CN107021513A - The method that lithium is extracted from salt lake bittern - Google Patents
The method that lithium is extracted from salt lake bittern Download PDFInfo
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- CN107021513A CN107021513A CN201710248598.XA CN201710248598A CN107021513A CN 107021513 A CN107021513 A CN 107021513A CN 201710248598 A CN201710248598 A CN 201710248598A CN 107021513 A CN107021513 A CN 107021513A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to the method that lithium is extracted from salt lake bittern, belong to bittern and put forward lithium technical field.Present invention solves the technical problem that being to provide the method that lithium is extracted from the relatively low salt lake bittern of lithium concentration.This method comprises the following steps：A, absorption：Aluminium salt and calcium hydroxide solid are sequentially added in salt lake bittern, stirring reaction in the reaction time >=1h, takes precipitation, obtains lithium adsorbed product；B, desorption：By lithium adsorbed product De contamination, lithium solution is obtained.The inventive method, can be relatively low from lithium concentration, and directly absorption carries lithium in the higher bittern of Mg/Li ratio, simple to operate without being evaporated concentration, it is not required that reduce Mg/Li ratio in advance.The formation of adsorbent and the absorption of lithium are carried out simultaneously, eliminate and adsorbent this link is manufactured separately, and raw material is cheap and easy to get, and process route is simple.The adsorption rate of the inventive method lithium is higher, and after conventional desorption, the magnesium lithium mass ratio in desorption liquid is very low.
Description
Technical field
The present invention relates to the method that lithium is extracted from salt lake bittern, belong to bittern and put forward lithium technical field.
Background technology
Since 21 century, lithium and its compound generate electricity and the conjunction of ultralight high intensity lithium in high-energy battery, Aero-Space, nuclear fusion
The fields such as gold are widely applied, and increasingly consequence is occupied in modern industry, thus have 21 century irreplaceable
Energy metal title.The particularly fast development of New Energy Industry, causes the market demand of lithium to sharply increase, lithium resource
Exploitation is particularly important.
Contain very abundant lithium resource in salt lake bittern, account for the 69% of global total amount.Salt lake carries lithium and traditional
Ore carries lithium and compared, with technique is simple, cost is low, efficiency high the features such as.At present, salt lake carries lithium turns into the main attack of lithium industry
Direction, thus obtained lithium product accounts for more than the 80% of global total amount.
However, brine composition is complicated, often coexisted with the different kinds of ions such as Na, K, Mg, Ca, B, the similitude of chemical property causes
Put forward lithium difficulty larger.And the characteristic of high Mg/Li ratio is presented in China salt lake mostly, the magnesium ion that largely exists so that the separation of lithium more
Plus it is difficult, therefore separating magnesium and lithium turns into and puies forward one of main difficult technical of lithium.
At present, bittern, which puies forward the method for lithium, mainly the precipitation method, solvent extraction, absorption method etc..Wherein, absorption method is due to returning
The features such as high income, good selectivity, there is larger superiority compared with other method.Traditional absorption method, is first to prepare
Adsorbent, then add an adsorbent into bittern carry out carry lithium, the preparation of adsorbent is committed step therein.Such as patent application
DE2058910A, which is disclosed, to be used on manganese bioxide ionic sieve selective absorption alkali metal ion from salt lake bittern, ion sieve
H+By Li+、Na+、K+Or Rb+Exchanged from salt lake bittern, patent US5389349A proposes a kind of new adsorbent：Aluminium salt
Type adsorption column, specifically using polymorph A l (OH)3With the LiX (lithium halide, lithium bicarbonate, lithium sulfate) of interlayer, being formed has chi
The very little molecular sieve adsorption post for being not less than 140 Unite States Standards, for reclaiming the lithium chloride in salt lake bittern.These methods are required to list
Adsorbent solely is prepared, its process route is complicated, undoubtedly adds the cost for carrying lithium.
Liu's height etc. carries lithium using aluminum hydroxide precipitation method progress, and (Liu is high, and clock brightness aluminum hydroxide precipitation methods propose the research of lithium
[J] salt industry and chemical industry, 2011,3:25-27), Aluminum Chloride Hexahydrate is first added in magnesium lithium mixed liquor, then that sodium hydroxide is added dropwise is molten
Liquid is so as to carry lithium.This method is applied to the higher bittern of lithium concentration and carries lithium, and still, the lithium content in China's salt lake bittern is relatively low
(typically in hundreds of mg/L scopes), using the method for the document from the relatively low extracting lithium from salt lake brine of lithium concentration, adsorption rate is low.Cause
This, improves lithium concentration, this can undoubtedly increase behaviour if applied this method in China's salt lake bittern, it is necessary to first be concentrated by evaporation
Make.In addition, containing substantial amounts of NaCl in the precipitated product that this method is obtained, it is meant that a large amount of sodium ion absorption are needed in product
To be removed using massive laundering, increase cost.
The content of the invention
For disadvantages described above, directly carried present invention solves the technical problem that being to provide from the relatively low salt lake bittern of lithium concentration
The method for taking lithium.
The method that the present invention extracts lithium from salt lake bittern, comprises the following steps：
A, absorption：Sequentially add aluminium salt and calcium hydroxide solid in salt lake bittern, stirring reaction, the reaction time >=1h,
Precipitation is taken, lithium adsorbed product is obtained；Wherein, in molar ratio, the mol ratio of the lithium in the aluminium and bittern in aluminium salt is 3~5:1；Hydrogen
The mol ratio 6~9 of calcium oxide and the lithium in bittern:1；
B, desorption：By lithium adsorbed product De contamination, lithium solution is obtained.
It is preferred that, the aluminium salt is aluminium chloride, aluminum nitrate or aluminum sulfate.
Further, preferably in molar ratio, the mol ratio of the lithium in the aluminium and bittern in aluminium salt is 4~5:1.
It is preferred that, the reaction time is 2~6h.
Preferably, in molar ratio, the mol ratio of the lithium in the aluminium and bittern in aluminium salt is 4:1, the reaction time is
2h。
Further, it is preferably added to after calcium hydroxide, the pH value of reaction system is 6.6~7.3.
It is preferred that, the Li in the bittern+Concentration is 200~500mg/L, and magnesium lithium mass ratio is 20~50:1.
Further, it is disposable to add in a steps, it is preferred that can be added in salt lake bittern after Aluminum Chloride Hexahydrate dissolving
Calcium hydroxide solid, on the premise of the adsorption effect of the present invention is not influenceed, simplifies operation.
Compared with prior art, the inventive method has the advantages that：
1) the inventive method, can be relatively low from lithium concentration, and directly absorption carries lithium in the higher bittern of Mg/Li ratio, without carrying out
It is concentrated by evaporation, it is not required that reduce Mg/Li ratio in advance, it is simple to operate.
2) formation of adsorbent and the absorption of lithium are carried out simultaneously, eliminate and adsorbent this link is manufactured separately, technique road
Line is simple.
3) adsorption rate of the inventive method lithium is higher, and after conventional desorption, the magnesium lithium mass ratio in desorption liquid is very low, is
0.10 or so.
4) the raw material calcium hydroxide used in the inventive method is cheap and easy to get, and cost is relatively low.
Brief description of the drawings
Fig. 1 is the XRD diffracting spectrums of adsorbed product prepared by the embodiment of the present invention 1~5.
Embodiment
The method that the present invention extracts lithium from salt lake bittern, comprises the following steps：
A, absorption：Sequentially add aluminium salt and calcium hydroxide solid in salt lake bittern, stirring reaction, the reaction time >=1h,
Precipitation is taken, lithium adsorbed product is obtained；Wherein, in molar ratio, the mol ratio of the lithium in the aluminium and bittern in aluminium salt is 3~5:1；Hydrogen
The mol ratio 6~9 of calcium oxide and the lithium in bittern:1；
B, desorption：By lithium adsorbed product De contamination, lithium solution is obtained.
The inventive method, adds aluminium salt and calcium hydroxide in bittern, forms LiCl2Al (OH)3·xH2O, to bittern
In lithium there is high efficiency selected suction-operated, lithium is adsorbed, common desorption method is recycled, by lithium from aluminium lithium compound
In separate, obtain the higher lithium solution of purity.
Aluminium salt commonly used in the art is applied to the present invention, it is preferred that the aluminium salt is aluminium chloride, aluminum nitrate or sulfuric acid
Aluminium.
In the inventive method, the addition of aluminium salt directly determines the growing amount of adsorbent, so as to influence adsorption rate.The present invention
Research finds, with aluminium lithium than increase, lithium adsorption rate significantly improves.When aluminium lithium ratio is 1, the adsorption rate of lithium after 6h is reacted only
For 30%, it means that substantial amounts of lithium stops not utilized in the solution；And when aluminium lithium ratio increases to 4, the adsorption rate of lithium is in 1h
80% just can be inside reached, reaction more than 2h can basically reach balance.It is further continued for increasing aluminium lithium ratio, the adsorption rate of lithium is almost unchanged.
Therefore, aluminium lithium mol ratio is preferably 4~5 in the experimental system of the present invention, and now the adsorption effect of lithium is more satisfactory.
The addition of calcium hydroxide on the absorption of lithium also can output influence, it is preferred that calcium hydroxide and the lithium in bittern
Mol ratio 6~9:1.
Reaction time is also to influence one of key factor of lithium adsorption effect.All things considered, lithium adsorption rate is with the reaction time
Extension and increase.Because the reaction time is longer, adsorbent reacts more abundant with bittern, and adsorption effect is then better.But with
The extension in reaction time, absorption gradually tends to balance, thus the growth of adsorption rate gradually slows down until no longer changing.It is preferred that
, the reaction time is 2~6h.
In addition, absorption reaches that also there are relation the time of balance and aluminium lithium ratio, suitably increasing aluminium lithium ratio can substantially shorten
Reaction reaches the time of balance.In body series, when aluminium lithium ratio is 4, lithium adsorption rate, up to 96.4%, continues to prolong after reaction 2h
Long reaction time, lithium adsorption rate is almost unchanged, illustrates that lithium is carried from bittern under the conditions of this can quickly reach satisfied effect.Cause
This, when aluminium lithium ratio is 4, the reaction time preferably is 2h.
Ca (OH) in the present invention2The formation of adsorbent is not only involved in, also the pH value of control system, pH value directly affects lithium
Adsorption effect.Research finds that when system pH is 6.6~7.3, the adsorption rate of lithium is higher, and is difficult to produce magnesium hydroxide
Precipitation, so as to improve the Selective adsorption of lithium.It is therefore preferable that adding after calcium hydroxide, the pH value of reaction system is 6.6~7.3.
The inventive method, can be relatively low from lithium concentration, and directly absorption carries lithium in the high bittern of Mg/Li ratio, without being evaporated
Concentration improves lithium concentration, it is not required that first precipitates magnesium to reduce Mg/Li ratio, will not can be adsorbed by control ph, magnesium ion in lithium
During precipitate, also will not enter final eluent in.It is preferred that, the Li in the bittern+Concentration be 200~
500mg/L, magnesium lithium mass ratio is 20~50:1；Li more preferably in bittern+Concentration is 500mg/L, and magnesium lithium mass ratio is 20:1.
Further, it is disposable to add in a steps, it is preferred that can be added in salt lake bittern after Aluminum Chloride Hexahydrate dissolving
Calcium hydroxide solid, on the premise of the adsorption effect of the present invention is not influenceed, simplifies operation.
Reaction in a steps of the present invention can be carried out at room temperature, without heating.
In b step, conventional desorption method is applied to the present invention.Such as：Direct 200 DEG C rear washings baked above, are obtained
To lithium-containing solution.
The embodiment of the present invention is further described with reference to embodiment, not therefore by present invention limit
System is among described scope of embodiments.
Embodiment 1
Adopt and extract lithium from bittern with the following method：
It will be equipped with the 250ml salt lake bitterns (Li in the bittern+Concentration is that 500mg/L, magnesium lithium mass ratio are 20) three mouthfuls
Flask is fixed in water-bath device, and it is 25 DEG C to control bath temperature, by the mol ratio 4 of the lithium in Aluminum Chloride Hexahydrate and bittern:1
Added into flask and calcium hydroxide solid 9g is added after Aluminum Chloride Hexahydrate, dissolving (be converted into the lithium in calcium hydroxide and bittern
Mol ratio be 6.75:1), stirring reaction, the reaction time is 2h, and the pH value of system is recorded at the end of reaction, is 6.6.
Centrifuged after reaction, take supernatant to survey its ion concentration, and corresponding adsorption rate is calculated by formula (A), lithium can be obtained
Adsorption rate is 96.4%.
Wherein, CtFor the ion concentration in t hours systems of reaction, C0For the initial concentration of the ion in bittern, unit is
mg/L。
Take precipitation, as lithium adsorbed product, characterized using X-ray diffraction, its collection of illustrative plates is shown in Fig. 1.
It is desorbed after the completion of absorption, the method for use is roasting-WATER-WASHING METHOD, and specific operating parameter is：At 450 DEG C
20min is calcined, then (25 DEG C) washing 10min of room temperature.In obtained eluent, the desorption rate of lithium is more than 95%, magnesium lithium
Mass ratio is 0.10 or so, the value and initial value (>20) compare, substantially reduce.
The absorption of lithium of the different aluminum lithium of embodiment 2 than under
Using the method in embodiment 1, only change the addition of aluminium chloride, the reaction time is respectively 1h, 2h, 4h and 6h,
The adsorption rate of lithium is determined, it the results are shown in Table 1.
The adsorption rate (%) of lithium of the different aluminum lithium of table 1 than under
Note：The scope of reaction end system pH is 6.6-6.8.
The absorption of the lithium of the different calcium hydroxide additions of embodiment 3
Using the method in embodiment 1, only change the addition of calcium hydroxide, the reaction time be respectively 1h, 2h, 4h and
6h, while the adsorbed product to be not added with aluminium reaction 6h under the same conditions determines the adsorption rate of lithium, its result as blank sample
It is shown in Table 2.
The difference Ca of table 2 (OH)2The adsorption rate (%) of lithium under addition
The absorption of lithium in the bittern of the different lithium contents of embodiment 4
Using the method in embodiment 1, only change the initial concentration of lithium in bittern, the reaction time be respectively 1h, 2h, 4h and
6h, determines the adsorption rate of lithium, it the results are shown in Table 3.
The adsorption rate (%) of lithium in the bittern of the different lithium contents of table 3
The absorption of lithium in the bittern of the different Mg/Li ratios of embodiment 5
Using the method in embodiment 1, only change Mg/Li ratio in bittern, the reaction time is respectively 1h, 2h, 4h and 6h, survey
Determine the adsorption rate of lithium, it the results are shown in Table 4.
The adsorption rate (%) of lithium in the bittern of the different Mg/Li ratios of table 4
Comparative example 1
Using document《Aluminum hydroxide precipitation method proposes the research of lithium》(Liu is high, and clock brightness aluminum hydroxide precipitation methods propose the research of lithium
[J] salt industry and chemical industry, 2011,3:Method in 25-27), will carry lithium raw material and replaces with salt lake bittern (halogen in embodiment 1
Li in water+Concentration is that 20) 500mg/L, magnesium lithium mass ratio be.It was found that the bittern for directly using it for low lithium concentration carries lithium, its
Adsorption effect is very poor.Its specific operating method is as follows：
Take the 100mL salt lake bitterns (Li in the bittern+Concentration is that 490mg/L, magnesium lithium mass ratio are 20), to add 4.64g
AlCl3·6H2O, controls 50 DEG C of bath temperature, and sodium hydroxide solution 27mL, 12min is added dropwise and drips off (average 2.25mL/min), instead
Answer 0.5h.(because not indicating when to start timing in document, since No. 1 sample be the timing alkali lye is added dropwise, and is taken after 0.5h for sampling
Sample；No. 2 are the samples taken after the timing since being added alkali lye, 0.5h), centrifuge.12min is differed on both times, it is determined
Adsorption rate, the results are shown in Table 5.
The experimental result of 5 comparative example of table 1
| Sequence number | No. 0 former bittern | No. 1 | No. 2 |
| Lithium concentration (mg/L) | 490 | 370 | 365 |
| Adsorption rate | — | 24.5% | 25.5% |
As can be seen from the above Examples and Comparative Examples, when method of the invention extracts lithium concentration relatively low bittern, lithium is inhaled
Attached rate is still more than 90%, and the adsorption rate of comparative example 1 is only 25.5%, and the adsorption rate of the inventive method is far above comparative example.
To sum up, the inventive method is more suitable for extracting lithium from low lithium bittern, and this also complies with the bittern feature of China.
Claims (8)
1. the method for lithium is extracted from salt lake bittern, it is characterised in that comprise the following steps：
A, absorption：Sequentially add aluminium salt and calcium hydroxide solid in salt lake bittern, stirring reaction, in the reaction time >=1h, it is heavy to take
Form sediment, obtain lithium adsorbed product；Wherein, in molar ratio, the mol ratio of the lithium in the aluminium and bittern in aluminium salt is 3~5:1；Hydroxide
The mol ratio 6~9 of calcium and the lithium in bittern:1；
B, desorption：By lithium adsorbed product De contamination, lithium solution is obtained.
2. the method according to claim 1 that lithium is extracted from salt lake bittern, it is characterised in that：The aluminium salt is chlorination
Aluminium, aluminum nitrate or aluminum sulfate.
3. the method according to claim 1 or 2 that lithium is extracted from salt lake bittern, it is characterised in that：In molar ratio, aluminium salt
In aluminium and bittern in lithium mol ratio be 4~5:1.
4. the method that lithium is extracted from salt lake bittern according to any one of claims 1 to 3, it is characterised in that：During reaction
Between be 2~6h.
5. the method according to claim 4 that lithium is extracted from salt lake bittern, it is characterised in that：In molar ratio, in aluminium salt
Aluminium and bittern in lithium mol ratio be 4:1, the reaction time is 2h.
6. the method that lithium is extracted from salt lake bittern according to any one of Claims 1 to 5, it is characterised in that：A steps
In, add after calcium hydroxide, the pH value of reaction system is 6.6~7.3.
7. the method that lithium is extracted from salt lake bittern according to any one of claim 1~6, it is characterised in that：The salt
Li in lake bittern water+Concentration is 200~500mg/L, and magnesium lithium mass ratio is 20~50:1.
8. the method that lithium is extracted from salt lake bittern according to any one of claim 1~7, it is characterised in that：A steps
In, aluminium salt is added in salt lake bittern, after dissolving, property adds calcium hydroxide solid again.
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Cited By (4)
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| CN112777614A (en) * | 2021-02-02 | 2021-05-11 | 江苏久吾高科技股份有限公司 | Method and device for adsorbing and extracting lithium from salt lake brine |
| CN113086994A (en) * | 2019-12-23 | 2021-07-09 | 财团法人工业技术研究院 | Method for recovering lithium |
| CN113368537A (en) * | 2021-06-28 | 2021-09-10 | 青海盐湖工业股份有限公司 | Method and device for preparing high-lithium mother liquor by using old brine through adsorption method |
| CN115418479A (en) * | 2022-08-16 | 2022-12-02 | 北京万邦达环保技术股份有限公司 | Novel process for extracting lithium from salt lake brine with high magnesium-lithium ratio |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113086994A (en) * | 2019-12-23 | 2021-07-09 | 财团法人工业技术研究院 | Method for recovering lithium |
| CN112777614A (en) * | 2021-02-02 | 2021-05-11 | 江苏久吾高科技股份有限公司 | Method and device for adsorbing and extracting lithium from salt lake brine |
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| CN113368537A (en) * | 2021-06-28 | 2021-09-10 | 青海盐湖工业股份有限公司 | Method and device for preparing high-lithium mother liquor by using old brine through adsorption method |
| CN115418479A (en) * | 2022-08-16 | 2022-12-02 | 北京万邦达环保技术股份有限公司 | Novel process for extracting lithium from salt lake brine with high magnesium-lithium ratio |
| CN115418479B (en) * | 2022-08-16 | 2023-11-10 | 北京万邦达环保技术股份有限公司 | Novel process for extracting lithium from salt lake brine with high magnesium-lithium ratio |
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