CN108018436A - Extract lithium without saponification process - Google Patents
Extract lithium without saponification process Download PDFInfo
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- CN108018436A CN108018436A CN201711261414.XA CN201711261414A CN108018436A CN 108018436 A CN108018436 A CN 108018436A CN 201711261414 A CN201711261414 A CN 201711261414A CN 108018436 A CN108018436 A CN 108018436A
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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
- C22B3/20—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
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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
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Abstract
The invention discloses a kind of extraction lithium without saponification process, including extracting, washing, being stripped, washing Suan Sige great workshop sections, 2~10 grades are wherein extracted, washs 0~20 grade, is stripped 2~10 grades, wash 2~10 grades of acid, bittern used is refines bittern after extraction boron, and bittern first adjusts acidity before charging, and control system pH is 0~2, extraction temperature is 25~50 DEG C, and obtained strip liquor directly obtains high-purity anhydrous lithium chloride product after oil removing, evaporation, crystallisation by cooling, filtering, drying.The present invention develop first extraction lithium without saponification process, substantially prolongs the service life of extractant, can be to avoid using expensive sodium hydroxide, while reduce sour consumption, reduce production cost；After removing saponification, whole set process is more easily controlled, operates, can continuous production, there is certain potential industrial production value.
Description
Technical field
The present invention relates to a kind of extraction lithium from salt lake bittern without method for saponification, belong to extraction chemical field.
Background technology
Lithium is mainly used in new energy battery, core becomes power generation, aerospace, medicine as a kind of new strategic energy
Deng field.The existence form of lithium resource has solid mineral and salt lake bittern, and from production cost, salt lake, which carries lithium, has definitely excellent
Gesture.China's saline lake lithium resource enriches, particularly the Caidamu Basin in Qinghai, and reserves are up to 24,470,000 tons（LiCl is counted）.
Extraction is that most promising bittern puies forward one of lithium method, and extractant mainly has acid amides kind of extractants, neutral phosphine
Extractant, ketone extractant, alcohol kind of extractants are come of age ether etc..1979, Qinghai Yanhu Inst., Chinese Academy of Sciences used phosphoric acid
Tributyl-ferric trichloride-kerosene system carries out the expanding test of extraction lithium in big bavin denier salt lake, obtains purity and there was only 98.5% or so
Lithium chloride products.In recent years, studying the extraction system of more and most possible industrialized production is：Amides compound is with
Property phosphorus species（TBP effects are best）As mixed extractant, ferric trichloride does co-extraction agent, and kerosene makees diluent.Such as：
Shanghai organic chemistry institutes of the Chinese Academy of Sciences in 2012 and Qinghai Yanhu Inst., Chinese Academy of Sciences have studied 20% N523（N, N-
Two（2-ethylhexyl）Acetamide）50% sulfonated kerosene systems of -30%TBP-extract lithium from the salt lake brine with high magnesium-lithium ratio of Qinghai
Technique.The extraction yield of three-level counter-current extraction cascade experiment the results show lithium is up to 96%." method that lithium is extracted from salt lake bittern "
（Application number：201410692875.2）In N, (2- the ethylhexyls) -3- butanone of N- bis- acetamide-tributyl phosphate-tri-
Iron chloride-kerosene system, invention improve corrosivity of the tributyl phosphate to extraction equipment of high concentration, and have reached existing
There is the efficiency of technology extraction lithium.
The country carried out industrial experiment or had acid amides kind of extractants applied to industrialized production at present（N503、
N523）, neutral phosphine extractant（TBP）, ketone extractant（DIBK）, the three kinds of extraction systems applied all contain tricresyl phosphate fourth
Ester, and tributyl phosphate plays main extraction, amide substance, which rises, assists phase separation.Due to tributyl phosphate in alkaline condition and
It can degrade on a small quantity under high temperature, if the bad service life that will influence extractant of saponification stage control.
The content of the invention
The present invention is directed to excessive, the destruction extractant, there is provided Yi Zhongcui that saponification easily occurs of saponification section in existing process
Take lithium includes extraction, washing, back extraction and four Ge great workshop sections of sour regurgitation without saponification process, technique.
It is a kind of extract lithium without saponification process, including extract, wash, being stripped, washing Suan Sige great workshop sections, it is characterised in that：
2~10 grades of extraction, 0~20 grade of washing, is stripped 2~10 grades, washes 2~10 grades of acid, and bittern used is refined bittern after extraction boron, into
Bittern first adjusts acidity before material, and control system pH is 0~2, and extraction temperature is 25~50 DEG C, and obtained strip liquor is through oil removing, steaming
Anhydrous lithium chloride product is directly obtained after hair, crystallisation by cooling, filtering, drying.
In above-mentioned no saponification process, 5~8 grades are preferably extracted, washs 8~12 grades, is stripped 8~10 grades, washes 3~6 grades of acid,
Each workshop section uses counter-current extraction, the i.e. grading organic phase of the first of extraction stages, and afterbody is into bittern；The first of washing stage
Grading load organic phases, afterbody is into wash water；First grading load organic phases of strip stages, afterbody is into hydrochloric acid；Wash
Acid phase is from the first grading unloaded organic phase, and afterbody is into remaining water phase after extraction.
In above-mentioned no saponification process, bittern will match somebody with somebody ferric trichloride, Fe before feeding first3+Molar concentration be bittern in Li+
1~2 times of concentration.Ferric trichloride is difficult to elute after entering organic phase, rear feeding without matching somebody with somebody iron.
In above-mentioned no saponification process, extractant used is selected from acid amides kind of extractants, neutral phosphine extractant, ketone extraction
Agent, alcohol kind of extractants are come of age ether extractant；Diluent be selected from kerosene, hydrotreated kerosene, sulfonated kerosene, industrial naptha, diluent with
The volume ratio of extractant is（0.1~2）：1；According to the difference of extractant species, incorporation time is 1~20 minute, settling time
For 10~30 minutes.
In above-mentioned no saponification process, 25 DEG C~50 DEG C of slective extraction temperature.Temperature is too low, and system viscosity is big, poor fluidity,
It is not easy to be uniformly mixed, causes effect of extracting poor；Temperature is excessive, organic phase volatilization, and loss of extractant is excessive.
In above-mentioned no saponification process, it is compared to O/A during extraction（0.5~5）：1；Washing stage is the anti-of back extraction process with water
Extract liquid, wash and be compared to O/A（10~30）：1；The solution concentration of strip stages lithium is the hydrochloric acid of 5~7 mol/L, instead
Extract compared to O/A and be（10~30）：1；The water phase isolated is washed after acid phase is saponification with water, and wash acid is compared to O/A（0.1~
20）：1.
Using liquid reflux washing after back extraction, it can not only suppress Li+Loss, it is also possible to make impurity cationic elute
It is more complete.The ion that washing removes is mainly Mg2+If it is less not wash or wash series, demagging can be increased in post processing
Process, using " two alkaline process "（Sodium carbonate, sodium hydroxide）.
In above-mentioned no saponification process, sour section water aqueous phase acidity after 1~3 grade is washed acid of washing rises, and is washed for lifting
Water, is mutually introduced neutralizing tank by sour effect, after neutralizing part acid, is returned again to wash sour section and carry out next stage and is washed acid；Draw what is neutralized
Number is 1~4 time, is neutralized using magnesium hydroxide, magnesia, lime, sodium hydroxide, ammonium hydroxide, ammonium chloride, the H of water phase after neutralization+
Concentration is 0.01~0.3 mol/L, preferably 0.05~0.1mol/L.
Wherein, organic phase HFeCl after back extraction4·2TBP、HFeCl42N, N represent amide-type, ketone extractant, by washing
Acid gets rid of most acid, washes acid with all or part of water phase for isolating after back extraction, washes and sour is compared to O/A（10~30）：
1.Water that sour section uses is washed mutually after acidity rising, it is necessary to and, after neutralizing part acid, return again in drawing and wash sour section and carry out down
Level-one washes acid.It is 1~4 time to draw the number neutralized, is neutralized using magnesium hydroxide, magnesia, lime, sodium hydroxide, ammonium hydroxide, chlorine
Change ammonium, the H of water phase after neutralizing every time+Concentration is 0.01~0.3 mol/L, then squeezes into next stage and wash sour section.Wash organic phase after acid
Predominantly FeCl3·mTBP、FeCl3NN, realizes the regeneration of organic phase.
In above-mentioned no saponification process, further strip liquor is handled to obtain lithium salts anhydrous lithium chloride or lithium carbonate produces
Product；8-20 grades of series is washed, anhydrous lithium chloride product is obtained after strip liquor evaporation, concentration, crystallization, drying and dehydrating；Wash series 0-7
Grade, the Mg that sodium carbonate removes part is added in strip liquor LiCl solution2+, NaOH depth demaggings are being used, are being eventually adding carbonic acid
Anhydrous Li2CO3 products are obtained after sodium precipitation lithium, washing and dehydration.
In above-mentioned no saponification process, the bittern is sulfate type or chloride type, wherein Li+Concentration be 0.5~8
G/L, Mg2+Ion concentration is 30~130 g/L, SO4 2-Ion concentration is 1~50 g/L, Cl-Ion concentration is 200~350 g/
L, Na+Ion concentration is 0.5~10 g/L, K+Ion concentration is 0.1~5 g/L.
The equipment used is extracted to be box extraction tank, extract centrifuge, centrifugation tower.
Technique used in the present invention removes saponification workshop section, falls acid in organic phase by repeatedly washing acid elution, realizes
The regeneration of organic phase.Wash sour process and increase to 2~10 grades by present 1 grade, washing lotion draws neutralization during washing acid, and neutralization can make
Existing sodium hydroxide is substituted with magnesium hydroxide inexpensively, magnesia, white lime etc..Therefore, this technique is not only prolonged significantly
The service life of extractant has been grown, has also reduced production cost, has easily been promoted the use of in Qaidam area.
The characteristic and innovative point of the present invention：
1. develop first extraction lithium without saponification process, substantially prolongs the service life of extractant, can be to avoid using valency
The more expensive sodium hydroxide of lattice, while reduce sour consumption, reduce production cost；
2. after removing saponification, whole set process is more easily controlled, operates, can continuous production, there is certain potential industrial production valency
Value.
Brief description of the drawings
Fig. 1 is present invention extraction lithium process flow chart.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, and using the hydrochloric acid of 6 mol/L during back extraction, washing acid makes
With the extraction raffinate after the extraction of workshop discharge, extraction raffinate acidity is 0.05.Fig. 1 is present invention extraction lithium process flow chart.Table 1 is real
Test bittern after Qinghai salt lake used carries boron to form, the Fe with water phase after iron3+Concentration is 22.30g/L.
Embodiment 1
65 mLTBP are added in 250 mL separatory funnels and 35 mL kerosene mix in 250 mL separatory funnels, add 100
The upper iron bittern of mL carries out single extraction（Iron in organic phase, Fe：Li=1.5）, stand split-phase, organic phase add 100 mL not on
Iron is extracted except boron bittern, coextraction 4 times（Industrialized production uses multi-stage counter current extraction）.6 M HCl are taken to be added to organic
It is stripped in phase（Industrialized production is stripped using multi-stage countercurrent）, it is stripped 3 times, each 5mL.Organic phase workshop after back extraction
50 mL of raffinate is first washed 1 time, and washing lotion extraction is washed 1 time again after being neutralized to pH=2 with magnesium hydroxide.100 mL workshops are taken to extract boron
Extraction raffinate（Not upper iron bittern）Reextraction is carried out, measures Li in raffinate+Concentration, calculates secondary extraction yield as 67.2%.
Contrast uses sodium hydroxide saponification under same experimental conditions（Saponification degree 75%）, the extracting power of extractant after saponification,
Extraction yield is 62.8%.Illustrate only by 2 grades wash acid can remove be stripped after acid in organic phase, make extractant regeneration.Because not yet
There is washing, obtained strip liquor Mg2+Concentration is higher, and available for lithium carbonate is prepared, preparation process increases demagging process, using " two
After alkaline process " demagging, then sinker is carried out, lithium carbonate is prepared after washing, drying.
Embodiment 2
15 mLN503,35 mLTBP and 50 mL kerosene are added in 250 mL separatory funnels to mix in 250 mL separatory funnels
It is even, add iron bittern on 100mL and carry out single extraction（Iron in organic phase, Fe：Li=1.3）, split-phase is stood, organic phase adds
The not upper iron of 100mL is extracted except boron bittern, coextraction 3 times（Industrialized production uses multi-stage counter current extraction）.It is anti-using workshop
Extract liquid（Li+38.5g/L H+0.551 g/L）Washing 3 times, each 3mL（Industrialized production is washed using multi-stage countercurrent）.Take 7 M
HCl is added in organic phase and is stripped, and is stripped 3 times, each 5mL（Industrialized production is stripped using multi-stage countercurrent）；After back extraction
Organic phase wash 2 times with workshop raffinate, 25 mL every time, after extraction is neutralized to pH=1 with magnesia after the 2nd washing, then
Be introduced to system and carry out third time washing, after extraction is neutralized to pH=1 with magnesia after third time is washed, be re-introduced into system into
The 4th washing of row（Industrialized production is washed using multi-stage countercurrent）, obtain regenerating after washing organic.100 mL workshops are taken to extract boron
Extraction raffinate（Not upper iron bittern）Reextraction is carried out, measures Li in raffinate+Concentration, calculates secondary extraction yield as 55.0%.Say
It is bright only to wash acid by 4 grades and can remove acid after back extraction in organic phase, make extractant regeneration, it is recyclable after extractant regeneration to make
With.Obtained strip liquor can obtain anhydrous lithium chloride product by oil removing, evaporation, concentration, crystallization, dehydration.
Embodiment 3
40 mLDIBK, 10 mLTBP and 50 mL kerosene are added in 250 mL separatory funnels to mix in 250 mL separatory funnels
It is even, add iron bittern on 100mL and carry out single extraction（Iron in organic phase, Fe：Li=1.3）, split-phase is stood, organic phase adds
The not upper iron of 100mL is extracted except boron bittern, coextraction 3 times（Industrialized production uses multi-stage counter current extraction）.5 M HCl are taken to add
Enter and be stripped into organic phase, is stripped 3 times, each 5mL（Industrialized production is stripped using multi-stage countercurrent）；It is organic after back extraction
Mutually washed 1 time, 20 mL with workshop raffinate, after the solution extraction after washing is neutralized to pH=1 with white lime, be re-introduced into system
Wash for the second time, after extraction is neutralized to pH=1 with white lime after second of washing, is re-introduced into system and wash for the third time
Wash（Industrialized production is washed using multi-stage countercurrent）, obtain regenerating after washing organic.100 mL workshops are taken to extract boron extraction raffinate（Not upper iron
Bittern）Reextraction is carried out, measures Li in raffinate+Concentration, calculates secondary extraction yield as 50.1%.Proof only passes through 4 grades
Wash acid can remove be stripped after acid in organic phase, make extractant regeneration, can be recycled after extractant regeneration.Because do not wash
Wash, obtained strip liquor Mg2+Concentration is higher, and available for lithium carbonate is prepared, preparation process increases demagging process, using " two alkaline process "
After demagging, then sinker is carried out, lithium carbonate is prepared after washing, drying.
Claims (8)
1. it is a kind of extract lithium without saponification process, including extract, wash, being stripped, washing Suan Sige great workshop sections, it is characterised in that：Extraction
2~10 grades are taken, washs 0~20 grade, is stripped 2~10 grades, washes 2~10 grades of acid, bittern used is to refine bittern, charging after extracting boron
Bittern first adjusts acidity before, and control system pH is 0~2, and extraction temperature is 25~50 DEG C, obtained strip liquor through oil removing, evaporation,
Anhydrous lithium chloride product is obtained after crystallisation by cooling, filtering, drying.
2. it is according to claim 1 extraction lithium without saponification process, it is characterised in that：5~8 grades of extraction, washing 8~12
Level, is stripped 8~10 grades, washes 3~6 grades of acid, each workshop section uses counter-current extraction, the i.e. grading organic phase of the first of extraction stages, most
Latter grading bittern；The first grading load organic phases of washing stage, afterbody is into wash water；The first of strip stages is grading negative
Organic phase is carried, afterbody is into hydrochloric acid；Acid phase is washed from the first grading unloaded organic phase, afterbody is into remaining water after extraction
Phase.
3. it is according to claim 1 extraction lithium without saponification process, it is characterised in that：Bittern will match somebody with somebody trichlorine before feeding first
Change iron, Fe3+Molar concentration be bittern in Li+1~2 times of concentration.
4. it is according to claim 1 extraction lithium without saponification process, it is characterised in that：Extractant used extracts selected from amide-type
Agent, neutral phosphine extractant, ketone extractant, alcohol kind of extractants is taken to come of age ether extractant；Diluent is selected from kerosene, hydrogenation coal
The volume ratio of oil, sulfonated kerosene, industrial naptha, diluent and extractant is（0.1~2）：1；According to the difference of extractant species,
Incorporation time is 1~20 minute, and settling time is 10~30 minutes.
5. it is according to claim 1 extraction lithium without saponification process, it is characterised in that：It is compared to O/A during extraction（0.5~
5）：1；Washing stage is the back extraction liquid that is stripped process with water, washs and is compared to O/A（10~30）：1；Strip stages lithium it is molten
Liquid concentration is the hydrochloric acid of 5~7 mol/L, is stripped and is compared to O/A（10~30）：1；Wash after acid phase is saponification with water and separate
The water phase gone out, wash acid is compared to O/A（0.1~20）：1.
6. it is according to claim 5 extraction lithium without saponification process, it is characterised in that：It is described to wash sour section water by 1~3
Aqueous phase acidity rises after level washes acid, washes sour effect for lifting, water is mutually introduced neutralizing tank, after neutralizing part acid, returns again to and washes
Sour section carries out next stage and washes acid；It is 1~4 time to draw the number neutralized, is neutralized using magnesium hydroxide, magnesia, lime, hydroxide
Sodium, ammonium hydroxide, ammonium chloride, the H of water phase after neutralization+Concentration is 0.01~0.3 mol/L, preferably 0.05~0.1mol/L.
7. it is according to claim 5 extraction lithium without saponification process, it is characterised in that：Further strip liquor is handled
Obtain lithium salts anhydrous lithium chloride or lithium carbonate product；Wash 8-20 grades of series, strip liquor evaporation, concentration, crystallization, drying and dehydrating
Anhydrous lithium chloride product is obtained afterwards；0-7 grades of series is washed, the Mg that sodium carbonate removes part is added in strip liquor LiCl solution2+,
Using NaOH depth demaggings, anhydrous Li2CO3 products are obtained after being eventually adding sodium carbonate precipitation lithium, washing and dehydration.
8. it is according to claim 5 extraction lithium without saponification process, it is characterised in that：The bittern is sulfate type or chlorine
Compound type, wherein Li+Concentration be 0.5~8 g/L, Mg2+Ion concentration is 30~130 g/L, SO4 2-Ion concentration is 1~50
G/L, Cl-Ion concentration is 200~350 g/L, Na+Ion concentration is 0.5~10 g/L, K+Ion concentration is 0.1~5 g/L
。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439914A (en) * | 2019-01-08 | 2019-03-08 | 安徽工业大学 | A method of the Selective Separation lithium from waste lithium ion cell anode material extract |
| 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 |
| CN110643813A (en) * | 2019-11-08 | 2020-01-03 | 湘潭大学 | Extraction system for separating calcium from calcium-containing brine by using secondary amide/alkyl ketone composite solvent to extract lithium, extraction method and application thereof |
| CN111793755A (en) * | 2020-08-03 | 2020-10-20 | 苏州增华新能源科技有限公司 | Organic phase online purification method and device in lithium extraction process of salt lake and application |
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| CN109439914A (en) * | 2019-01-08 | 2019-03-08 | 安徽工业大学 | A method of the Selective Separation lithium from waste lithium ion cell anode material extract |
| CN110643813A (en) * | 2019-11-08 | 2020-01-03 | 湘潭大学 | Extraction system for separating calcium from calcium-containing brine by using secondary amide/alkyl ketone composite solvent to extract lithium, extraction method and application thereof |
| CN110643813B (en) * | 2019-11-08 | 2021-05-04 | 湘潭大学 | Extraction system for separating calcium from calcium-containing brine by using secondary amide/alkyl ketone composite solvent to extract lithium, extraction method and application thereof |
| CN111793755A (en) * | 2020-08-03 | 2020-10-20 | 苏州增华新能源科技有限公司 | Organic phase online purification method and device in lithium extraction process of salt lake and application |
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