CN87103431A - A kind of method of from contain lithium bittern, extracting Lithium chloride (anhydrous) - Google Patents
A kind of method of from contain lithium bittern, extracting Lithium chloride (anhydrous) Download PDFInfo
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- CN87103431A CN87103431A CN87103431.XA CN87103431A CN87103431A CN 87103431 A CN87103431 A CN 87103431A CN 87103431 A CN87103431 A CN 87103431A CN 87103431 A CN87103431 A CN 87103431A
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- lithium
- bittern
- extraction
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- anhydrous
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Abstract
A kind of method of from contain lithium bittern, extracting Lithium chloride (anhydrous).Make extraction agent with tributyl phosphate, complexing agent can recycle in extraction liquid.Can from bittern, directly extract lithium chloride.Three-waste free pollution of the present invention, remarkable in economical benefits, lithium chloride per ton can be made a profit about 8,000 to 10,000 yuan.
Description
The invention belongs to development of resources comprehensive utilization separation and extraction technology.
From bittern, can directly and economically extract lithium chloride and be one of problem that domestic and international scientific worker concentrates on studies.China's salt lake resources is abundant, and the content of lithium is quite high in the bittern, and the lithium resource in the development and use bittern is significant to national economy.No. 3537813 patents of the U.S. have proposed a kind ofly to add iron trichloride in dense bittern, make extraction system extraction lithium with diisobutyl ketone 80%-tributyl phosphate 20%, and the lithium water that enters organic phase is stripped the method that empty organic phase recycles.Owing in anti-stripping agent, contain Licl and Fecl
3, need to add Nacl, to replenish the chlorine root.With two-(2-ethylhexyl) phosphoric acid-tributyl phosphate extraction Fecl
3, water is stripped and is reclaimed molysite again.In Licl and Nacl solution, reclaim lithium salts again.The problem that this method exists is that diisobutyl ketone solubleness in water is big, and the price height; It is loaded down with trivial details that molysite reclaims technical process; The lithium percentage extraction is low, the percentage extraction of seven grades of lithiums only about 80%.The present invention is at these problems, has taked a kind of processing method of directly extracting lithium chloride from dense magnesium bittern highly selective.This law had both improved the yield of lithium, had reduced again and had carried the lithium cost.
Main points of the present invention are with natural energy or fuel bittern evaporation to be concentrated, and separate the salt of separating out, sylvite and vitriol partly, obtain every liter of bittern and contain lithium chloride and reach several grams, and chlorine root concentration reaches 6Mol above high-load lithium, boron, magnesium, chloride soln.This solution is removed after the boron, add any in the complexing agents such as iron trichloride, cupric chloride, zinc chloride, manganous sulfate, nickelous chloride, iron trichloride preferably, solution forms tetrachloro ferrous acid lithium.
Its reaction is:
As extraction agent, it consists of TBP50～70%, thinner 200 with tributyl phosphate (being called for short TBP) in the present invention
#Solvent kerosene 30～50%.During extraction, since P=0 base effect among the TBP, LiFecl
4Enter organic phase, form and consist of LiFecl
4The extracted species of 2TBP, extracted species are distributed in the excessive extraction agent.Extracted species is formed by means of chemical method, ultraviolet spectroscopy and slope method mensuration.The extracting power of coexisting ion when extraction is in proper order: Li
+＞Ca
++＞Na
+＞Mg
++＞K
+＞Rb
+≈ Cs
+Various salting-out agent to the salting-out effect of extraction lithium are in proper order: Alcl
3＞Mgcl
2＞Nacl＞Srcl
2＞NH
4Cl＞Cacl
2This extraction agent extraction ability is stable, and phase-splitting is good, no emulsification phenomenon, and selectivity is strong, and the percentage extraction of lithium remains between the 97%-99% in repeatedly circulating, and coexistent impurity almost reaches whole separation in the bittern, lithium magnesium separation factor reaches 1.87 * 10
5The solubleness of TBP in bittern is more much smaller than pure water.
Solution is after extraction, and the organic phase that contains lithium is washed with dilute hydrochloric acid, removes partly impurity.
Behind acid elution, promptly strip with 6～9MolHcl, Licl enters water, and its reaction is:
Free acid in the organic phase washs with clear water, reclaims hydrochloric acid, uses alkali (caustic alkali, carbonic acid alkali, ammonium or ammoniacal liquor etc.) neutralization H wherein
+, organic phase is recovered the ability of its extraction lithium.Iron is with HFecl
4Form is present in the organic phase, directly recycles in the Returning process.Obviously, this present invention's molysite natural circulation is used, and is conveniently simple and easy than prior art.
Aqueous phase at lithium chloride contains a spot of impurity, as organism, magnesium, boron, sulfate radical, hydrochloric acid etc.Separate hydrochloric acid with the dialysis of film nature; Add LiOHH
2Among the O and spent acid and demagging; Remove most of organism with activated carbon.Then solution evaporation is extremely done, the And calcination, boron forms magnesium borate, separates boron magnesium slag with water extraction.When water logging, add Bacl
2But sulfate radical.Remove impurity as stated above and just obtain refining lithium chloride solution.This solution evaporation to boiling point more than 150 ℃, is discharged oven dry, 250～280 ℃ of dehydrations of what, the cooling fragmentation is the Lithium chloride (anhydrous) product.Lithium chloride purity reaches 99%, and to product, the total recovery of lithium is 90.8% from raw brine.Technical process is as follows:
From block diagram as can be seen, the present invention can directly obtain lithium chloride products from bittern, has changed traditional to add the processing method that hydrochloric acid changes into lithium chloride with lithium hydroxide or Quilonum Retard.
Technical process of the present invention is simple, the extraction agent stable performance, and price is lower, the percentage extraction height.Complexing agent recycles in extraction liquid.Three-waste free pollution of the present invention, remarkable in economical benefits, preresearch estimates lithium chloride price 1.8 per ton～2.0 ten thousand yuan, its cost is then about 10,000 yuan.
The contriver once made a plurality of embodiment.Enumerate three examples below.
Example 1:
Salt lake brine of big bavin dawn of Qinghai takes off boron mother liquor extraction lithium through the saturated magnesium chloride of Exposure to Sunlight, and its mother liquor is formed (mol)
Lithium 0.28～0.31 sodium 0.0734
Magnesium 4.30～4.54 chlorine 9.19
Potassium 0.0155 sulfate radical 0.25
Boron trioxide 0.14 sour 0.12 proportion 1.38
This bittern feeds intake 150 milliliters at every turn.
Extraction agent consists of TBP60%, thinner 200
#Solvent kerosene 40%.Compared (organic phase/water, down with) 1.3: 1, iron lithium mol ratio 1.3: 1, every grade of vibration balancing 10 minutes minutes, the level Four crosscurrent extraction, extraction temperature is room temperature, normal pressure.The raffinate lithium concentration is 0.00199Mol, and the percentage extraction of lithium is more than 99%, and that impurity such as magnesium enter the amount of organic phase is very little, and the organic phase of load lithium suitably after the washing, is stripped with the 6NHcl four-stage counter-current.The strip liquor lithium concentration is that 3.3Mol(is equivalent to every liter and contains lithium chloride 137 gram), magnesium 0.02876Mol, Hcl1.1Mol removes disacidify and magnesium and can produce the Lithium chloride (anhydrous) product.Extraction agent and molysite recycle on stream, and the lithium total yield is more than 98%.
Example 2:
Yunyang, Sichuan well halogen, original bittern is formed (grams per liter):
Li
+0.003732 Mg
++0.2976
Na
+21.3146 Sr
++0.02846
K
+0.2649 Cl
-26.3147
Ca
++1.4502 SO
＝ 44.7318
This well halogen through fuel heating concentrate produce salt, sylvite, boric acid after, its concentrated mother liquor consists of (mol):
Li
+0.181 H
+0.03631
Na
+0.717 Cl
-6.5767
K
+0.406 SO
＝ 40.2285
Ca
++Little B
2O
30.1493
Mg
++3.1292 proportion 1.28
Under normal temperature and pressure conditions, above-mentioned bittern extracts in the extraction tank that stirs for 25 liters.Extraction agent is 60%TBP, and thinner is 200
#Solvent kerosene 40%.Compare 1: 1, iron lithium mol ratio is 1.3: 1, and every grade is vibrated 10 minutes, the level Four extraction, and the percentage extraction of lithium is 97.1%.Strip with 6MolHCl, lithium all enters water, lithium 2.0Mol in the strip liquor, remove small amount of impurities after, produce Lithium chloride (anhydrous), product purity is more than 97.5%, total recovery yield 90.6% of lithium.Molysite and organic phase recycle on stream.
Example 3:
The salt lake brine concentrated solution, the composition (mol) that takes off behind the boron is:
Li
+0.400; Na
+0.0492
K
+0.0167; Mg
++4.563
H
+0.0786 Cl
-9.439
SO
＝ 40.196 B
2O
30.099
1.340/20 ℃ of viscosity 2.801 centipoise proportion
Extraction agent consists of TBP80%, thinner sulfonated kerosene 20%, (2.2 liters of mixing sections) continuous extraction in 20 grades horizontal extraction box, paddle agitator, rotating speed per minute 480 changes 5 grades of extractions, stream is than (organic phase than water, down with) 2: 1,6.58 minutes duration of contact; 5 grades of washings of dilute hydrochloric acid, stream were than 21: 1, and 6.58 minutes duration of contact, 10.6 minutes duration of contact are flowed than 21: 1 in 6 grades of reextraction of 7Mol hydrochloric acid; Clear water is washed acid for 4 grades, stream ratio 24.5: 1,10.6 minutes duration of contact.Day is handled 0.15～0.2 meter in bittern
3, the composition of raffinate (mol) is: Li 0.00399.Strip liquor is formed (mol):
Li
+3.09 Na
+0.00760
K
+0.000321 H
+0.5941
B
2O
30.01231 Cl
-3.991
SO
= 40.000693 1.10/20 ℃ of proportion
Viscosity 1.154 centipoises
Above-mentioned strip liquor borrows the dialysis of film nature to separate hydrochloric acid, after organism is removed in charcoal absorption, adds LiOHH
2O with neutralize remaining acid and precipitate Mg(OH)
2, solution is heating evaporation in enamel chuck evaporating pot, and vacuumizes, and to solution boiling point more than 150 ℃, discharges oven dry, and 450～500 ℃ of calcinations, the cooling back during with water extraction boron and residual magnesium form the magnesium borate residue, add BaCl
2Solution removes SO
= 4, the elimination together of barium sulfate boron magnesium slag.Clear liquid evaporation formality is the same, discharges the back oven dry in evaporating pot, 250～280 ℃ of dehydrations, obtains the Lithium chloride (anhydrous) product, and typical products analysis (weight %) is:
Na
+0.083 Cd
++0.0001
K
+0.006 Zn
++0.0009
Mg
++0.0007 Cu
++0.0001
Cl
-83.62 Fe
+++0.0001
SO
＝ 40.01 Co
++0.0001
B
2O
30.023 Ni
++＜0.0001
H
2O 0.4881 Pb
++0.00016
LiCl is calculated by difference assay, and actual purity is more than 99%.
To product, the total yield of lithium is 90.8% from raw brine.
Claims (5)
1, a kind of processing method of extracting Lithium chloride (anhydrous) from contain lithium bittern, it can add complexing agent in dense bittern, extract lithium with extraction agent, removes impurity with acid elution, through stripping, washing technical process such as acid, oven dry and get Lithium chloride (anhydrous).Feature of the present invention is with tributyl phosphate and thinner 200
#Kerosene is formed extraction agent.
2, in accordance with the method for claim 1, it is characterized in that the composition tributyl phosphate 50～70% of extraction agent, thinner 200
#Solvent kerosene 30～50%.
3, in accordance with the method for claim 1, it is characterized in that complexing agent recycles in extraction liquid, replenish in the middle of need not.
4, in accordance with the method for claim 1, the concentration that it is characterized in that removing with acid elution the acid of impurity is 0.5～2.0Mol.
5, in accordance with the method for claim 1, it is characterized in that the present invention can directly obtain the Lithium chloride (anhydrous) product, need not to change into lithium chloride through pilot processs such as lithium hydroxide or Quilonum Retards.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87103431.XA CN1005145B (en) | 1987-05-07 | 1987-05-07 | Process for extracting absolute lithium chloride from brine containing chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87103431.XA CN1005145B (en) | 1987-05-07 | 1987-05-07 | Process for extracting absolute lithium chloride from brine containing chloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN87103431A true CN87103431A (en) | 1987-11-04 |
| CN1005145B CN1005145B (en) | 1989-09-13 |
Family
ID=4814429
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN87103431.XA Expired CN1005145B (en) | 1987-05-07 | 1987-05-07 | Process for extracting absolute lithium chloride from brine containing chloride |
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|---|---|---|---|---|
| CN102275956A (en) * | 2011-07-21 | 2011-12-14 | 清华大学 | Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio |
| CN102312110A (en) * | 2010-07-09 | 2012-01-11 | 何涛 | Method for extracting alkali metal from salt lake brine and seawater through membrane extraction-back extraction |
| CN102897804A (en) * | 2012-09-18 | 2013-01-30 | 清华大学 | Method for preparing lithium carbonate directly from lithium chloride and carbon dioxide |
| CN104404268A (en) * | 2014-10-31 | 2015-03-11 | 天津科技大学 | Novel co-extraction system for extraction of lithium from high magnesium-lithium ratio bittern and co-extraction method using the same |
| CN105152190A (en) * | 2015-09-18 | 2015-12-16 | 湘潭大学 | Method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium |
| CN105439176A (en) * | 2014-09-28 | 2016-03-30 | 中国科学院上海高等研究院 | Method for extracting high purity lithium salt from high-magnesium lithium-containing bittern |
| CN106119575A (en) * | 2016-08-17 | 2016-11-16 | 青海柴达木兴华锂盐有限公司 | Box extraction tank is in the application of extraction Lithium from Salt Lake Brine |
| CN106219564A (en) * | 2016-08-17 | 2016-12-14 | 青海柴达木兴华锂盐有限公司 | Box extraction tank is the application of boron in extraction salt lake bittern |
| 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 |
| CN106629788A (en) * | 2017-02-13 | 2017-05-10 | 青海盐湖工业股份有限公司 | Production process of lithium chloride |
| WO2017136328A1 (en) * | 2016-02-01 | 2017-08-10 | Northwestern University | Compounds for lithium extraction via ion exchange |
| CN107096384A (en) * | 2017-05-16 | 2017-08-29 | 郑州天萃取科技有限公司 | Lithium isotope is extracted using centrifugal extractor6Li method |
| CN107119197A (en) * | 2017-05-16 | 2017-09-01 | 郑州天萃取科技有限公司 | The method that salt lake carries lithium is carried out using 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 |
| CN108217697A (en) * | 2018-01-31 | 2018-06-29 | 上海易信生物科技有限公司 | A kind of method that high-purity lithium salts is extracted from brine containing lithium |
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|---|---|---|---|---|
| CN102312110A (en) * | 2010-07-09 | 2012-01-11 | 何涛 | Method for extracting alkali metal from salt lake brine and seawater through membrane extraction-back extraction |
| CN102312110B (en) * | 2010-07-09 | 2013-10-09 | 何涛 | Method for extracting alkali metal from salt lake brine and seawater through membrane extraction-back extraction |
| CN102275956B (en) * | 2011-07-21 | 2013-10-16 | 清华大学 | Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio |
| CN102275956A (en) * | 2011-07-21 | 2011-12-14 | 清华大学 | Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio |
| CN102897804A (en) * | 2012-09-18 | 2013-01-30 | 清华大学 | Method for preparing lithium carbonate directly from lithium chloride and carbon dioxide |
| CN105439176A (en) * | 2014-09-28 | 2016-03-30 | 中国科学院上海高等研究院 | Method for extracting high purity lithium salt from high-magnesium lithium-containing bittern |
| CN105439176B (en) * | 2014-09-28 | 2017-10-13 | 中国科学院上海高等研究院 | It is a kind of that the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern |
| CN104404268B (en) * | 2014-10-31 | 2017-05-17 | 天津科技大学 | Novel co-extraction system for extraction of lithium from high magnesium-lithium ratio bittern and co-extraction method using the same |
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| CN105152190A (en) * | 2015-09-18 | 2015-12-16 | 湘潭大学 | Method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium |
| WO2017136328A1 (en) * | 2016-02-01 | 2017-08-10 | Northwestern University | Compounds for lithium extraction via ion exchange |
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| CN108217697A (en) * | 2018-01-31 | 2018-06-29 | 上海易信生物科技有限公司 | A kind of method that high-purity lithium salts is extracted from brine containing lithium |
| CN109574047A (en) * | 2018-10-22 | 2019-04-05 | 天齐锂业（江苏）有限公司 | The method of high-purity Sustiva and lithium chloride is recycled from medicine waste liquid containing lithium |
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| CN109680146A (en) * | 2018-12-19 | 2019-04-26 | 南京工业大学 | A kind of supported liquid membrane mentions lithium device and embrane method brine proposes lithium technique |
| CN115198108A (en) * | 2021-04-13 | 2022-10-18 | 浙江新化化工股份有限公司 | Method for extracting lithium |
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| Publication number | Publication date |
|---|---|
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