CN105925800B - The method and apparatus for concentrating lithium leachate - Google Patents
The method and apparatus for concentrating lithium leachate Download PDFInfo
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- CN105925800B CN105925800B CN201610439071.0A CN201610439071A CN105925800B CN 105925800 B CN105925800 B CN 105925800B CN 201610439071 A CN201610439071 A CN 201610439071A CN 105925800 B CN105925800 B CN 105925800B
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 155
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000000706 filtrate Substances 0.000 claims abstract description 54
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 23
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims description 56
- 239000000463 material Substances 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims 1
- 238000003672 processing method Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 19
- 238000004519 manufacturing process Methods 0.000 description 15
- 230000008569 process Effects 0.000 description 12
- 238000001704 evaporation Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 7
- 229910052808 lithium carbonate Inorganic materials 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 230000006872 improvement Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008719 thickening Effects 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000001595 contractor effect Effects 0.000 description 2
- 238000009295 crossflow filtration Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 241001131796 Botaurus stellaris Species 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The method of present invention concentration lithium leachate, the weight/mass percentage composition of soluble lithium salt content >=60000mg/L and water-insoluble in the lithium leachate are not less than 0.1%, concentration lithium including multiple process steps leaches liquid processing method, wherein, the output quantity of the 3rd filtrate can be maintained at by the 3rd described filter plant is not less than 8L/ (m2H) and make it is described concentration lithium leachate in soluble lithium salt content reach more than 130000mg/L.
Description
Technical field
The present invention relates to lithium production field, and in particular to a kind of method and apparatus of concentration lithium leachate.
Background technology
Liquid concentration is that the unit operation of partial solvent is removed from solution, is the part of solute and the uniform mixed liquor of solution
Separation process.Traditional concentration of solution containing salinity typically uses evaporation concentration technique, and evaporation concentration technique is primarily present following
Problem, one is still to cause the yield of subsequent product relatively low containing substantial amounts of solute in the mother liquor after evaporative crystallization；Two be evaporation
Still there are a large amount of impurity to stop in original solution afterwards, cause product purity not high, inferior quality；Three be easy in evaporating concentration process
Cause the thermal decomposition of product, causing the yield of product further reduces；Four be that the whole evaporation process used time is longer, it is higher to consume energy,
So that production cost is greatly increased.In order to solve the technical problem that aforesaid liquid concentration is present, applicant, which contemplates, uses embrane method
Separation concentration technique replaces traditional evaporation concentration technique to concentrate solution containing salinity.But, applicant is had found by studying
Current membrane separating concentration technique can only be directed to containing the not high solution concentration of salinity in actual mechanical process effectively, for height
Salinity can not be concentrated effectively containing mixture solution, it is found by the applicant that be concentrated into saline solns can for general membrane separating method for concentration
The salt content of soluble is that 60000mg/L has reached the concentration limit, also can not further be concentrated even if operating pressure is improved
Go out the higher solution of salt content.However, concentration operation of the high salinity containing mixture solution is exactly frequently necessary in industrial processes
The technological operation of progress, thus need badly a kind of can concentrate method of the high salinity containing mixture solution at present.
For example, relating to the above-mentioned concentration to lithium leachate in lithium production.Lithium is a kind of important strategic
Resource substance, is the indispensable important source material of modern high technology product.Lithium carbonate is the secondary lithium salts of production and lithium metal product
Basic material, thus become the maximum lithium product of consumption in lithium industry, other lithium products are on it all under lithium carbonate
Swim product.The production technology of lithium carbonate can be divided into salt lake bittern according to the difference of raw material sources and extract and ore extraction.At present,
China then mainly uses solid mineral extraction process, and ore extracts lithium mainly using solid lithium ores such as spodumene, lepidolites
Produce lithium carbonate and other lithium products.The with a long history of lithium resource is extracted from ore, technology is also more ripe, main production
There are lime sinter process and sulfuric acid process, wherein sulfuric acid process is the topmost method used at present.Current sulfuric acid process step
It is as follows：Fine grinding, roasting, acidleach, removing calcium and magnesium, filtering, evaporation and concentration, sinker, separating, washing, the drying of lithium ore, wherein going
The concentration of the lithium leachate of gained generally uses evaporating and concentrating process after calcium and magnesium.The applicant's research is found, in above-mentioned technique
Lithium leachate is lithium leachate, and the filtering accuracy that link is filtered when being operated according to above-mentioned processing step is relatively low, lithium after filtering
Impurity content is higher in leachate, causes subsequent product quality relatively low；Being concentrated by evaporation, link duration, thickening efficiency are low, consume
Can be high, cause the cost for producing lithium to greatly increase.The applicant attempts to utilize traditional membrane separating concentration technique replacement above-mentioned
Found during operation, lithium leachate the situation that concentration is stagnated occurs at the very start in concentration in aforesaid operations, even if improving operation pressure
Power also can not be concentrated effectively.
The content of the invention
The technical problems to be solved by the invention are the method for providing a kind of excellent concentration lithium leachate of concentrated effect
And equipment.
In order to solve above-mentioned problem of the prior art, the present invention is realized using following technical scheme：
The method of present invention concentration lithium leachate, soluble lithium salt content >=60000mg/L in the lithium leachate and
The weight/mass percentage composition of water-insoluble is not less than 0.1%, comprises the following steps：
A, by the lithium leachate by filtering particle diameter it is 0.1-50 μm of the first filter plant, wherein, the lithium is leached
Liquid forms the first filtrate after passing through the filter medium of the first filter plant；
B, by second filter plant of first filtrate by interception rate >=99.5% to the material of molecular weight >=1000, its
In, first filtrate forms the second filtrate after passing through the filter medium of the second filter plant；
C, by the second filtrate by molecular weight for 100-1000 materials interception rate >=90% the 3rd filter plant, its
In, second filtrate forms concentration lithium leachate after being stopped by the filter medium of the 3rd filter plant, set through the 3rd filtering
The 3rd filtrate is formed after standby filter medium；
D, the 4th filter plant that the 3rd filtrate is passed through to interception rate >=99.99% to the material of molecular weight≤100, its
In, the 3rd filtrate forms concentration lithium leachate after being stopped by the filter medium of the 4th filter plant, set through the 4th filtering
The 4th filtrate is formed after standby filter medium, the 4th filter plant, which stops the concentration lithium leachate to be formed and is back to the 3rd filtering, to be set
Standby repeat step c；
The output quantity of 3rd filtrate can be maintained at by the 3rd described filter plant is not less than 8L/ (m2H) and make described
Soluble lithium salt content in concentration lithium leachate reaches more than 130000mg/L.
Lithium leachate enters the first filter plant under the driving of pump, and lithium leachate is first in the filtering of the first filter plant
It is lower that the solid matter for removing larger particles of the particle diameter more than 0.1-50 μm, such as sediment of some calcium-magnesium-containings are screened according to particle diameter
Matter, increases coarse filtration operating unit before the filtering of the first filter plant, filters out the large-sized solid particulate matter in liquid containing salinity
Matter, it is to avoid filter medium causes mechanical damage in these volumes the first filter plant of larger solid particulate matter confrontation.From the first mistake
Some impurity that can not be removed, such as one are also screened by above-mentioned particle diameter containing some in the first filtrate obtained by filter equipment filtering
A little colloidal substances, remove the material of molecular weight >=1000 by the molecular weight screening of the second filter plant that to obtain purity higher
Solution.By the filtering of above-mentioned double-filtration equipment, realize the deep purifying to lithium leachate to meet subsequent concentration process
In requirement to lithium leachate.The second filtrate flowed out from the second filter plant can under the operation condition of the 3rd filter plant
Realize that salt content is concentrated into 130000mg/L for 60000mg/L all can also further concentrate, finally give concentration lithium leachate,
It is not in the situation that concentration is stagnated in concentration process.The 3rd filtrate flowed out from the 3rd filter plant passes through the 4th filter plant
Isolated 4th filtrate and concentration lithium leachate, the 4th filtrate are the higher pure water of purity, general up to the pure of ultra-pure water
Degree, the 4th filter plant further increases the yield of lithium.The present invention mainly has some following benefit, and one is that can solve the problem that industry
The technical problem that upper lithium leachate can not be concentrated effectively, is not easy the situation that concentration is stagnated occur in concentration process；Two be on
State the combination operation of two-stage secondary filter and concentration so that final products purity is very high, product yield is high, product quality with
And concentrated effect is all very good；Three are facts have proved under above-mentioned each Parameter Conditions, can be produced in the case where being operated compared with low energy consumption
The product of higher quality, production efficiency is higher, and economic benefit is best.
As the further improvements in methods of above-mentioned concentration lithium leachate, it is suitable that the 3rd filter plant includes at least two
Secondary connected filter, each filter is to molecular weight is interception rate >=90% of 100-1000 materials and keeps the 3rd to filter
The output quantity of liquid is not less than 8L/ (m2·h).Under these conditions, two filters stop to be formed dense by filter medium
The soluble-salt content of contracting lithium leachate is substantially incremented by successively, and keeps the output quantity of the 3rd filtrate, thereby guarantees that concentration effect
Really.The renewal of filtration flux can effectively be realized by increasing the filter quantity of the 3rd filter plant, be more favorable for the second filtrate
Concentration, realize and multistage containing mixture solution of high salinity concentrated, multistage concentration here can use multiple combinations mode, can be with
It is open, semi open model.Using it is open when, formed dense is stopped in the concentration of last filter in the 3rd filter plant
Contracting lithium leachate is flowed directly out, during using semi open model, and the 3rd filter plant last filter concentration stops what is formed
Concentration lithium leachate, which returns to the concentration lithium leachate that its inlet and a upper filter flow out and converged, is again introduced into last mistake
Device is filtered, the thickening efficiency of solution is thus improved.
As the further improvements in methods of above-mentioned concentration lithium leachate, the 3rd filter plant is sequentially connected by two
Filter constitute, the soluble lithium salt content for the concentration lithium leachate that two filters are formed after stopping is followed successively by
130000mg/L、180000mg/L.On this condition, after removal of impurities preferably, products obtained therefrom quality is most for lithium leachate concentrated effect
It is good.
As the further improvements in methods of above-mentioned concentration lithium leachate, the filter medium of the 3rd filter plant by
DTRO films are constituted.The DTRO films are disc tube reverse osmosis (dt-ro) film, are suitable for the highly-saline lithium leachate of processing filtering, are more favorable for
Keep the concentrated, stable of the 3rd filter plant.
As the further improvements in methods of above-mentioned concentration lithium leachate, the filtration temperature of lithium leachate remains at 5
Between DEG C -40 DEG C.Under the temperature conditionss, filtering, the concentration of lithium leachate are more suitable for.
Present invention also offers a kind of equipment for concentrating lithium leachate, including the filtering particle diameter being sequentially connected is 0.1-50 μm
The first filter plant, the second filter plant to interception rate >=99.5% of the material of molecular weight >=1000, be to molecular weight
3rd filter plant of interception rate >=90% of 100-1000 materials, the concentration lithium leachate liquid outlet of the 3rd filter plant is connected with
The 4th filtering that first collection device, the 3rd filtrate liquid outlet are connected with interception rate >=99.99% of the material of molecular weight≤100 is set
Standby, the concentration lithium leachate outlet of the 4th filter plant is connected with the inlet of the 3rd filter plant, in addition to causes lithium
The salt content of pump and measure each link lithium leachate salt content of the leachate along the flowing of filter plant step by step determines device.
As the further improvement of the equipment of above-mentioned concentration lithium leachate, it is suitable that the 3rd filter plant includes at least two
Secondary connected filter, each filter is to molecular weight is interception rate >=90% of 100-1000 materials and keeps concentrating lithium
The output quantity of leachate is not less than 8L/ (m2·h).Under these conditions, Multistage filtering device stops to be formed by filter medium
Concentration lithium leachate soluble-salt content it is substantially incremented by successively, and keep the 3rd filtrate output quantity, thereby guarantee that dense
Contracting effect.The renewal of filtration flux can effectively be realized by increasing the filter quantity of the 3rd filter plant, be more favorable for second
The concentration of filtrate, realizes that, to multistage concentration of the high salinity containing mixture solution, multistage concentration here can use multiple combinations mode,
It can be open, semi open model.
Specifically, using it is open when, the 3rd filter plant include be sequentially connected first level filtering device, two grades of mistakes
Device is filtered, the two-stage filter is provided with the concentration lithium leachate outlet for the leachate discharge of concentration lithium, therefore the 3rd mistake
Two-stage filter concentration is stopped the concentration lithium leachate formed and flowed directly out in filter equipment；During using semi open model, described
Three filter plants include first level filtering device, the two-stage filter being sequentially connected, and the two-stage filter is provided with for dense
The concentration lithium leachate outlet of contracting lithium leachate discharge and the concentration lithium that first level filtering device is back to for concentration lithium leachate
Leachate refluxing opening, the concentration lithium leachate refluxing opening is connected with the inlet of first level filtering device, two-stage filter
Concentrate lithium leachate refluxing opening and be provided with the first valve, the concentration lithium leachate outlet of two-stage filter is provided with the second valve.The
The concentration lithium leachate that two-stage filter concentration obstruction in three filter plants is formed returns to its inlet and filled with upper one filtering
The concentration lithium leachate for putting outflow converges and is again introduced into last filter, reaches and is then exhausted from after concentration salt content, thus
Improve the thickening efficiency of solution.
As the further improvements in methods of above-mentioned concentration lithium leachate, the 3rd filtrate liquid outlet is provided with the 3rd valve
Door, is provided between the dope liquid outlet of the 4th filter plant and the inlet of the 3rd filter plant for the leachate storage of concentration lithium
The pans deposited.The pans can play storage concentration lithium leachate, stablize concentration lithium leaching hydraulic coupling, will concentrate
Lithium leachate is diverted to the effect of other operation link equipment.
Below by way of accompanying drawing and embodiment, the invention will be further described.
Brief description of the drawings
Fig. 1 is the equipment flowsheet schematic diagram of embodiment one in the present invention.
Fig. 2 is the equipment flowsheet schematic diagram of embodiment two in the present invention.
Fig. 3 is the equipment flowsheet schematic diagram of embodiment three in the present invention.
Embodiment
Below by way of method of the high salinity of present invention concentration containing mixture solution and its application in processing lithium leachate to this
Invention is described further, and the lithium leachate removes the leachate after magnesium calcium precipitate for lithium sulfate in lithium carbonate production process,
The weight/mass percentage composition of soluble lithium salt content >=60000mg/L and water-insoluble in the lithium leachate are not less than 0.1%.
As shown in figure 1, the embodiment of the present invention one provides a kind of high method of the salinity containing mixture solution of concentration in processing lithium leaching
The application gone out in liquid, comprises the following steps：
A, in the presence of power set pump 110, lithium leachate first pass around plate-frame filtering device carry out coarse filtration, filter out
Bulky grain solid impurity in lithium leachate, by lithium leachate by filtering the first filter plant 1 that particle diameter is 0.1-50 μm, the
The filter medium that one filter plant 1 is used intercepts material of the particle diameter more than 0.1-50 μm for microfiltration membranes；
B, afterwards through the formation of the first filter plant 1 the first filtrate flow to the interception rate of the material of molecular weight >=1000 >=
99.5% the second filter plant 2, the second filter plant 2 is also using microfiltration membranes as filter medium, and the first filtrate passes through second
Filter medium the second filtrate of formation of filter plant, the impurity such as the colloidal substance of the first filtrate middle-molecular-weihydroxyethyl >=1000 is situated between by filtering
Matter is intercepted and filtered out；
C, by the second filtrate by molecular weight for 100-1000 materials interception rate >=90% the 3rd filter plant, its
In, second filtrate forms concentration lithium leachate after being stopped by the filter medium of the 3rd filter plant, set through the 3rd filtering
The 3rd filtrate is formed after standby filter medium；
D, the 4th filter plant that the 3rd filtrate is passed through to interception rate >=99.99% to the material of molecular weight≤100, its
In, the 3rd filtrate forms concentration lithium leachate after being stopped by the filter medium of the 4th filter plant, set through the 4th filtering
The 4th filtrate is formed after standby 5 filter medium, the 4th filter plant 5 stops the concentration lithium leachate formed and is back to the 3rd filtering
Device repeats steps c；
The output quantity of 3rd filtrate can be maintained at by the 3rd described filter plant is not less than 8L/ (m2H) and make described
Soluble lithium salt content in concentration lithium leachate reaches more than 130000mg/L.
The filter medium of 3rd filter plant is made up of DTRO films.Whole process temperature control equipment is controlled first
The filtration temperature of lithium leachate remains at 40 DEG C in filter plant 1, the second filter plant 2, the 3rd filter plant 3.First
The filter plant 2 of filter plant 1 and second uses end-filtration mode or cross-flow filtration mode.3rd filter plant 3 can be with
For single filter, each filter is to molecular weight is interception rate >=90% of 100-1000 materials and keeps the 3rd to filter
The output quantity of liquid is not less than 8L/ (m2·h).Lead to after the lithium leachate in the 3rd filter plant 3 is concentrated into target lithium salt content
Cross the first collection device and collect the concentration lithium leachate, the concentration lithium leachate being collected into can temporarily be preserved and can also directly flowed
Entering is used for subsequent production in next link sinker equipment of lithium production technology.4th filtrate of the 4th filter plant 5 outflow is super
Other links of production are used directly for after pure water, collection.
Concentration is carried out to lithium leachate by the above method, concentrated effect is excellent, high lithium salts point solution can be realized
Concentration, the lithium leachate purity of gained is high after concentration, also very high for the lithium carbonate product quality obtained by subsequent production,
Processing procedure can be run compared with low energy consumption, and production cost is low, good in economic efficiency.
You need to add is that, the 3rd filtrate liquid outlet of the 3rd filter plant 3 can be periodically turned off in concentration process
3rd valve 510, then inputs clear water into the 3rd filter plant 3, and clear water enters the 3rd filtering with 1.5-3m/s flow velocity and set
It is standby, it can preferably clear water flow velocity be 2.5-3m/s, continuously be passed through 24-64h, thus, it is possible to play periodic cleaning filter plant, protect
Demonstrate,prove the effect of filter plant filtration flux.
Such as Fig. 1, the present embodiment one additionally provides a kind of equipment for concentrating lithium leachate, including the filtering particle diameter being sequentially connected
For 0.1-50 μm of the first filter plant 1, the second filter plant 2 to interception rate >=99.5% of the material of molecular weight >=1000,
To threeth filter plant 3 of the molecular weight for interception rate >=90% of 100-1000 materials, first filter plant 1, the second mistake
It is cross-flow filtration device and/or end-filtration device, the filter medium of the filter medium of the 3rd filter plant 3 to filter equipment 2
It is made up of DTRO films.The concentration lithium leachate liquid outlet of 3rd filter plant 3 is connected with the first collection device, the 3rd filtrate liquid outlet
It is connected with the 4th filter plant 5 of interception rate >=99.99% of the material of molecular weight≤100, the concentration lithium of the 4th filter plant 5
Leachate outlet is connected with the inlet of the 3rd filter plant 3, in addition to causes lithium leachate along the flowing of filter plant step by step
Pump and the salt content measure device for determining each link lithium leachate salt content.The 3rd filtrate liquid outlet is provided with the 3rd valve
510, it is provided between the dope liquid outlet of the 4th filter plant and the inlet of the 3rd filter plant for concentration lithium leachate
The pans of storage.On this condition, after removal of impurities lithium leachate concentrated effect is best, products obtained therefrom performance optimal.Described
The filter medium of three filter plants is made up of DTRO films.The DTRO films are disc tube reverse osmosis (dt-ro) film, are suitable for processing filtering high
The lithium leachate of salinity, is more favorable for keeping the concentrated, stable of the 3rd filter plant.The concentration lithium of 3rd filter plant 3
Leachate liquid outlet is connected with the first collection device, and first collection device is concentration lithium leachate storage device or sinker dress
Put, concentration lithium leachate can be stored temporarily, follow-up sinker device can also be flowed directly into and carry out sinker operation.
Embodiment two
As shown in Fig. 2 the present embodiment concentrates application and reality of high method of the salinity containing mixture solution in processing lithium leachate
The difference for applying example one is, in the present embodiment the 3rd filter plant 3 include two first level filtering devices 31 being sequentially connected with,
Two-stage filter 32, both the 3rd filtrate liquid outlets converge to be connected with pans 4, what two filters were formed after stopping
The soluble lithium salt content of concentration lithium leachate is followed successively by 130000mg/L, 180000mg/L.Lithium is concentrated in the present embodiment to leach
The equipment of liquid is Open architecture, i.e., the lithium salt content that two-stage filter 32 is isolated from the 3rd filter plant 3 is
180000mg/L concentration lithium leachates flow directly out and are collected for use as subsequent technique.
Embodiment three
As shown in figure 3, the present embodiment concentrates application and reality of high method of the salinity containing mixture solution in processing lithium leachate
The difference for applying example one is,
The equipment for concentrating lithium leachate in the present embodiment in the present embodiment is semi-open type structure, i.e., from the 3rd filter plant 3
The inlet that the lithium salts leachate that middle two-stage filter 22 is isolated returns to first level filtering device 21 is concentrated again, lithium salt content
Reach and flowed out after 180000mg/L.3rd filter plant 2 includes the first level filtering device 31 and two-stage filter being sequentially connected
32, two-stage filter 32 is leached provided with the outlet of concentration lithium salts leachate and concentration lithium salts leachate refluxing opening, concentration lithium salts
Liquid refluxing opening is connected provided with the first valve 310 and with the inlet of first level filtering device 31, in the outlet of concentration lithium salts leachate
Provided with the second valve 320.3rd filtrate liquid outlet of first level filtering device 31 and two-stage filter 32 converge and with pans 4
It is connected.The soluble lithium salt content for the concentration lithium leachate that two filters are formed after stopping be followed successively by 130000mg/L,
180000mg/L.Concrete operations are that line opens the first valve 310, close the second valve 320, the lithium salts of lithium leachate to be concentrated contains
Amount closes the first valve 310 after reaching 180000mg/L, opens the second valve 320 so that concentration lithium leachate is discharged and received
Collection, the 3rd filtrate enters pans 4.On this condition, the present embodiment compared to embodiment one, the lithium leachate of embodiment two it is dense
Contracting effect more preferably, more stablize, for the lithium carbonate product quality obtained by subsequent production also highest by concentration process.
Claims (10)
1. concentrate the soluble lithium salt content >=60000mg/L and water-insoluble in the method for lithium leachate, the lithium leachate
Weight/mass percentage composition be not less than 0.1%, it is characterised in that comprise the following steps：
A, by the lithium leachate by filtering particle diameter it is 0.1-50 μm of the first filter plant (1), wherein, the lithium leachate
The first filtrate is formed after through the filter medium of the first filter plant (1)；
B, by second filter plant (2) of first filtrate by interception rate >=99.5% to the material of molecular weight >=1000, wherein,
First filtrate forms the second filtrate after passing through the filter medium of the second filter plant (2)；
C, by the second filtrate by molecular weight for 100-1000 materials interception rate >=90% the 3rd filter plant (3), its
In, second filtrate forms concentration lithium leachate after being stopped by the filter medium of the 3rd filter plant (3), through the 3rd filtering
The 3rd filtrate is formed after the filter medium of equipment (3)；
D, the 3rd filtrate is passed through the 4th filter plant (5), wherein, the 3rd filtrate is by the filtering of the 4th filter plant (5)
Medium forms concentration lithium leachate after stopping, through the filter medium of the 4th filter plant after be formed as the 4th filter of ultra-pure water
Liquid, the 4th filter plant (5) stops the concentration lithium leachate formed and is back to the 3rd filter plant (3) repeat step c；
The output quantity of 3rd filtrate is maintained at by the 3rd described filter plant (3) is not less than 8L/ (m2H) and the concentration is made
Soluble lithium salt content in lithium leachate reaches more than 130000mg/L.
2. the method for lithium leachate is concentrated as claimed in claim 1, it is characterised in that the 3rd filter plant (3) includes
At least two filters being sequentially connected, each filter to molecular weight for 100-1000 materials interception rate >=90% and
The output quantity of the 3rd filtrate is kept to be not less than 8L/ (m2·h)。
3. the method for lithium leachate is concentrated as claimed in claim 2, it is characterised in that the 3rd filter plant (3) is by two
The individual filter being sequentially connected is constituted, the soluble lithium salt content for the concentration lithium leachate that two filters are formed after stopping
It is followed successively by 130000mg/L, 180000mg/L.
4. the method for lithium leachate is concentrated as claimed in claim 1, it is characterised in that the mistake of the 3rd filter plant (3)
Filter medium is made up of DTRO films.
5. the method for lithium leachate is concentrated as claimed in claim 1, it is characterised in that the filtration temperature of lithium leachate is protected all the time
Hold between 5 DEG C -40 DEG C.
6. concentrate the equipment of lithium leachate, it is characterised in that the filtering particle diameter including being sequentially connected is 0.1-50 μm of the first mistake
Equipment (1) is filtered, the second filter plant (2) to interception rate >=99.5% of the material of molecular weight >=1000, is 100- to molecular weight
3rd filter plant (3) of interception rate >=90% of 1000 materials, the concentration lithium leachate liquid outlet of the 3rd filter plant (3) connects
There are the first collection device, the 3rd filtrate liquid outlet to be connected with the 4th filter plant (5) of output ultra-pure water, the 4th filter plant
(5) concentration lithium leachate outlet is connected with the inlet of the 3rd filter plant (3), in addition to causes lithium leachate along mistake step by step
The pump for filtering equipment flowing and the salt content for determining each link lithium leachate salt content determine device.
7. the equipment of lithium leachate is concentrated as claimed in claim 6, it is characterised in that the 3rd filter plant (3) includes
At least two filters being sequentially connected, each filter to molecular weight for 100-1000 materials interception rate >=90% and
The output quantity of concentration lithium leachate is kept to be not less than 8L/ (m2·h)。
8. the equipment of lithium leachate is concentrated as claimed in claim 7, it is characterised in that the 3rd filter plant (3) includes
First level filtering device (31), the two-stage filter (32) being sequentially connected, the two-stage filter (32) are provided with for concentrating
The concentration lithium leachate outlet of lithium leachate discharge.
9. the equipment of lithium leachate is concentrated as claimed in claim 7, it is characterised in that the 3rd filter plant (3) includes
First level filtering device (31), the two-stage filter (32) being sequentially connected, the two-stage filter (32) are provided with for concentrating
The concentration lithium leachate outlet of lithium leachate discharge and the concentration that first level filtering device (31) are back to for concentration lithium leachate
Lithium leachate refluxing opening, the concentration lithium leachate refluxing opening is connected with the inlet of first level filtering device (31), secondary filtration
The concentration lithium leachate refluxing opening of device (32) is provided with the first valve (310), the concentration lithium leachate of two-stage filter (32)
Outlet is provided with the second valve (320).
10. the equipment of lithium leachate is concentrated as claimed in claim 6, it is characterised in that the 3rd filtrate liquid outlet is provided with
3rd valve (510), the concentration lithium immersion liquid liquid outlet of the 4th filter plant (5) and the inlet of the 3rd filter plant (3)
Between be provided with pans (4) for concentration lithium leachate storage.
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