CN106119575A - Box extraction tank is in the application of extraction Lithium from Salt Lake Brine - Google Patents
Box extraction tank is in the application of extraction Lithium from Salt Lake Brine Download PDFInfo
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- CN106119575A CN106119575A CN201610678929.9A CN201610678929A CN106119575A CN 106119575 A CN106119575 A CN 106119575A CN 201610678929 A CN201610678929 A CN 201610678929A CN 106119575 A CN106119575 A CN 106119575A
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- extraction
- lithium
- saponification
- salt
- acid
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Classifications
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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
-
- 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
- C22B3/40—Mixtures
- C22B3/409—Mixtures at least one compound being an organo-metallic compound
-
- 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 invention discloses the application in extraction Lithium from Salt Lake Brine of the box extraction tank, utilize the technique of box extraction tank extraction Lithium from Salt Lake Brine include extraction, washing, back extraction, saponification and wash Suan Wuge great workshop section, obtained industrialized producing technology parameter.Box extraction tank is cheap, has the features such as stable, easy to operate, easy-maintaining；Whole set process has the advantages such as product purity is high, the response rate is high, production cost is low, the strip liquor obtained through simple oil removing, evaporation, crystallisation by cooling, filter, dry after, can obtain the industrial grade methanol product that purity is more than 99.6%, this technique is easily in Chaidamu of Qinghai Province popularization and application.
Description
Technical field
The present invention relates to the application at extraction Lithium from Salt Lake Brine of a kind of box extraction tank.
Background technology
The saline lake lithium resource of Chaidamu Basin, Qinghai Province is the abundantest, mainly has chloride type and sulfate type, wherein association
The content of magnesium is the highest, magnesium/lithium ratio (mass ratio) up to 40～1200 in salt.Owing to the chemical property of magnesium, lithium is closely similar, make
Separation and Extraction lithium is the most difficult, be referred to as technical bottleneck and govern Qinghai salt for a long time and carry lithium industrial expansion.High Mg/Li ratio
The extraction of saline lake lithium resource is also a global difficult problem, for many years, domestic and international many companies, put into huge fund, to high Mg/Li ratio salt
Lake bittern water carries lithium and is studied for a long period of time, does not all make a breakthrough, and the mainly production cost of product is high.High Mg/Li ratio salt to be realized
Lake proposes the industrialization of lithium, and product cost is it is necessary to have international competitiveness, good product quality, operating process are simple, be suitable for working as
Ground condition.
Extract from salt lake bittern at present the method for separating Li mainly have the sedimentation method, resin adsorption method, calcining leaching method, half
Permeable membrane dialysis, solvent extraction etc..The sedimentation method are primarily adapted for use in magnesium/lithium ratio (mass ratio) salt less than 10, are not suitable for green grass or young crops
The salt lake in sea.Using resin adsorption method to carry lithium, its technique includes resin absorption, eluting, concentrates, the process such as membrance separation and carbonization.
Owing to salt lithium concentration is relatively low, a large amount of salt need enter resin bed, resin absorption major problem is that water consumption, resin consumption and
Power consumption is very big, simultaneously because resin significantly changes adaptability not to temperature, broken.Calcining leaching method is first by richness lithium halogen
Water high-temperature spray pelletize, then through high temperature sintering, magnesium chloride calcination is become magnesium oxide, the hydrochloric acid mist discharge that simultaneously will generate.High
Temperature burn after pressed powder, be dissolved in water, lithium chloride is dissolved in water, and magnesia crystal is water insoluble, and a large amount of magnesium are by the row of separation
Remove.The problem existed mainly has 3 points: one is that a large amount of dilute hydrochloric acid of by-product reclaims problem, produces several times in carbonic acid in production process
The magnesium chloride of lithium production capacity mass ratio needs to burn into magnesium oxide, and the hydrochloric acid of generation forms acid mist pollution, and a large amount of dilute hydrochloric acid cannot be located
Reason；Two is a large amount of magnesium oxide slags produced in calcining, and owing to containing boron in magnesium slag, magnesium boron separates extremely difficult, forms decades of times
Useless magnesium slag in lithium carbonate cannot utilize；Three is that tile stove equipment corrosion problem is also difficult to solve by the sour environment of high-temperature calcination.
When semipermeable membrane electroosmose process reclaims lithium from salt lake brine with high magnesium-lithium ratio, salt is through univalent anion selectivity exchange membrane and
Valency cation selective exchange membrane carries out electrodialysis, then through continuous circulation process, obtains rich lithium in electrodialyzer enriched chamber
Concentrated solution, substantial amounts of magnesium, sulfate radical, boron etc. is then trapped in diluting compartment, and the solution Mg/Li ratio obtained is about 1:1, needs again
Degree of depth demagging, is eventually adding soda precipitation and produces lithium carbonate product, and the total recovery that there is problems of lithium is relatively low.
Solvent extraction is suitable for low from lithium content and that Mg/Li ratio (Mg/Li) is higher salt carrying lithium, has and can grasp continuously
Make, concentration ratio is high, yield high, product purity advantages of higher, and first extracts boron before extracting lithium, accomplishes comprehensive utilization of resources, great
The market competitiveness, easily promotes the use of.The equipment of enterprise's use that extraction carries lithium is centrifugal extractor at present, and its advantage is main
Have: speed is fast, take that extractant is few, efficiency is high.Shortcoming has: involve great expense, equipment investment volume huge, the machining accuracy of extracter
Not, maintenance difficult, for this equipment can inside this system safety, long-term, stable operation need inspection.
Summary of the invention
It is an object of the present invention to provide and box extraction tank is applied to salt lake bittern carries lithium, get through whole set process flow process, and real
Existing industrialization large-scale production.
It is as follows that the present invention realizes process:
The application in extraction Lithium from Salt Lake Brine of the box extraction tank, Li in described salt+Concentration be (0.5～8) g/L, Mg2+
Concentration be (50～130) g/L, SO4 2-Concentration be (1～50) g/L, Cl-Concentration be (200～350) g/L, Na+Concentration
For (0.5～10) g/L, K+Concentration be (0.1～5) g/L.
Present invention process route includes extraction, washing, back extraction, saponification, washes Suan Wuge great workshop section, wherein: extract 5～8 grades,
Wash 8～12 grades, back extraction 8～12 grades, saponification 2～3 grades；Washing acid 1～2 grade, described salt is salt refined after extracting boron, obtains
Strip liquor through oil removing, evaporation, crystallisation by cooling, filter, dry after obtain anhydrous Lithium chloride.
The each workshop section of the present invention all uses the first grading organic facies of counter-current extraction, i.e. extraction stages, last grading salt；
The first grading load organic phases of washing stage, last grading wash water, the first grading load organic phases of strip stages, finally
One grading hydrochloric acid, the first of saponification stage grading wash organic facies after acid, last grading sodium hydroxide, washes acid phase from the first order
Enter unloaded organic facies, after last grading saponification, remain aqueous phase.
Salt elder generation acid adjustment degree before present invention charging, controlling system pH is 0.01～2.
The present invention feeds front salt ferric chloride to be joined, Fe first3+Molar concentration be Li in salt+Concentration 1～
1.5 again.Reason is Li+Aquation can be big, the surrounding in solution has four hydrones to surround, general extractant be difficult to directly from
Solution extracts lithium, therefore uses before salt charging and add complex salt ferric chloride, then extract complex.Ferric chloride enters organic
Be difficult to the most afterwards elute, rear feeding without joining ferrum.
Extractant used by the present invention is selected from hexanoyl acetone, two pivaloyl ketones, BA, dibenzoyl ketone, thiophene first
Acyl trifluoroacetone, diisobutyl ketone, benzoyltrifluoroacetone, 1,1,2,2,3,3-fluoro heptyl-7,7-dimethyl-4,6-octyl group are double
Ketone, tributyl phosphate, butyl phosphoric acid dibutyl ester, trioctyl phosphine oxide, N, N-bis-(2-ethylhexyl) acrylamide, 1-benzene
Base azo-2-naphthols, incorporation time is 3～10 minutes, and settling time is 10～25 minutes.
Diluent of the present invention is kerosene (including aerial kerosene, sulfonated kerosene) or industrial naptha, diluent and extractant
Volume ratio is (0.1～2): 1.Extraction phase is (0.5～5) than O/A: 1, extraction temperature 25 DEG C～50 DEG C.Temperature is the lowest, and system is glued
Degree is big, and poor fluidity is difficult to mix homogeneously, causes effect of extracting poor；Temperature is too high, and organic facies is volatilized, and loss of extractant is excessive.
Washing stage water of the present invention be strip stages back extraction after liquid, washing compares O/A for (10～30): 1.
Use liquid backflow washing after back extraction, be possible not only to suppress Li+Loss, it is also possible to make the more complete of impurity cationic eluting；
The solution concentration of described back extraction lithium is the hydrochloric acid of (3～8) mol/L, preferably the hydrochloric acid of (5～7) mol/L, and O/A is compared in back extraction
For (10～30): 1；Described saponification uses the sodium hydroxide of (1～6) mol/L, the preferably sodium hydroxide of (3～4) mol/L, saponification
Compare O/A for (0.5～5): 1；Described acid section water of washing is isolated aqueous phase after saponification, washes acid and compares O/A for (0.5～5):
1。
The characteristic of the present invention and innovative point: box extraction tank is successfully applied to salt lake bittern and carries lithium by inventor, gets through
Whole set process flow process, and realize industrialization large-scale production.Box extraction tank has that equipment is simple, cost is low, stable, behaviour
Making the features such as maintenance operation convenient, the later stage is simple, maintenance cost is cheap, the fund alleviating the Enterprise Construction initial stage greatly is thrown
Enter, and box extraction line is more stable effectively for the control of the quality of product.After the present invention uses box extraction tank, yield is high,
The product obtained is high-purity lithium chloride, and the performance of enterprises is good.Whole set process is continuous, production cost is low.
Accompanying drawing explanation
Fig. 1 box extraction tank extraction lithium process chart.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described, and experiment is all on the box extraction tank of 30 grades of 10L
Completing, trough material is PP, uses the hydrochloric acid of (6～7) mol/L during back extraction, and saponification uses the sodium hydroxide of (3～4) mol/L,
The table 1 salt lake, Qinghai used by experiment carries salt composition after boron, joins the Fe of aqueous phase after ferrum3+Concentration is 22.30g/L.
Embodiment 1
As shown in Fig. 1 flow process, this flow experiment incorporation time 5 minutes, settling time 20 minutes, use counter-current extraction, organic facies
It is 50% diisobutyl ketone-20% tributyl phosphate-30% sulfonated kerosene, compares (O/A)=2:1, extract progression 6 grades；(O/ is compared in washing
A)=20:1, washs progression 10 grades；(O/A)=20:1, back extraction progression 10 grades are compared in back extraction；(O/A)=10:1, saponification are compared in saponification
Progression 2 grades；Washing acid and compare (O/A)=2:1, wash acid progression 2 grades, the extraction yield being computed lithium reaches 91.77%.The strip liquor warp obtained
Oil removing, evaporate, cool down, filter, obtain the anhydrous Lithium chloride product that product purity is 99.61% after drying and dewatering, reach GB/T
10575-2007 GB LiCl-0 product index.
Embodiment 2
This flow experiment incorporation time 4 minutes, settling time 16 minutes, use counter-current extraction, organic facies is 30%N, N-bis-(2-
Ethylhexyl) acrylamide-30% tributyl phosphate-40% sulfonated kerosene, compare (O/A)=1:1, extract progression 8 grades；Washing phase
Ratio (O/A)=20:1, washs progression 10 grades；(O/A)=10:1, back extraction progression 8 grades are compared in back extraction；(O/A)=15:1 is compared in saponification,
Saponification progression 2 grades；Washing acid and compare (O/A)=1:1, wash acid progression 2 grades, the extraction yield being computed lithium reaches 95.16%.Obtain is anti-
Extraction liquid through oil removing, evaporate, cool down, filter, obtain the anhydrous Lithium chloride product that product purity is 99.78% after drying and dewatering, reach
GB/T 10575-2007 GB LiCl-0 product index.
Embodiment 3
This flow experiment incorporation time 3 minutes, settling time 12 minutes, use counter-current extraction, organic facies is 65% tricresyl phosphate fourth
Ester-35% sulfonated kerosene, compares (O/A)=1.5:1, extracts progression 7 grades；(O/A)=20:1 is compared in washing, washs progression 10 grades；
(O/A)=20:1, back extraction progression 10 grades are compared in back extraction；(O/A)=8:1, saponification progression 2 grades are compared in saponification；Wash acid compare (O/A)=
1.5:1, washes acid progression 1 grade, and the extraction yield being computed lithium reaches 98.26%.The strip liquor obtained through oil removing, evaporate, cool down, filter,
Obtain the anhydrous Lithium chloride product that product purity is 99.85% after drying and dewatering, reach GB/T 10575-2007 GB LiCl-0
Product index.
Embodiment 4
This flow experiment incorporation time 6 minutes, settling time 24 minutes, use counter-current extraction, organic facies is 30%N, N-bis--(2-
Ethylhexyl) ethyl sulfonamide-20%% tributyl phosphate-50% sulfonated kerosene.Compare (O/A)=1:1, extract progression 8 grades；Washing
Compare (O/A)=10:1, wash progression 10 grades；(O/A)=20:1, back extraction progression 8 grades are compared in back extraction；(O/A)=10 are compared in saponification:
1, saponification progression 3 grades；Washing acid and compare (O/A)=1:1, wash acid progression 1 grade, the extraction yield being computed lithium reaches 95.19%.Obtain is anti-
Extraction liquid through oil removing, evaporate, cool down, filter, obtain the anhydrous Lithium chloride product that product purity is 99.70% after drying and dewatering, reach
GB/T 10575-2007 GB LiCl-0 product index.
Claims (10)
- The application in extraction Lithium from Salt Lake Brine of the most box extraction tank.
- Apply the most according to claim 1, it is characterised in that: Li in described salt+Concentration be (0.5～8) g/L, Mg2+'s Concentration is (50～130) g/L, SO4 2-Concentration be (1～50) g/L, Cl-Concentration be (200～350) g/L, Na+Concentration be (0.5～10) g/L, K+Concentration be (0.1～5) g/L.
- Apply the most according to claim 2, it is characterised in that process route includes extraction, washing, back extraction, saponification, washes acid five Ge great workshop section, wherein: extract 5～8 grades, washs 8～12 grades, back extraction 8～12 grades, saponification 2～3 grades；Wash acid 1～2 grade, described halogen Water for extracting refined salt after boron, the strip liquor obtained through oil removing, evaporation, crystallisation by cooling, filter, dry after obtain anhydrous chlorination Lithium.
- Apply the most according to claim 3, it is characterised in that: each workshop section all uses the first of counter-current extraction, i.e. extraction stages Grading organic facies, last grading salt；The first grading load organic phases of washing stage, last grading wash water, back extraction rank First grading load organic phases of section, last grading hydrochloric acid, the first of saponification stage grading washes organic facies after acid, afterbody Enter sodium hydroxide, wash acid phase from the first grading unloaded organic facies, residue aqueous phase after last grading saponification.
- Apply the most according to claim 3, it is characterised in that: salt elder generation acid adjustment degree before charging, controlling system pH is 0.01 ～2.
- Apply the most according to claim 3, it is characterised in that: salt ferric chloride to be joined before charging, Fe first3+Mole dense Degree is Li in salt+1～1.5 times of concentration.
- Apply the most according to claim 3, it is characterised in that: extractant used is selected from hexanoyl acetone, two pivaloyl ketones, benzene Acyl acetone, dibenzoyl ketone, thenoyltrifluoroacetone, diisobutyl ketone, benzoyltrifluoroacetone, 1,1,2,2,3,3-fluoro heptan Base-7,7-dimethyl-4,6-octyl group diketone, tributyl phosphate, butyl phosphoric acid dibutyl ester, trioctyl phosphine oxide, N, N-bis-(2- Ethylhexyl) acrylamide, 1-phenylazo-2-naphthols.
- Apply the most according to claim 3, it is characterised in that: diluent is kerosene or industrial naptha, diluent and extractant Volume ratio be (0.1～2): 1.
- Apply the most according to claim 3, it is characterised in that: extraction phase is (0.5～5) than O/A: 1, extraction temperature 25 DEG C～ 50℃。
- Apply the most according to claim 3, it is characterised in that: described washing stage water be strip stages back extraction after liquid Body, it is (10～30) that O/A is compared in washing: 1；The solution concentration of back extraction lithium is the hydrochloric acid of (3～8) mol/L, and O/ is compared in back extraction A is (10～30): 1；Saponification uses the sodium hydroxide of (1～6) mol/L, and saponification compares O/A for (0.5～5): 1；Wash acid section to use Water is isolated aqueous phase after saponification, washes acid and compares O/A for (0.5～5): 1.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779612A (en) * | 2017-12-08 | 2018-03-09 | 中国科学院青海盐湖研究所 | A kind of technique that lithium is extracted from alkaline bittern |
| CN107937734A (en) * | 2017-12-08 | 2018-04-20 | 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 mixer-settler |
| 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 |
| CN108018436A (en) * | 2017-12-04 | 2018-05-11 | 青海柴达木兴华锂盐有限公司 | Extract lithium without saponification process |
| CN108149030A (en) * | 2017-11-15 | 2018-06-12 | 青海柴达木兴华锂盐有限公司 | A kind of extraction equipment and extraction process of highly effective integration lithium ion |
| CN109468459A (en) * | 2018-11-20 | 2019-03-15 | 清华大学 | Lithium extractant and the method that lithium is extracted from salt lake bittern |
| WO2019114816A1 (en) * | 2017-12-16 | 2019-06-20 | 虔东稀土集团股份有限公司 | Extraction method for lithium element |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149030A (en) * | 2017-11-15 | 2018-06-12 | 青海柴达木兴华锂盐有限公司 | A kind of extraction equipment and extraction process of highly effective integration lithium ion |
| CN108018436A (en) * | 2017-12-04 | 2018-05-11 | 青海柴达木兴华锂盐有限公司 | Extract lithium without saponification process |
| CN107779612A (en) * | 2017-12-08 | 2018-03-09 | 中国科学院青海盐湖研究所 | A kind of technique that lithium is extracted from alkaline bittern |
| CN107937734A (en) * | 2017-12-08 | 2018-04-20 | 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 mixer-settler |
| 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 |
| CN107779612B (en) * | 2017-12-08 | 2019-12-13 | 中国科学院青海盐湖研究所 | Process for extracting lithium from alkaline brine |
| CN107937734B (en) * | 2017-12-08 | 2020-04-28 | 中国科学院青海盐湖研究所 | Process for extracting lithium from lithium-containing alkaline brine based on mixed clarifying tank |
| 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 |
| WO2019114816A1 (en) * | 2017-12-16 | 2019-06-20 | 虔东稀土集团股份有限公司 | Extraction method for lithium element |
| CN109468459A (en) * | 2018-11-20 | 2019-03-15 | 清华大学 | Lithium extractant and the method that lithium is extracted from salt lake bittern |
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