithium hydroxide can be stably obtained. The new equipment provided by the invention can recover lithium ions lost in the salt washing process, so that the lithium ion recovery rate of more than 80% in the brine adsorption and desorption process is achieved.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention.
Claims (8)
1. The equipment for extracting lithium from brine by an adsorption method comprises a belt vacuum filter (100), and is characterized in that the belt vacuum filter (100) is connected with a solid-liquid mixing mechanism (1) for mixing brine and an adsorbent, a raw material brine area (2), a salt washing area (3) and a desorption area (4) which are connected with each other are sequentially arranged on the belt vacuum filter (100) along the transmission direction of the belt vacuum filter (100), the solid-liquid mixing mechanism (1) is connected with the raw material brine area (2), a first liquid conveying mechanism (5) for conveying salt washing liquid and a second liquid conveying mechanism (6) for conveying desorption liquid are respectively connected with the salt washing area (3) and the desorption area (4),
the first liquid conveying mechanism (5) comprises at least two mutually independent salt washing liquid circulating components (7) which are sequentially connected, different salt washing liquid circulating components (7) are connected one by one from one side close to the desorption zone (4) to the other side,
the second liquid conveying mechanism (6) comprises at least two mutually independent desorption liquid circulating components (10) which are sequentially connected, and different desorption liquid circulating components (10) are connected one by one from one side far away from the salt washing area (3) to the other side.
2. The device for extracting lithium from brine by an adsorption method according to claim 1, wherein a discharge port of a salt washing liquid circulating assembly (7) closest to a raw brine area (2) is connected with the tail of a belt vacuum filter (100), a salt washing liquid conveyor is arranged above the salt washing liquid circulating assembly (7) closest to a desorption area (4), and a discharge port of the salt washing liquid circulating assembly (7) on one side close to the desorption area (4) in each two adjacent salt washing liquid circulating assemblies (7) is arranged above the belt vacuum filter (100) and corresponds to a feed port of the other salt washing liquid circulating assembly (7).
3. The device for extracting lithium from brine by an adsorption method according to claim 2, wherein the brine circulation assembly (7) comprises a brine vacuum box (8) connected with the belt vacuum filter (100) and a brine conveying assembly (9) connected with the brine vacuum box (8), and a discharge hole of the brine conveying assembly (9) on the brine circulation assembly (7) on one side, close to the desorption area (4), of each two adjacent brine circulation assemblies (7) is positioned above the belt vacuum filter (100) and corresponds to the brine vacuum box (8) on the other brine circulation assembly (7).
4. The device for extracting lithium from brine by an adsorption method according to claim 1, wherein a discharge port of a desorption solution circulation assembly (10) closest to the salt washing area (3) is connected with a subsequent finishing working section, a feed port of a desorption solution circulation assembly (10) farthest from the salt washing area (3) is connected with a desorption solution conveyor above a belt vacuum filter (100), and a discharge port of a desorption solution circulation assembly (10) on the side far from the salt washing area (3) in each two adjacent desorption solution circulation assemblies (10) is located above the belt vacuum filter (100) and corresponds to a feed port of another desorption solution circulation assembly (10).
5. The apparatus for extracting lithium from brine by adsorption according to claim 4, wherein the desorption solution circulation unit (10) comprises a desorption solution vacuum box (11) connected with the belt vacuum filter (100), and a desorption solution transportation unit (11 a) connected with the desorption solution vacuum box (11), and the desorption solution transportation unit (11 a) on the desorption solution circulation unit (10) on the side far away from the salt washing area (3) in each two adjacent desorption solution circulation units (10) is positioned above the belt vacuum filter (100) and corresponds to the desorption solution vacuum box (11) on the other desorption solution circulation unit (10).
6. The device for extracting lithium from brine by an adsorption method according to claim 1, further comprising a salt-washing and water-returning area (12) connected with the desorption area (4), wherein a discharge hole of the first liquid conveying mechanism (5) is connected with the salt-washing and water-returning area (12).
7. The device for extracting lithium from brine by an adsorption method according to claim 1, further comprising a salt-washing and water-returning area (12) connected with the desorption area (4), wherein a discharge port of a salt-washing liquid circulation assembly (7) nearest to the raw brine area (2) is connected with the salt-washing and water-returning area (12), and the salt-washing and water-returning area (12) is connected with the solid-liquid mixing mechanism (1) through a conveying belt (13).
8. The device for extracting lithium from brine by an adsorption method according to claim 6 or 7, wherein the brine washing and backwater area (12) comprises a brine washing backwater vacuum box (14) connected with a belt type vacuum filter (100), the brine washing backwater vacuum box (14) is connected with a brine washing recovery solid-liquid separator (16) through a brine washing backwater conveying assembly (15), and the raw brine area (2) is connected with a raw brine solid-liquid separator (18) through a raw brine conveying assembly (17).
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| CN202010645609.XA CN111729350B (en) | 2020-07-07 | 2020-07-07 | Equipment for extracting lithium from brine by adsorption method |
| PCT/CN2021/104835 WO2022007811A1 (en) | 2020-07-07 | 2021-07-06 | Device for extracting lithium from brine by using adsorption method |
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| CN111826531A (en) * | 2020-07-07 | 2020-10-27 | 浙江衢州明德新材料有限公司 | Method for extracting lithium from brine by using powdery adsorbent |
| CN111825152B (en) * | 2020-07-07 | 2022-11-01 | 西宁永正锂业有限公司 | Belt filter and application thereof in adsorption method brine lithium extraction |
| CN111729350B (en) * | 2020-07-07 | 2023-09-08 | 衢州永正锂业科技有限公司 | Equipment for extracting lithium from brine by adsorption method |
| CN114906966A (en) * | 2022-05-11 | 2022-08-16 | 顶峰油脂化工(泰兴)有限公司 | Vacuum belt type salt washing filter and treatment method of salt-containing wastewater |
| CN115261639A (en) * | 2022-07-18 | 2022-11-01 | 西宁永正锂业有限公司 | Nondestructive recovery process, nondestructive recovery device and nondestructive circulation system of powdery adsorbent for lithium extraction from brine |
| CN115744941B (en) * | 2022-11-15 | 2023-10-13 | 江苏万邦达环保科技有限公司 | Salt lake brine adsorption lithium extraction equipment with low-loss adsorbent |
| CN115992315B (en) * | 2023-03-23 | 2023-06-13 | 河北云瑞化工设备有限公司 | Device and method for extracting lithium from salt lake brine with high magnesium-lithium ratio |
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