CN107119197A - The method that salt lake carries lithium is carried out using centrifugal extractor - Google Patents
The method that salt lake carries lithium is carried out using centrifugal extractor Download PDFInfo
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- CN107119197A CN107119197A CN201710341625.8A CN201710341625A CN107119197A CN 107119197 A CN107119197 A CN 107119197A CN 201710341625 A CN201710341625 A CN 201710341625A CN 107119197 A CN107119197 A CN 107119197A
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- 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
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- 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
- C22B3/02—Apparatus therefor
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- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
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- 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
Abstract
The method that salt lake carries lithium, including extraction section, pickling section and back extraction section are carried out the invention discloses a kind of application centrifugal extractor.Centrifugal extractor is applied to salt lake and carried after lithium technology by the present invention, can efficiently solve equipment corrosion and the molten damage problem of extractant, and recovery rate can be improved again and the efficiency of work is extracted.The market that salt lake puies forward lithium commercial Application is opened, with good market application foreground.
Description
Technical field
The present invention relates to salt lake Ti Li fields, the side that salt lake carries lithium is carried out more particularly, to a kind of application centrifugal extractor
Method.
Background technology
The main preservation of lithium resource in nature is in granitic pegmatite-type mineral deposit, salt lake bittern, seawater and GEOTHERMAL WATER.According to
Statistics, salt lake bittern lithium resource reserves account for the 70~80% of lithium resource total amount, therefore salt lake bittern carries lithium and will given birth to as lithium salts
The main expansion direction of production.
The process for extracting lithium salts from salt lake bittern both at home and abroad is made a general survey of, mainly there is the precipitation method, extraction, ion exchange
Absorption method, carbonizatin method, calcining leaching method, Xu Shi methods and electroosmose process etc..The wherein precipitation method, extraction, ion exchange adsorption
Study extensively and profoundly with carbonizatin method, be that main salt lake bittern puies forward lithium method, lithium salts is extracted from bittern industrially general
All it is to use evaporation-crystallization-precipitation method, the final products of the method are typically all lithium carbonate.
However, aluminic acid salt precipitation method, which carries lithium, is primarily present big fresh water consumption, carbodiimide solution and roasting leaching liquid evaporation energy consumption
High and carbonic acid sodium waste is more, causes the problems such as production cost is higher, industrial applications are not yet realized so far；High magnesium lithium is directed to recently
The salt lake bittern of ratio puies forward carbonate precipitation method, boron magnesium or boron lithium coprecipitation, two sections of magnesium sinkings of ammonia and ammonium hydrogen carbonate that lithium occurs
The methods such as lithium method are put forward, further expand of still needing is tried or pilot scale investigation, to further perfect.
China's salt lake Brine resources containing lithium have two outstanding features:One is that lithium content is high, and lithium mass concentration is high in bittern
Up to 2.2-3.1g/L；Two be that Mg/Li ratio is high, and than external high decades of times or even hundred times, this brings one to the exploitation of China's lithium resource
Fixed difficulty.Thus, a kind of extractive technique that efficiently separates of lithium resource is worked out, is large-scale development China saline lake lithium resource
It is crucial.For the especially high magnesium chloride Salt-lake brine of bittern, a variety of extractants were once studied both at home and abroad, such as phosphorous organic extraction
Take agent, amine extractant, diketone, ketone, alcohol, crown ether, mixed extractant etc..
It is worthy of note that:The experimental size for proposing lithium research in China with TBP extractions is big and the most deep, from high magnesium lithium
Than being carried in bittern, lithium is maximally efficient, is that the salt lake high Mg/Li ratio bittern with prospects for commercial application puies forward one of lithium method, but single
One with TBP as extractant there are the relatively low defect of extraction efficiency, and the method is serious to equipment corrosion, and extractant is molten
Damage larger and easily environment is polluted.Therefore, a kind of corrosion resistant novel device is developed, is mutually tied with efficient extracting method
Close, be to solve the problems, such as that existing salt lake puies forward the key of lithium.
The content of the invention
In view of this, the purpose of the present invention is to be carried out in view of the shortcomings of the prior art there is provided one kind application centrifugal extractor
The method that salt lake carries lithium, sophisticated equipment is combined with Particular craft, and it is serious to solve the equipment corrosion that salt lake carried during lithium,
Extractant is molten to be damaged larger and easily pollutes problem to environment, while having reached the effect of higher extracted efficiency.
To reach above-mentioned purpose, the present invention uses following technical scheme：
A kind of application centrifugal extractor carries out the method that salt lake carries lithium, comprises the following steps：
(1) extraction section：The salt lake lithium water of pretreatment and extractant are mixed to join Centrifugical extraction using volume ratio as 1: 1-5
Machine is extracted；Temperature is 25-35 DEG C；4-5 stage countercurrents are extracted；The extractant is tributyl phosphate and kerosene, its volume ratio
For tributyl phosphate/kerosene=1: 1-3；
(2) pickling section：By step 1) extraction gained organic phase pickling is carried out in the centrifugal extractor, temperature is 25-
35℃；3-4 stage countercurrents are extracted；The mordant is 3-4mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 3-5:
1；
(3) it is stripped section：By step 2) gained organic phase be stripped in the centrifugal extractor, temperature is 25-
35℃；3-4 stage countercurrents are stripped；Strippant is 4-6mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 8-10:
1。
Further, the pretreatment of the salt lake lithium water is to add excessive FeCl into salt lake lithium water to be extracted3,
Form LiFeCl4。
Further, the volume ratio of the tributyl phosphate and kerosene is tributyl phosphate/kerosene=1: 3.
Further, the centrifugal extractor, including frame, motor, shell, heavy phase weir plate and horizontal cover, the level
Lid and shell are individually fixed in frame, and the side wall of outer shell is provided with heavy out and light phase export, the horizontal cover
Portion is symmetrically arranged with snubber block；The motor is fixed on above horizontal cover；Also include the rotary drum being hung on by axle suspension in horizontal cover,
The rotary drum is fixed on axle by locknut, and the outer wall of described shell is provided with the charging aperture tangent with housing, the charging aperture
Including heavy phase charging aperture and light phase charging aperture, upper inside wall is provided with heavy phase liquid collecting cavity, light phase liquid collecting cavity, and inner wall lower is provided with water conservancy diversion
Leaf, housing bottom inner surface, which is provided with the middle of eddy-current disc, eddy-current disc, is provided with baiting valve；Described axle is customization motor shaft, is motor
Axle is integrally lengthened.
Further, the rotary drum is hung in horizontal cover, its underpart bearing-free, without mechanical seal, and rotary drum is composite wood
Material is molded, and material is polypropylene or perfluoroalkoxy resin.
Further, described shell is the Unitarily molded shaping of composite, and material is polypropylene or perfluoro alkoxy tree
Fat.
Further, the heavy phase weir plate is is divided into multiple segmental arcs, and heavy phase weir plate is spliced by the plurality of segmental arc.
Further, the charging of described centrifugal extractor, heavy out, light phase export use flanged (FLGD) elbow and can
The bellows connection of telescoping tube, pipeline connection is the Unitarily molded shaping of composite, and material is polypropylene or perfluoro alkoxy
Resin.
Described centrifugal extractor heavy out, light phase export are provided with sampling valve, temperature detection mouthful.
In order to improve extraction efficiency, the centrifugal extractor and extraction process of the present invention are effectively combined, We conducted
Substantial amounts of experimental exploring, it is especially desirable to, it is noted that the selection of extractant, the selection of multi-stage counter current extraction test solvent and parameter
Setting, the selection of multistage pickling experiment acid and being set in whole effect of extracting for test parameters be particularly important.Below
Our screenings to extractant, the setting of multi-stage counter current extraction experiment parameter, the setting experiment of multistage pickling experiment parameter are brief
Enumerate and carry out brief analysis.
Experiment 1：The choice experiment of extractant
Selection isopropanol, fluoro β-diketone+TRPO, tributyl phosphate and diluent sulfonated kerosene are used as extractant
Composition, change extractant species and proportioning, carry out pilot plant test.Zymotic fluid and variety classes and the extractant of proportioning are distinguished
30 DEG C are heated to, shake flat experiment is carried out in separatory funnel, after after two-phase completely layering, sampling is detected.Experimental result is as follows：
Shaking flask extraction experiments result under the variety classes extractant of table 1.
It can be seen from the experimental result in table 1：From fluoro β-diketone：TRPO=2:3 as extractant when, extraction
Rate highest is taken, but β-diketone kind of extractants cost is too high, it is impossible to industrial applications are realized, are considered, from TBP：Sulfonation
Kerosene=1:3 extractant system is optimal.
Experiment 2：Multi-stage counter current extraction is tested
It is 160ml/min in flux, volume ratio O/A is 3: 1, and feeding temperature is 35 DEG C, under the operating condition of counter-current extraction,
Using CWL50-M Novel series efficient centrifugal extracters as extraction equipment, change extraction series, observation experiment effect.Will be pre-
Bittern after processing (contains LiFeCl4Solution) and extractant be heated to 35 DEG C, bittern with 40ml/min inlet amount from
The heavy phase charging aperture of extractor enters equipment, and extractant is entered with 120ml/min inlet amount from the light phase charging aperture of extractor
Equipment, after two-phase discharges stabilization, sampling detection, while facilities for observation corrosion condition.Extraction series sets gradually as 1,2,
3rd, 4,5,6, repeat aforesaid operations, experimental result such as table 2.
The multi-stage counter current extraction experimental result of table 2.
| Sequence number | Extract series | Extraction yield/% | Equipment corrosion situation | Separating effect |
| 1 | 1 | 37.94 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
| 2 | 2 | 61.44 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
| 3 | 3 | 75.96 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
| 4 | 4 | 85.02 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
| 5 | 5 | 90.48 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
| 6 | 6 | 90.50 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
It can be seen from the experimental result in upper table：With the increase of extraction series, extraction yield gradually rises, separating effect
Good, after the extraction of 5 stage countercurrents, lithium is with LiFeCl42TBP extracted species form extracts in organic phase, and the extraction yield of lithium is reachable
To 90.48%.The extraction yield of lithium there will be no lifting substantially under higher extraction series, and equipment does not have corrosion condition.
Experiment 3：Multistage pickling experiment
It is 120ml/min in flux, volume ratio O/A is 5: 1, and feeding temperature is 35 DEG C, under the operating condition of counter-current extraction,
Using CWL50-M Novel series efficient centrifugal extracters as extraction equipment, change extraction series, observation experiment effect.Will be through
The load organic phases and 3~4mol/l hydrochloric acid crossed after 5 grades of extractions are heated to 35 DEG C, and load organic phases are with 100ml/min's
Inlet amount enters equipment from the light phase charging aperture of extractor, and hydrochloric acid is with 20ml/min inlet amount from the heavy phase charging aperture of extractor
Into equipment, after two-phase discharges stabilization, facilities for observation corrosion condition.Extraction series is set gradually as 1,2,3,4, in repetition
State operation, experimental result such as table 3.
The multistage pickling experimental result of table 3.
It can be seen from the experimental result in upper table：With the increase of pickling series, equipment does not find any corrosion phenomenon,
No matter high-level or low level extraction, separating effect is good.
Experiment 4：Multi-stage countercurrent back extraction experiment
It is 110ml/min in flux, volume ratio O/A is 10: 1, and feeding temperature is 35 DEG C, the operating condition that countercurrent reextraction takes
Under, using CWL50-M Novel series efficient centrifugal extracters as back extraction taking equipment, change back extraction series, observation experiment effect
Really.Load organic phases and strippant are heated to 35 DEG C, strippant is with 10ml/min inlet amount from the weight of extractor
Phase charging aperture enters equipment, and load organic phases enter equipment from the light phase charging aperture of extractor with 100ml/min inlet amount, treated
Two-phase discharges after stabilization, sampling detection, while facilities for observation corrosion condition.Extraction series is set gradually as 1,2,3,4, repetition
Aforesaid operations, experimental result such as table 4.
The multi-stage countercurrent of table 4. is stripped experimental result
| Sequence number | It is stripped series | Stripping rate/% | Equipment corrosion situation | Separating effect |
| 1 | 1 | 54.52 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
| 2 | 2 | 78.83 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
| 3 | 3 | 90.31 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
| 4 | 4 | 95.68 | Corrosion is not found | Aqueous phase and organic phase are without muddiness |
It can be seen from the experimental result in upper table：By back extraction, lithium in the form of LiCl to enter in aqueous phase.With back extraction
The increase of series, stripping rate gradually rises, and equipment does not find corrosion condition, and good separating effect, is stripped by 4 stage countercurrents
After taking, stripping rate can reach 95.68%, and the LiCl product purities finally given are up to 96.5%.
Experiment 5：Equipment corrosion resistance is tested
It is 160ml/min in flux, volume ratio O/A is 3: 1, and feeding temperature is 35 DEG C, the operating condition of 5 counter-current extractions
Under, CWL-M Novel series efficient centrifugals extracter, conventional centrifugal extracter, mixer-settler is respectively adopted as extraction equipment,
Continuous operation one week, observes each equipment corrosion situation.Experimental result such as table 5：
The equipment corrosion resistance experimental result of table 5.
| Sequence number | Device name | Equipment corrosion situation |
| 1 | Mixer-settler | It is corroded inside cell body, out-of-flatness lines occurs |
| 2 | Conventional centrifugal extracter | Rotary drum is corroded, and a large amount of black and yellow spotting occurs |
| 3 | CWL-M Series Centrifugal extracters | Rotary drum is intact, and any corrosion is not found |
It can be seen from the experimental result in upper table：Traditional extraction equipment all occurs in that different degrees of corrosion, CWL-M systems
Row centrifugal extractor does not find any corrosion, illustrates that the decay resistance of CWL-M Series Centrifugal extracters is optimal.
The beneficial effects of the invention are as follows：
1. the centrifugal extractor that the present invention is provided, which is a kind of new and effective salt lake, puies forward lithium equipment, strong with corrosion resistance,
Delicate structure, the significant advantage such as extraction yield height.Centrifugal extractor housing, rotary drum and pipeline are that composite is integrally molded to
Type, material is polypropylene, and perfluoroalkoxy resin effectively raises the decay resistance of equipment.Centrifugal extractor passes through electricity
Machine drives extraction reactor to carry out extractive reaction, realizes the semi-automatic and integration of extraction, back extraction and pickling, meanwhile, by
In being provided with balancing damping structure used in the present invention on centrifugal extractor, the vibrations of extractive reaction are advantageously reduced, are enhanced whole
The stability of individual machine.
2. the salt lake that the present invention is provided puies forward lithium method, the lithium salts of higher degree, extraction are obtained by extraction, pickling and back extraction
Take stage preferably phosphoric acid tributyl/kerosene=1: 1-3 as extractant, both ensure that higher recovery rate, production is reduced again
Cost, easy to utilize and industrialized production；Pickling and back extraction stage first with the hydrochloric acid of low concentration, then with more highly concentrated
The hydrochloric acid of degree is washed to organic solvent containing lithium, and the impurity that hydrochloric acid is dissolved in organic solvent is removed step by step, lithium salts is improved
Purity.
3. centrifugal extractor is applied to salt lake and carried after lithium technology by the present invention, equipment corrosion and extraction can be efficiently solved
The molten damage problem of agent, can improve recovery rate and extract the efficiency of work again.The market that salt lake puies forward lithium commercial Application is opened, is had
Good market application foreground.
Brief description of the drawings
Fig. 1 is process chart of the invention；
Fig. 2 is the structural representation of centrifugal extractor of the present invention.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
A kind of application centrifugal extractor carries out the method that salt lake carries lithium, comprises the following steps：
(1) extraction section：Excessive FeCl is added into salt lake lithium water to be extracted3, form LiFeCl4Solution；Will
LiFeCl4Solution is mixed to join centrifugal extractor as 1: 1 using volume ratio with extractant and extracted；Temperature is 25 DEG C；4 grades inverse
Stream extraction；Extractant is tributyl phosphate and kerosene, and its volume ratio is, tributyl phosphate/kerosene=1: 1；
(2) pickling section：Step (1) is extracted into gained organic phase pickling is carried out in the centrifugal extractor, mordant is
3mol/l hydrochloric acid；Organic phase and the volume ratio of hydrochloric acid are 3: 1；Temperature is 25 DEG C；3 stage countercurrents are extracted；
(3) it is stripped section：Organic phase obtained by step (2) is stripped in the centrifugal extractor, strippant
For 4mol/l hydrochloric acid；Organic phase and the volume ratio of hydrochloric acid are 8: 1；Temperature is 25 DEG C；3 stage countercurrents are stripped.
As shown in Fig. 2 the centrifugal extractor used in the present invention, including frame 14, motor 1, shell 13, the and of heavy phase weir plate 4
Horizontal cover 2, horizontal cover 2 and shell 13 are individually fixed in frame, and the side wall of shell 13 is provided with heavy out 5 and light phase export
16, the bottom of horizontal cover 2 is symmetrically arranged with snubber block 3；Motor is fixed on the top of horizontal cover 2；The centrifugal extractor of the present invention is also
Including hanging on the rotary drum 12 in horizontal cover 2 by axle 6, rotary drum 12 is fixed on axle 6 by locknut 7, and the outer wall of shell 13 is set
There is the charging aperture 11 tangent with the housing of shell 13, charging aperture 11 includes heavy phase charging aperture and light phase charging aperture, and upper inside wall is provided with
Heavy phase liquid collecting cavity 15, light phase liquid collecting cavity 17, inner wall lower are provided with water conservancy diversion leaf 8, and the bottom interior surface of housing 13 is provided with eddy-current disc 9, whirlpool
Baiting valve 10 is provided with the middle of flow table 9；Its axis 6 is customization motor shaft, is that motor shaft is integrally lengthened.Rotary drum 12 hangs on horizontal cover
On 2, its underpart bearing-free, without mechanical seal, rotary drum 12 is that composite is molded, and material is polypropylene or perfluoro alkoxy
Resin.Shell 13 be the Unitarily molded shaping of composite, material be polypropylene or perfluoroalkoxy resin.Heavy phase weir plate 4 is
Each and every one many segmental arcs are divided into, heavy phase weir plate 4 is spliced by the plurality of segmental arc.Centrifugical extraction machine inlet 11, heavy out 5,
Light phase export 16 is using the bellows connection of flanged (FLGD) elbow and telescopic tube, and pipeline connection is the overall mould of composite
Type is moulded into, material is polypropylene or perfluoroalkoxy resin；Heavy out 5, light phase export 16 are provided with sampling valve, temperature detection
Mouthful.
As Fig. 1 gives the flow chart of one embodiment of the invention.In Fig. 1, (a) is pretreated salt lake halogen
Water (adds FeCl3, solution formation LiFeCl4), provide it in extraction reactor (b), it connects with organic liquid (c) herein
Touch.The raffinate (e) of outflow it will be discharged from extraction reactor (b).What will be flowed out from novel extraction reactor (b) contains chlorine
The organic liquid (d) for changing lithium is provided into pickling extraction reactor (f), it is contacted with the hydrochloric acid (g) provided herein.Will be from acid
Pickling extraction raffinate (h) discharge of outflow in extraction reactor (f) is washed, by pipeline by the organic liquid of the chloride containing lithium after pickling
(i) back extraction device (j) is supplied to, it is contacted with the strippant (k) provided herein.Will be from back extraction device by pipeline
(j) the regeneration organic liquid (l) of outflow, which is provided, in arrives in organic phase storage tank (n), is then recycled to extraction reactor (b)
In, the aqueous solution (m) of outflow is crude product from back extraction device (j), delivers to subsequent processing and carries out removal of impurities and drying.It is described
Extraction reactor (b), pickling extraction reactor (f) and back extraction device (j) are extraction reactor of the present invention.
Embodiment 2
A kind of application centrifugal extractor carries out the method that salt lake carries lithium, comprises the following steps：
(1) extraction section：Excessive FeCl is added into salt lake lithium water to be extracted3, form LiFeCl4Solution；Will
LiFeCl4Solution is mixed to join centrifugal extractor as 1: 5 using volume ratio with extractant and extracted；Temperature is 35 DEG C；5 grades inverse
Stream extraction；The extractant is tributyl phosphate and kerosene, and its volume ratio is, tributyl phosphate/kerosene=1: 3；
(2) pickling section：Step (1) is extracted into gained organic phase pickling is carried out in the centrifugal extractor, mordant is
3-4mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 5: 1；Temperature is 35 DEG C；4 stage countercurrents are extracted；
(3) it is stripped section：Organic phase obtained by step (2) is stripped in the centrifugal extractor, strippant
For 6mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 10: 1；Temperature is 35 DEG C；4 stage countercurrents are stripped.
Wherein the structure of centrifugal extractor is as described in Example 1.The flow of embodiment is as described in Example 1.
Embodiment 3
A kind of application centrifugal extractor carries out the method that salt lake carries lithium, comprises the following steps：
(1) extraction section：Excessive FeCl is added into salt lake lithium water to be extracted3, form LiFeCl4Solution；Will
LiFeCl4Solution is mixed to join centrifugal extractor as 1: 3 using volume ratio with extractant and extracted；Temperature is 30 DEG C；4 grades inverse
Stream extraction；Extractant is tributyl phosphate and kerosene, and its volume ratio is, tributyl phosphate/kerosene=1: 2；
(2) pickling section：Step (1) is extracted into gained organic phase pickling is carried out in the centrifugal extractor, mordant is
3.5mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 4: 1；Temperature is 30 DEG C；3 stage countercurrents are extracted；
(3) it is stripped section：Organic phase obtained by step (2) is stripped in the centrifugal extractor, strippant
For 5mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 9: 1；Temperature is 30 DEG C；3 stage countercurrents are stripped.
Wherein the structure of centrifugal extractor is as described in Example 1.The flow of embodiment is as described in Example 1.
Embodiment 4
A kind of application centrifugal extractor carries out the method that salt lake carries lithium, comprises the following steps：
(1) extraction section：Excessive FeCl is added into salt lake lithium water to be extracted3, form LiFeCl4Solution；Will
LiFeCl4Solution is mixed to join centrifugal extractor as 1: 2 using volume ratio with extractant and extracted；Temperature is 28 DEG C；5 grades inverse
Stream extraction；The extractant is tributyl phosphate and kerosene, and its volume ratio is, tributyl phosphate/kerosene=1: 1；
(2) pickling section：Step (1) is extracted into gained organic phase pickling is carried out in the centrifugal extractor, mordant is
4mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 4: 1；Temperature is 28 DEG C；4 stage countercurrents are extracted；
(3) it is stripped section：Organic phase obtained by step (2) is stripped in the centrifugal extractor, strippant
For 6mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 8: 1；Temperature is 28 DEG C；4 stage countercurrents are stripped.
Wherein the structure of centrifugal extractor is as described in Example 1.The flow of embodiment is as described in Example 1.
Embodiment 5
A kind of application centrifugal extractor carries out the method that salt lake carries lithium, comprises the following steps：
(1) extraction section：Excessive FeCl is added into salt lake lithium water to be extracted3, form LiFeCl4Solution.Will
LiFeCl4Solution is mixed to join centrifugal extractor as 1: 3 using volume ratio with extractant and extracted；Temperature is 32 DEG C；5 grades inverse
Stream extraction；The extractant is tributyl phosphate and kerosene, and its volume ratio is, tributyl phosphate/kerosene=1: 2；
(2) pickling section：Step (1) is extracted into gained organic phase pickling is carried out in the centrifugal extractor, mordant is
4mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 4: 1；Temperature is 32 DEG C；4 stage countercurrents are extracted；
(3) it is stripped section：Organic phase obtained by step (2) is stripped in the centrifugal extractor, strippant
For 5mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 10: 1；Temperature is 32 DEG C；4 stage countercurrents are stripped.
Wherein the structure of centrifugal extractor is as described in Example 1.The flow of embodiment is as described in Example 1.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, this area is common
Other modifications or equivalent substitution that technical staff is made to technical scheme, without departing from technical solution of the present invention
Spirit and scope, all should cover among scope of the presently claimed invention.
Claims (9)
1. a kind of application centrifugal extractor carries out the method that salt lake carries lithium, it is characterised in that comprise the following steps：
（1）Extraction section：The salt lake lithium water of pretreatment and extractant are mixed to join into centrifugal extractor as 1: 1-5 using volume ratio to enter
Row extraction；Temperature is 25-35 DEG C；4-5 stage countercurrents are extracted；The extractant is tributyl phosphate and kerosene, and its volume ratio is, phosphorus
Sour tributyl/kerosene=1: 1-3；
（2）Pickling section：By step 1）Extraction gained organic phase carries out pickling in the centrifugal extractor, and temperature is 25-35 DEG C；
3-4 stage countercurrents are extracted；The mordant is 3-4mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 3-5: 1；
（3）It is stripped section：By step 2）Gained organic phase is stripped in the centrifugal extractor, and temperature is 25-35 DEG C；
3-4 stage countercurrents are stripped；Strippant is 4-6mol/l hydrochloric acid；The organic phase and the volume ratio of hydrochloric acid are 8-10: 1.
2. application centrifugal extractor according to claim 1 carries out the method that salt lake carries lithium, it is characterised in that the salt lake
The pretreatment of lithium water is to add excessive FeCl into salt lake lithium water to be extracted3, form LiFeCl4。
3. application centrifugal extractor according to claim 1 carries out the method that salt lake carries lithium, it is characterised in that the phosphoric acid
The volume ratio of tributyl and kerosene is tributyl phosphate/kerosene=1: 3.
4. application centrifugal extractor according to claim 1 carries out the method that salt lake carries lithium, it is characterised in that the centrifugation
Extracter, including frame（14）, motor（1）, shell (13), heavy phase weir plate（4）With horizontal cover (2), the horizontal cover (2) and outer
Shell (13) is individually fixed in frame (14), and shell (13) side wall is provided with heavy out (5) and light phase export (16), institute
The bottom for stating horizontal cover (2) is symmetrically arranged with snubber block (3)；The motor (1) is fixed on above horizontal cover (2)；Also include logical
The rotary drum (12) that axle (6) is hung in horizontal cover (2) is crossed, the rotary drum (12) is fixed on axle (6) by locknut (7), described
Shell (13) outer wall be provided with the charging aperture (11) tangent with housing, the charging aperture (11) include heavy phase charging aperture and light phase
Charging aperture, upper inside wall is provided with heavy phase liquid collecting cavity (15), light phase liquid collecting cavity (17), and inner wall lower is provided with water conservancy diversion leaf (8), shell
(13) bottom interior surface, which is provided with the middle of eddy-current disc (9), eddy-current disc (9), is provided with baiting valve (10)；Described axle (6) is customization motor
Axle, is that motor shaft is integrally lengthened.
5. application centrifugal extractor according to claim 4 carries out the method that salt lake carries lithium, it is characterised in that the rotary drum
(12) hang in horizontal cover (2), its underpart bearing-free, without mechanical seal, rotary drum (12) is that composite is molded, material
For polypropylene or perfluoroalkoxy resin.
6. application centrifugal extractor according to claim 4 carries out the method that salt lake carries lithium, it is characterised in that described is outer
Shell (13) is the Unitarily molded shaping of composite, and material is polypropylene or perfluoroalkoxy resin.
7. application centrifugal extractor according to claim 4 carries out the method that salt lake carries lithium, it is characterised in that the heavy phase
Weir plate (4) is is divided into multiple segmental arcs, and heavy phase weir plate (4) is spliced by the plurality of segmental arc.
8. application centrifugal extractor according to claim 4 carries out the method that salt lake carries lithium, it is characterised in that the charging
Mouthful（11）, heavy out（5）, light phase export（16）Using the bellows connection of flanged (FLGD) elbow and telescopic tube, pipeline
Connection is the Unitarily molded shaping of composite, and material is polypropylene or perfluoroalkoxy resin.
9. application centrifugal extractor according to claim 4 carries out the method that salt lake carries lithium, it is characterised in that the heavy phase
Outlet（5）, light phase export（16）It is provided with sampling valve, temperature detection mouthful.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108004420A (en) * | 2017-12-08 | 2018-05-08 | 中国科学院青海盐湖研究所 | The technique that lithium is extracted from the bittern of alkalescence containing lithium based on centrifugal extractor |
| CN109082523A (en) * | 2018-09-28 | 2018-12-25 | 中国恩菲工程技术有限公司 | Method centrifugation back extraction equipment and be stripped scandium |
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| CN203816271U (en) * | 2014-04-14 | 2014-09-10 | 郑州天一萃取科技有限公司 | High-flux centrifugal extractor |
| CN106075952A (en) * | 2016-07-25 | 2016-11-09 | 郑州天萃取科技有限公司 | Centrifugal extractor rotary drum and the manufacture method of this rotary drum |
| CN106337138A (en) * | 2016-11-03 | 2017-01-18 | 深圳市捷鑫资产管理有限公司 | Technology for preparing high-purity anhydrous lithium chloride through centrifugal extraction of salt lake brine |
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| CN87103431A (en) * | 1987-05-07 | 1987-11-04 | 中国科学院青海盐湖研究所 | A kind of method of from contain lithium bittern, extracting Lithium chloride (anhydrous) |
| CN203816271U (en) * | 2014-04-14 | 2014-09-10 | 郑州天一萃取科技有限公司 | High-flux centrifugal extractor |
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| CN108004420A (en) * | 2017-12-08 | 2018-05-08 | 中国科学院青海盐湖研究所 | The technique that lithium is extracted from the bittern of alkalescence containing lithium based on centrifugal extractor |
| CN108004420B (en) * | 2017-12-08 | 2020-04-28 | 中国科学院青海盐湖研究所 | Centrifugal extractor-based process for extracting lithium from lithium-containing alkaline brine |
| CN109082523A (en) * | 2018-09-28 | 2018-12-25 | 中国恩菲工程技术有限公司 | Method centrifugation back extraction equipment and be stripped scandium |
| CN109082523B (en) * | 2018-09-28 | 2023-07-25 | 中国恩菲工程技术有限公司 | Centrifugal stripping equipment and scandium stripping method |
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Application publication date: 20170901 |