CN102633284A - Method for separating magnesium and extracting lithium from salt lake brine with high magnesium-lithium ratio - Google Patents
Method for separating magnesium and extracting lithium from salt lake brine with high magnesium-lithium ratio Download PDFInfo
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- CN102633284A CN102633284A CN2012101438796A CN201210143879A CN102633284A CN 102633284 A CN102633284 A CN 102633284A CN 2012101438796 A CN2012101438796 A CN 2012101438796A CN 201210143879 A CN201210143879 A CN 201210143879A CN 102633284 A CN102633284 A CN 102633284A
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Abstract
The invention discloses a method for separating magnesium and extracting lithium from salt lake brine with a high magnesium-lithium ratio. With adoption of the method, tributyl phosphate is taken as an extractant, number 200 solvent oil or kerosene is taken as a diluent, perchlorate is taken as a co-extraction agent, and water is taken as a stripping agent to form an extraction system; and lithium carbonate is prepared through extraction, reversed-phase extraction and deep magnesium removal by the salt lake brine. The method has the following beneficial effects: 1. the property of the co-extraction agent is stable, lithium magnesium separation can be carried out in neutral brine and the pH value of an aqueous phase needs not to be controlled; 2. the emulsification phenomenon doesn't exist and a third phase doesn't appear in the extraction process, two phases are easy to separate, the reversed-phase extraction is carried out by water and the device has little corrosion; and 3. the whole technique is simple in process, high in lithium extraction rate, good in separation effect and low in economic cost, is suitable for industrial production of the salt lake brine and is low in environmental damage degree because the co-extraction agent in water can be recycled.
Description
Technical field
The invention belongs to field of inorganic chemical engineering, relate to a kind of technology of from salt lake brine, extracting lithium, refer more particularly to a kind of from high Mg/Li ratio bittern separating magnesium and the method for extracting lithium.
Background technology
Recent two decades comes; Lithium and compound thereof obtain increasingly extensive application because of its excellent properties; The whole world constantly increases the demand of lithium, and the salt lake lithium resource accounts for 69% of world's lithium resource industrial reserves, and the Chilean Atacama type of wherein low Mg/Li ratio bittern salt lake is able at first develop.China is a salt lake resources big country; The liquid lithium resource is very abundant; Yet the most of salt lake of China has the high characteristics of magnesium lithium mass ratio; As big bavin dawn, Yi Liping, East Platform Ji like this, the West Platform Ji like this with the magnesium lithium mass ratio in salt lakes such as Cha Er sweat all more than 40～1800, the similarity of magnesium lithium character is brought difficulty to exploitation and utilization of salt lake resources.Will from bittern, extract the necessary first separating magnesium of lithium, the method for separating Li magnesium mainly contains in the bittern at present: the precipitator method, calcination method, absorption method and extraction process etc.Wherein precipitator method alkali consumption is big, the lithium recovery is low, is not suitable for handling the bittern and the low lithium bittern that contain a large amount of earth alkali metal.Calcination method is through spraying drying, roasting and leaching process, and water yield evaporation is big, energy consumption is high, equipment corrosion is serious, the sub product outlet is narrow.The key of absorption method is sorbent material, and lithium ion sieve type manganese oxygen, titanyl material come into one's own, but there be damage, the granulation problem of dissolving on the low side, the poor permeability of its actual adsorptive capacity.By contrast, but solvent extration has advantages such as operate continuously, concentration ratio is high, equipment is simple, turnout is big, and key is confirming of selection of Extractant and abstraction technique.Wherein tributyl phosphate (TBP) and FeCl
3The system of coming together altogether is once by primary study, and described in document CN87103431A, its technology bottleneck is that the bittern extraction will carry out Li under acidic conditions
+Back extraction require with 6～9mol/L hydrochloric acid soln, have emulsion and third phase to occur in the extraction, therefore do not see industriallization report so far.People such as Zhou adopt ZnCl
2, CrCl
3The agent extraction behavior to TBP under 3 kinds of thinners of coming together is altogether studied, but do not obtain improvement effect (Zhou Z.-Y., Qin W., Fei W.-Y..J.Chem.Eng.Data, 2011,56,3518-3522).And adopt acid amides, alcohol or ketone to help the collection agent when in document CN101698488A and CN102275956A, using TBP, still adopt FeCl
3Lithium is carried in the back extraction of coming together altogether under agent and the acidic conditions, and molysite is resided in the organic phase always, and the technological improvement degree has its limitation.
Summary of the invention
The objective of the invention is to the deficiency that exists in the art methods, a kind of cost-effective separating magnesium and the method for extracting lithium are provided.
Technical scheme provided by the invention and technological process are following:
A kind of from the high Mg/Li ratio salt lake brine separating magnesium and the method for extracting lithium, may further comprise the steps:
1) preparation of bittern: the magnesium lithium mass ratio after Exposure to Sunlight concentrates back or sylvite and extracts is to add the perchlorate agent of coming together altogether in 10: 1～500: 1 the bittern, and come together altogether agent and lithium mol ratio are 0.5: 1～3: 1, and brine ph, is in 1～9 scope.
2) extraction: carry out the bittern extraction with tributyl phosphate as organic phase, extraction phase compares V
o/ V
wBe 0.5: 1～3: 1,1～5 grade of extraction progression, single extraction time 1～30min, 0～60 ℃ of extraction temperature.
3) reversed phase extraction: use water as reverse-extraction agent, carry out reversed phase extraction to containing the lithium organic phase, V is compared in back extraction
w/ V
oBe 0.02: 1～2: 1,1～5 grade of back extraction progression, single back extraction time 1～30min, 0～100 ℃ of back extraction temperature.
4) organic phase circulation: be transferred to the 1st grade of extraction plant to last step back extraction organic phase, extraction phase recycles.
5) degree of depth demagging: in strip aqueous, add yellow soda ash or caustic soda, be settled out magnesiumcarbonate or Marinco H, control pH value of solution>=12 make Mg
2+Deposition is complete, filtering separation.
6) preparation Quilonum Retard: add yellow soda ash in the strip aqueous after degree of depth demagging, produce the Quilonum Retard deposition, make lithium carbonate product after filtration, the drying; Strip aqueous is carried out circulating inside after carrying lithium, uses repeatedly after the agent of coming together altogether in the water recycling.
7) agent of coming together altogether of the perchlorate that adopts of the present invention is a kind of or its mixture in sodium perchlorate, potassium perchlorate, magnesium perchlorate and the calcium perchlorate; The organic phase thinner that adopts is No. 200 solvent oils or kerosene, and its volumn concentration is less than 50%.
The present invention compared with prior art has the following advantages:
1) in solvent extraction process, use the perchlorate agent of coming together altogether, oleophilicity negatively charged ion perchlorate stable in properties, existence form does not receive the influence of brine ph; Lithium ion gets into organic phase mutually through the micro emulsion that comprises nanometer water nuclear, demonstrates special selected property and high percentage extraction, lithium magnesium good separation.
2) the bittern extraction is carried out under neutrality, slightly acidic or weak basic condition, and pH value of solution value accommodation is wide; Two phase separate easily, no emulsification phenomenon and third phase occur; Water replaces hydrochloric acid to make reverse-extraction agent, has fundamentally solved FeCl
3Altogether in the collection process equipment corrosion with need in the consumption alkali with etc. problem.
3) this method can be handled high Mg/Li ratio bittern such as boracic, sulfur-bearing acid groups, and flexibility is strong, Financial cost is low, discharging that can strict control magnesium-containing brine in the production process, and is little to the environmental disruption degree.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is further specified:
Embodiment 1:
Technical process is as shown in Figure 1.
1) gets bittern 50mL after concentrating, wherein contain: Li
+2.21g/L, Mg
2+100.71g/L, Na
+3.53g/L, K
+1.85g/L magnesium lithium mass ratio is 45.6.
2) in bittern, add the agent sodium perchlorate that comes together altogether; Consumption is as the criterion with
; 25 ℃ are stirred down, dissolve; Obtain extracting preceding aqueous salt brine, the pH value of solution value equals 5.
3) in adding organic phase TBP, under 25 ℃, carry out the single extraction, extract time of vibration 10min, leave standstill 15min, two be separated then with the isopyknic ratio of water.
4) doing reverse-extraction agent with pure water, is to mix at 1: 1 by organic phase and water volume ratio, carries out back extraction under 25 ℃, and back extraction time 10min leaves standstill 15min, two is separated then.
5) water is regulated pH>=12 with caustic soda after the back extraction, and magnesium is with Mg (OH)
2The form deposition is separated out, and aqueous phase adds sodium carbonate solution generation deposition after the filtration, gets lithium carbonate product after separation, the drying.
Through detecting, the lithium percentage extraction reaches 45.8%, the magnesium percentage extraction is 5.3%, and the lithium back extraction ratio reaches 64.1%, the magnesium back extraction ratio is 69.2%, and magnesium lithium mass ratio drops to 5.7 by 45.6 in extraction and back extraction process.
Embodiment 2:
1) get bittern 50mL after concentrating, it consists of Li
+0.48g/L, Mg
2+96.21g/L, Na
+3.53g/L, K
+1.85g/L magnesium lithium mass ratio is 200.4.
2) in bittern, add the agent sodium perchlorate that comes together altogether; Consumption is as the criterion with
; 25 ℃ are stirred down, dissolve; Obtain extracting preceding aqueous salt brine, the pH value of solution value transfers to 7.
3) be 2: 1 adding organic phases by oil phase and water volume ratio, organic phase is made up of 80%TBP and 20% kerosene, under 25 ℃, carries out the single extraction, extracts time of vibration 30min, leaves standstill 30min, two is separated then.
4) doing reverse-extraction agent with pure water, is to mix at 1: 1 by organic phase and water volume ratio, carries out back extraction under 50 ℃, and back extraction time 10min leaves standstill 30min, two is separated then.
5) water is regulated pH>=12 with yellow soda ash and caustic soda after the back extraction, and magnesium is with MgCO
3And Mg (OH)
2Form precipitates to be separated out, and filtration back aqueous phase adds sodium carbonate solution again and produces deposition, gets lithium carbonate product after separation, the drying.
Through detecting, the lithium percentage extraction reaches 46.2%, the magnesium percentage extraction is 9.0%, and the lithium back extraction ratio reaches 64.4%, the magnesium back extraction ratio is 57.4%, and magnesium lithium mass ratio drops to 34.8 by 200.4 in extraction and back extraction process.The TBP solvent can extract lithium, Na in the bittern from contain the low bittern of lithium
+, K
+Percentage extraction low, little to lithium magnesium sepn process influence.
Embodiment 3:
1) get the bittern 50mL that concentrates back boracic, sulfate radical, it consists of: Li
+1.80g/L, Mg
2+90.51g/L, Na
+6.89g/L, K
+1.85g/L,
28.82g/L, B
2O
320.89g/L magnesium lithium mass ratio is 50.3.
2) in bittern, add the agent sodium perchlorate that comes together altogether; Consumption is as the criterion with
; 25 ℃ are stirred down, dissolve, obtain extracting preceding aqueous salt brine.
3) be 2: 1 adding organic phase TBP by oil phase and water volume ratio, under 25 ℃, carry out the single extraction, extract time of vibration 10min, leave standstill 30min, two be separated then.
4) doing reverse-extraction agent with pure water, is to mix at 1: 1 by organic phase and water volume ratio, carries out back extraction under 60 ℃, and back extraction time 10min leaves standstill 15min, two is separated then.
5) water is regulated pH>=12 with yellow soda ash and caustic soda after the back extraction, and magnesium is with MgCO
3And Mg (OH)
2Form precipitates to be separated out, and filtration back aqueous phase adds sodium carbonate solution again and produces deposition, gets lithium carbonate product after separation, the drying.
Through detecting, the lithium percentage extraction reaches 67.5%, the magnesium percentage extraction is 8.3%, and the lithium back extraction ratio reaches 83.6%, the magnesium back extraction ratio is 89.4%, and magnesium lithium mass ratio drops to 6.6 by 50.3 in extraction and back extraction process.Show that this system can extract lithium from the bittern of boracic and sulfate radical.
Embodiment 4:
1) get bittern 50mL after concentrating, its composition is identical with embodiment 1.
2) in bittern, add the agent sodium perchlorate that comes together altogether; Consumption is as the criterion with
; 25 ℃ are stirred down, dissolve, obtain extracting preceding aqueous salt brine.
3) in adding organic phase TBP, under 25 ℃, carry out 3 continuous extractions, add extraction agent after vibration time 10min at every turn, leave standstill 15min, two be separated then with 1: 1 ratio of water volume ratio.
4) merging to the organic phase of 3 continuous extractions together, do reverse-extraction agent with pure water, is to mix at 1: 1 by organic phase and water volume ratio, under 70 ℃, carries out back extraction, and back extraction time 10min leaves standstill 30min, two is separated then.
5) water is regulated pH>=12 with caustic soda after the back extraction, and magnesium is with Mg (OH)
2Form precipitates to be separated out, and filtration back aqueous phase adds sodium carbonate solution again and produces deposition, gets lithium carbonate product after separation, the drying.
After testing; Lithium is continuous to extract that total extraction yield reaches 88.2% for 3 times, to merge back lithium single back extraction ratio be 87.1% to extraction phase; Magnesium is continuous to extract that total extraction yield is 15.2%, magnesium single back extraction ratio is 93.3% for 3 times, and magnesium lithium mass ratio drops to 8.4 by 45.6 in extraction and back extraction process.Lithium magnesium separation factor is 14.0.
Embodiment 5:
1) get bittern 50mL after concentrating, its composition is identical with embodiment 1.
2) in bittern, add the agent magnesium perchlorate that comes together altogether; Consumption is as the criterion with
; 25 ℃ are stirred down, dissolve; Obtain extracting preceding aqueous salt brine, the pH value of solution value equals 5, and the solution Mg/Li ratio becomes 49.1 behind the adding magnesium perchlorate.
3) be 2: 1 adding organic phase TBP by oil phase and water volume ratio, under 25 ℃, carry out the single extraction, extract time of vibration 10min, leave standstill 30min, two be separated then.
4) doing reverse-extraction agent with pure water, is to mix at 1: 1 by organic phase and water volume ratio, carries out back extraction under 50 ℃, and back extraction time 10min leaves standstill 15min, two is separated then.
5) water is regulated pH>=12 with caustic soda after the back extraction, and magnesium is with Mg (OH)
2The form deposition is separated out, and aqueous phase adds sodium carbonate solution generation deposition after the filtration, gets lithium carbonate product after separation, the drying.
Through detecting, the lithium percentage extraction reaches 64.3%, the magnesium percentage extraction is 12.6%, and the lithium back extraction ratio reaches 85.9%, the magnesium back extraction ratio is 75.9%, and magnesium lithium mass ratio drops to 8.5 by 49.1 in extraction and back extraction process.
Claims (4)
1. separating magnesium and the method for extracting lithium from a high Mg/Li ratio salt lake brine is characterized in that:
1) preparation of bittern: the magnesium lithium mass ratio after Exposure to Sunlight concentrates back or sylvite and extracts is to add the perchlorate agent of coming together altogether in 10: 1～500: 1 the salt lake brine, and come together altogether agent and lithium mol ratio are 0.5: 1～3: 1, and brine ph, is in 1～9 scope;
2) extraction: carry out the bittern extraction with tributyl phosphate as organic phase, extraction phase compares V
o/ V
wBe 0.5: 1～3: 1,1～5 grade of extraction progression, single extraction time 1～30min, 0～60 ℃ of extraction temperature;
3) reversed phase extraction: use water as reverse-extraction agent, carry out reversed phase extraction to containing the lithium organic phase, V is compared in back extraction
w/ V
oBe 0.02: 1～2: 1,1～5 grade of back extraction progression, single back extraction time 1～30min, 0～100 ℃ of back extraction temperature;
4) degree of depth demagging: in strip aqueous, add yellow soda ash or caustic soda, be settled out magnesiumcarbonate or Marinco H, control pH value of solution>=12 make Mg
2+Deposition is complete, filtering separation;
5) preparation Quilonum Retard: add yellow soda ash in the strip aqueous after degree of depth demagging, produce the Quilonum Retard deposition, make lithium carbonate product after filtration, the drying; Strip aqueous is carried out circulating inside after carrying lithium, uses repeatedly after the agent of coming together altogether in the water recycling.
2. as claimed in claim 1 a kind of from the high Mg/Li ratio salt lake brine separating magnesium and the method for extracting lithium, it is characterized in that the agent of coming together altogether of used perchlorate is a kind of or its mixture in sodium perchlorate, potassium perchlorate, magnesium perchlorate, the calcium perchlorate.
3. as claimed in claim 1 a kind of from the high Mg/Li ratio salt lake brine separating magnesium and the method for extracting lithium, it is characterized in that used organic phase contains No. 200 solvent oils of thinner or kerosene, but its volumn concentration is less than 50%.
4. as claimed in claim 1 a kind of from the high Mg/Li ratio salt lake brine separating magnesium and the method for extracting lithium, it is characterized in that carrying out being transferred to the 1st grade of extraction plant to the back extraction organic phase of last step behind the reversed phase extraction, directly repeated use.
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|---|---|---|---|---|
| CN103898341A (en) * | 2014-03-06 | 2014-07-02 | 中国科学院青海盐湖研究所 | Method for separating and extracting lithium from lithium sulfate coarse ore |
| CN104232896A (en) * | 2014-09-18 | 2014-12-24 | 中国科学院青海盐湖研究所 | Method for separating lithium from salt lake brine |
| CN104232897A (en) * | 2014-09-18 | 2014-12-24 | 中国科学院青海盐湖研究所 | Lithium ion extraction system |
| 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 |
| CN105540624A (en) * | 2015-12-07 | 2016-05-04 | 上海实业振泰化工有限公司 | Preparation method of high purity acicular magnesium hydroxide |
| CN108193058A (en) * | 2017-11-29 | 2018-06-22 | 潍坊学院 | A kind of method for the ion liquid abstraction that lithium is extracted from salt lake |
| CN110817909A (en) * | 2019-11-19 | 2020-02-21 | 中国科学院过程工程研究所 | Lithium-magnesium separation method |
| CN111139356A (en) * | 2020-01-19 | 2020-05-12 | 意定(上海)信息科技有限公司 | Method for extracting lithium from lithium-containing low-magnesium brine |
| CN115477355A (en) * | 2022-09-30 | 2022-12-16 | 武汉工程大学 | Method for extracting lithium from lithium-containing wastewater by using TBP (tunnel boring machine) |
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| CN103898341B (en) * | 2014-03-06 | 2015-10-21 | 中国科学院青海盐湖研究所 | From the method for the rough separation and Extraction lithium of Lithium Sulphate |
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| CN104232896A (en) * | 2014-09-18 | 2014-12-24 | 中国科学院青海盐湖研究所 | Method for separating lithium from salt lake brine |
| CN104232897A (en) * | 2014-09-18 | 2014-12-24 | 中国科学院青海盐湖研究所 | Lithium ion extraction system |
| 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 |
| 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 |
| WO2017045485A1 (en) * | 2015-09-18 | 2017-03-23 | 湘潭大学 | Method for producing lithium carbonate by separating magnesium from and enriching lithium in low-lithium brine |
| CN105540624A (en) * | 2015-12-07 | 2016-05-04 | 上海实业振泰化工有限公司 | Preparation method of high purity acicular magnesium hydroxide |
| CN108193058A (en) * | 2017-11-29 | 2018-06-22 | 潍坊学院 | A kind of method for the ion liquid abstraction that lithium is extracted from salt lake |
| CN110817909A (en) * | 2019-11-19 | 2020-02-21 | 中国科学院过程工程研究所 | Lithium-magnesium separation method |
| CN111139356A (en) * | 2020-01-19 | 2020-05-12 | 意定(上海)信息科技有限公司 | Method for extracting lithium from lithium-containing low-magnesium brine |
| CN115477355A (en) * | 2022-09-30 | 2022-12-16 | 武汉工程大学 | Method for extracting lithium from lithium-containing wastewater by using TBP (tunnel boring machine) |
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