CN107021513B - 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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- CN107021513B CN107021513B CN201710248598.XA CN201710248598A CN107021513B CN 107021513 B CN107021513 B CN 107021513B CN 201710248598 A CN201710248598 A CN 201710248598A CN 107021513 B CN107021513 B CN 107021513B
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- lithium
- salt lake
- lake bittern
- aluminium
- brine
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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
-
- 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
-
- 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
-
- 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
Abstract
The present invention relates to the methods that lithium is extracted from salt lake bittern, belong to brine and put forward lithium technical field.The technical problem to be solved by the present invention is to provide the methods that lithium is extracted from the lower salt lake bittern of lithium concentration.This method comprises the following steps：A, it adsorbs：Aluminium salt and calcium hydroxide solid are sequentially added in salt lake bittern, is stirred to react, and the reaction time >=1h takes precipitation, obtains lithium adsorbed product；B, it is desorbed：By lithium adsorbed product De contamination, lithium solution is obtained.The method of the present invention, can be relatively low from lithium concentration, and directly absorption carries lithium in the higher brine of Mg/Li ratio, is concentrated without being evaporated, need not also reduce Mg/Li ratio in advance, easy to operate.The formation of adsorbent and the absorption of lithium are carried out at the same time, and eliminate and adsorbent this link is prepared separately, and raw material is cheap and easy to get, process route is simple.The adsorption rate of the method for the present invention 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 methods that lithium is extracted from salt lake bittern, belong to brine and put forward lithium technical field.
Background technology
Since 21 century, lithium and its compound are closed in high-energy battery, aerospace, nuclear fusion power generation and ultralight high intensity lithium
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 especially 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, accounts for about the 69% of global total amount.Salt lake carry lithium with it is traditional
Ore carries lithium and compares, and has the characteristics that simple for process, at low cost, efficient.Currently, salt lake proposes the main attack that lithium has become lithium industry
Direction, thus obtained lithium product account for 80% or more of global total amount.
However, brine composition is complicated, often coexisted with different kinds of ions such as Na, K, Mg, Ca, B, the similitude of chemical property makes
It is larger to put forward lithium difficulty.And the characteristic of high Mg/Li ratio is presented in China salt lake mostly, a large amount of existing magnesium ions make the separation of lithium more
Add difficulty, therefore separating magnesium and lithium becomes and puies forward one of main difficult technical of lithium.
Currently, the method that brine carries lithium mainly has 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 methods.Traditional absorption method is first to prepare
Adsorbent, then add an adsorbent into brine and carry lithium, the preparation of adsorbent is committed step therein.Such as patent application
DE2058910A discloses using manganese bioxide ionic sieve the selective absorption alkali metal ion from salt lake bittern, on ion sieve
H+By Li+、Na+、K+Or Rb+It is exchanged from salt lake bittern, patent US5389349A proposes a kind of new adsorbent：Aluminium salt
Type adsorption column specifically uses polymorph A l (OH)3With the LiX (lithium halide, lithium bicarbonate, lithium sulfate) of interlayer, being formed has ruler
The very little molecular sieve adsorption column for being not less than 140 Unite States Standards, for recycling the lithium chloride in salt lake bittern.These methods are required to list
Adsorbent is solely prepared, process route is complicated, undoubtedly increases the cost for carrying lithium.
Liu's height etc. using aluminum hydroxide precipitation method carry lithium, 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 to carry lithium.This method carries lithium suitable for the higher brine of lithium concentration, and still, the lithium content in China's salt lake bittern is relatively low
(generally in hundreds of mg/L ranges), using the method for the document from the lower extracting lithium from salt lake brine of lithium concentration, adsorption rate is low.
Therefore, it if applied this method in China's salt lake bittern, needs first to be concentrated by evaporation raising lithium concentration, this can undoubtedly increase behaviour
Make.In addition, containing a large amount of NaCl in the precipitated product that this method obtains, it is meant that a large amount of sodium ions are adsorbed in product, are needed
It to use massive laundering to remove, increase cost.
Invention content
For disadvantages described above, the technical problem to be solved by the present invention is to provide directly carried from the lower salt lake bittern of lithium concentration
The method for taking lithium.
The method that the present invention extracts lithium from salt lake bittern, includes the following steps：
A, it adsorbs：Aluminium salt and calcium hydroxide solid are sequentially added in salt lake bittern, are stirred to react, the reaction time >=1h,
Precipitation is taken, lithium adsorbed product is obtained；Wherein, in molar ratio, the molar ratio of the lithium in the aluminium and brine in aluminium salt is 3~5:1；Hydrogen
The molar ratio 6~9 of calcium oxide and the lithium in brine:1；
B, it is desorbed：By lithium adsorbed product De contamination, lithium solution is obtained.
Preferably, the aluminium salt is aluminium chloride, aluminum nitrate or aluminum sulfate.
Further, preferably in molar ratio, the molar ratio of the lithium in the aluminium and brine in aluminium salt is 4~5:1.
Preferably, the reaction time is 2~6h.
Preferably, in molar ratio, the molar ratio of the lithium in the aluminium and brine in aluminium salt is 4:1, the reaction time is
2h。
Further, after being preferably added to calcium hydroxide, the pH value of reaction system is 6.6~7.3.
Preferably, the Li in the brine+A concentration of 200~500mg/L, magnesium lithium mass ratio are 20~50:1.
Further, in a steps, it is preferred that after Aluminum Chloride Hexahydrate dissolving can be added in salt lake bittern, be added at one time
Calcium hydroxide solid simplifies operation under the premise of not influencing the adsorption effect of the present invention.
Compared with prior art, the method for the present invention has the advantages that：
1) the method for the present invention, can be relatively low from lithium concentration, and directly absorption carries lithium in the higher brine of Mg/Li ratio, without carrying out
It is concentrated by evaporation, need not also reduce Mg/Li ratio in advance, it is easy to operate.
2) formation of adsorbent and the absorption of lithium are carried out at the same time, and eliminate and adsorbent this link is prepared separately, technique road
Line is simple.
3) adsorption rate of the method for the present invention 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 method for the present invention is cheap and easy to get, and cost is relatively low.
Description of the drawings
Fig. 1 is the XRD diffracting spectrums of adsorbed product prepared by the embodiment of the present invention 1~5.
Specific implementation mode
The method that the present invention extracts lithium from salt lake bittern, includes the following steps：
A, it adsorbs：Aluminium salt and calcium hydroxide solid are sequentially added in salt lake bittern, are stirred to react, the reaction time >=1h,
Precipitation is taken, lithium adsorbed product is obtained；Wherein, in molar ratio, the molar ratio of the lithium in the aluminium and brine in aluminium salt is 3~5:1；Hydrogen
The molar ratio 6~9 of calcium oxide and the lithium in brine:1；
B, it is desorbed：By lithium adsorbed product De contamination, lithium solution is obtained.
Aluminium salt and calcium hydroxide is added in the method for the present invention in brine, forms LiCl2Al (OH)3·xH2O, to brine
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 suitable for the present invention, it is preferred that the aluminium salt is aluminium chloride, aluminum nitrate or sulfuric acid
Aluminium.
In the method for the present invention, the addition of aluminium salt directly determines the production quantity of adsorbent, to influence adsorption rate.The present invention
The study found that with aluminium lithium than increase, lithium adsorption rate significantly improves.When aluminium lithium ratio be 1 when, react 6h after lithium adsorption rate only
It is 30%, it means that a large amount of lithium stops not utilized in the solution；And when aluminium lithium ratio increases to 4, the adsorption rate of lithium is in 1h
It just can inside reach 80%, reaction 2h or more can basically reach balance.It is further continued for increasing aluminium lithium ratio, the adsorption rate of lithium is almost unchanged.
Therefore, aluminium lithium molar ratio is preferably 4~5 in the experimental system of the present invention, and the adsorption effect of lithium is more satisfactory at this time.
The addition of calcium hydroxide on the absorption of lithium also can output influence, it is preferred that lithium in calcium hydroxide and brine
Molar ratio 6~9:1.
One of an important factor for reaction time is also influence lithium adsorption effect.All things considered, lithium adsorption rate is with the reaction time
Extension and increase.This is because the reaction time is longer, adsorbent reacts more abundant with brine, 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, which reaches the time of balance and aluminium lithium ratio, also relationship, suitably increasing aluminium lithium ratio can be obviously shortened
Reaction reaches the time of balance.In this system, when aluminium lithium ratio is 4, lithium adsorption rate is up to 96.4% after reaction 2h, after reneing
In the long reaction time, lithium adsorption rate is almost unchanged, illustrates that satisfied effect can be quickly reached by carrying lithium from brine under this condition.Cause
This, when aluminium lithium ratio is 4, the preferred reaction time is 2h.
Ca (OH) in the present invention2It is not only involved in the formation of adsorbent, also the pH value of control system, pH value directly affect lithium
Adsorption effect.The study found that when system pH is 6.6~7.3, the adsorption rate of lithium is higher, and magnesium hydroxide not easy to produce
Precipitation, to improve the Selective adsorption of lithium.It is therefore preferable that after calcium hydroxide is added, the pH value of reaction system is 6.6~7.3.
The method of the present invention, can be relatively low from lithium concentration, and directly absorption carries lithium in the high brine of Mg/Li ratio, without being evaporated
Concentration improves lithium concentration, also need not first precipitate magnesium to reduce Mg/Li ratio, can will not be adsorbed in lithium by control ph, magnesium ion
It precipitates, will not enter in final eluent in the process.Preferably, the Li in the brine+A concentration of 200~
500mg/L, magnesium lithium mass ratio are 20~50:1；Li in more preferable brine+A concentration of 500mg/L, magnesium lithium mass ratio are 20:1.
Further, in a steps, it is preferred that after Aluminum Chloride Hexahydrate dissolving can be added in salt lake bittern, be added at one time
Calcium hydroxide solid simplifies operation under the premise of not influencing the adsorption effect of the present invention.
Reaction in a steps of the present invention can carry out at room temperature, without heating.
In b step, common desorption method is suitable for the present invention.Such as：Direct 200 DEG C rear washings baked above, obtain
To lithium-containing solution.
The specific implementation mode of the present invention is further described with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
Lithium is extracted from brine with the following method：
250ml salt lake bitterns (the Li in the brine will be housed+A concentration of 500mg/L, magnesium lithium mass ratio are three mouthfuls 20)
Flask is fixed in water-bath device, and control bath temperature is 25 DEG C, by the molar ratio 4 of the lithium in Aluminum Chloride Hexahydrate and brine:1
Aluminum Chloride Hexahydrate is added into flask, calcium hydroxide solid 9g is added after dissolving and (is converted into calcium hydroxide and the lithium in brine
Molar ratio be 6.75:1) it, is stirred to react, reaction time 2h, the pH value of system is recorded at the end of reaction, be 6.6.
It is centrifuged after reaction, takes 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 brine, unit is
mg/L。
Precipitation, as lithium adsorbed product are taken, is characterized using X-ray diffraction, 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 roasted, then (25 DEG C) washing 10min of room temperature.In obtained eluent, the desorption rate of lithium is 95% or more, magnesium lithium
Mass ratio is 0.10 or so, the value and initial value (>20) it compares, substantially reduces.
The absorption of lithium of the 2 different aluminum lithium of embodiment than under
Using the method in embodiment 1, only changing the addition of aluminium chloride, the reaction time is respectively 1h, 2h, 4h and 6h,
The adsorption rate of lithium is measured, the result is shown in tables 1.
The adsorption rate (%) of lithium of the 1 different aluminum lithium of table than under
Note：The ranging from 6.6-6.8 of reaction end system pH.
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 measures the adsorption rate of lithium, result as blank sample
It is shown in Table 2.
2 difference Ca (OH) of table2The adsorption rate (%) of lithium under addition
The absorption of lithium in the brine of the different lithium contents of embodiment 4
Using the method in embodiment 1, only change the initial concentration of lithium in brine, the reaction time be respectively 1h, 2h, 4h and
6h measures the adsorption rate of lithium, and the result is shown in tables 3.
The adsorption rate (%) of lithium in the brine of the different lithium contents of table 3
The absorption of lithium in the brine of the different Mg/Li ratios of embodiment 5
Using the method in embodiment 1, only change Mg/Li ratio in brine, the reaction time is respectively 1h, 2h, 4h and 6h, is surveyed
The adsorption rate for determining lithium, the result is shown in tables 4.
The adsorption rate (%) of lithium in the brine 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 replace with salt lake bittern (halogen in embodiment 1
Li in water+20) a concentration of 500mg/L, magnesium lithium mass ratio are.It was found that the brine for directly using it for low lithium concentration carries lithium,
Adsorption effect is very poor.Its specific operating method is as follows：
Take the 100mL salt lake bitterns (Li in the brine+A concentration of 490mg/L, magnesium lithium mass ratio are 20), 4.64g to be added
AlCl3.6H2O, 50 DEG C of control bath temperature are added dropwise sodium hydroxide solution 27mL, 12min and drip 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 lye is added dropwise, and is taken after 0.5h for sampling
Sample；No. 2 are the timing since adding lye, the sample taken after 0.5h), it centrifuges.The two differs 12min on the time, measures it
Adsorption rate the results are shown in Table 5.
5 comparative example of table, 1 experimental result
| Serial number | No. 0 former brine | 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 the lower brine of method extraction lithium concentration of the invention, lithium is inhaled
Attached rate is still 90% or more, and the adsorption rate of comparative example 1 is only 25.5%, and the adsorption rate of the method for the present invention is far above comparative example.
To sum up, the method for the present invention is more suitable for extracting lithium from low lithium brine, this also complies with the brine feature of China.
Claims (6)
1. the method for extracting lithium from salt lake bittern, which is characterized in that include the following steps：
A, it adsorbs：Aluminium salt and calcium hydroxide solid are sequentially added in salt lake bittern, is stirred to react, and the reaction time is 2~6h, is taken
Precipitation, obtains lithium adsorbed product；Wherein, in molar ratio, the molar ratio of the lithium in the aluminium and brine in aluminium salt is 4~5:1；Hydrogen-oxygen
Change the molar ratio 6~9 of calcium and the lithium in brine:1；
B, it is desorbed：By lithium adsorbed product De contamination, lithium solution is obtained；
Li in the salt lake bittern+A concentration of 200~500mg/L, magnesium lithium mass ratio are 20~50:1.
2. the method according to claim 1 for extracting lithium 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 for extracting lithium from salt lake bittern, it is characterised in that：In molar ratio, in aluminium salt
Aluminium and brine in lithium molar ratio be 4:1, reaction time 2h.
4. the method for extracting lithium from salt lake bittern according to claims 1 to 3 any one of them, it is characterised in that：A steps
In, after calcium hydroxide is added, the pH value of reaction system is 6.6~7.3.
5. the method for extracting lithium from salt lake bittern according to claims 1 to 3 any one of them, it is characterised in that：A steps
In, aluminium salt is added in salt lake bittern, after dissolving, calcium hydroxide solid is added in property again.
6. the method according to claim 4 for extracting lithium from salt lake bittern, it is characterised in that：In a steps, in salt lake halogen
Aluminium salt is added in water, after dissolving, calcium hydroxide solid is added in property again.
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| TWI730557B (en) * | 2019-12-23 | 2021-06-11 | 財團法人工業技術研究院 | Method for recovering lithium |
| CN112777614B (en) * | 2021-02-02 | 2023-09-15 | 江苏久吾高科技股份有限公司 | Method and device for extracting lithium from salt lake brine through adsorption |
| CN113368537B (en) * | 2021-06-28 | 2022-05-24 | 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 |
| 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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| CN1243112C (en) * | 2002-12-27 | 2006-02-22 | 中国科学院青海盐湖研究所 | Process for extracting lithium from salt lake brine by adsorptive method |
| CN106140121A (en) * | 2016-06-17 | 2016-11-23 | 江西赣锋锂业股份有限公司 | A kind of renovation process of aluminium salt lithium adsorbent performance recovery |
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