CN111424183A - Method for extracting and preparing lithium carbonate from brine of sulfate type salt lake and chloride type salt lake - Google Patents

Method for extracting and preparing lithium carbonate from brine of sulfate type salt lake and chloride type salt lake Download PDF

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CN111424183A
CN111424183A CN202010435418.0A CN202010435418A CN111424183A CN 111424183 A CN111424183 A CN 111424183A CN 202010435418 A CN202010435418 A CN 202010435418A CN 111424183 A CN111424183 A CN 111424183A
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孟元
巴特尔
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Abstract

The invention belongs to the field of chemical industry, and provides a method for extracting lithium ions and preparing lithium carbonate from sulfate type and chloride type salt lakes aiming at the problems that sulfate type and chloride type salt lake brine is acidic, the content of lithium ions is low, the magnesium and lithium are high and the like. The preparation method comprises the following steps: concentrating the brine to a proper lithium ion concentration, adjusting the pH value to be neutral and alkaline by adding alkali or alkaline solution on the premise of not precipitating magnesium hydroxide or slightly precipitating magnesium hydroxide, adding an extracting agent according to a certain ratio, and extracting and separating to obtain a lithium-containing organic phase; introducing CO2And pure water to obtain L iHCO3Adding alkali into the stripping solution to remove a small amount of magnesium ions by precipitation in the form of magnesium hydroxide, and heating the demagging stripping solution to L iHCO3Decomposing to form L i slightly soluble in water2CO3Separating the precipitate to obtain L i2CO3And (4) crystals. The method is organically linked with a novel extracting agent extraction method by changing the pH value of the brine at reasonable cost, and the adaptability of the novel extraction technology to lithium extraction of various salt lakes is expanded.

Description

Method for extracting and preparing lithium carbonate from brine of sulfate type salt lake and chloride type salt lake
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method for extracting and preparing lithium carbonate from brine of a sulfate type salt lake and a chloride type salt lake.
Background
With the increasing severity of energy crisis and environmental pollution, the development of clean new energy is not slow enough. In the face of the severe situation of environmental deterioration, it has become common knowledge to greatly reduce the exploitation and use of fossil energy. Lithium ion batteries, as an ideal secondary battery, have received extensive attention due to their high energy density and long cycle life, and the lithium ion battery yield has been explosively increased, and as an indispensable raw material for preparing lithium ion battery materials, the demand for lithium carbonate has also been on the rise. In the next 10 years, the global consumption of lithium resources is multiplied, and the lithium battery field is expected to increase to 65% in 2025.
China is rich in lithium resources, the lithium resource amount is 540 ten thousand tons, the lithium storage amount is 320 ten thousand tons, and the second world is. The lithium resources of the Chinese brine are mainly concentrated in Qinghai and Tibet, and the lithium ion-containing salt lake in the region mainly comprises three types, namely a sulfate type, a chloride type and a carbonate type, and has the common characteristic that the lithium ion content is low and can reach a certain concentration after concentration. For brine of any system and whatever lithium extraction technology is adopted, generally, higher lithium ion concentration is beneficial to the reaction processing process, and the efficiency optimization of industrial engineering is facilitated in the aspects of treatment capacity, energy consumption, reduction of operation cost, improvement of yield and the like. The traditional method for removing magnesium by using alkali precipitation is only suitable for salt lakes with low magnesium-lithium ratio, and salt lakes with high magnesium-lithium ratio only adopt a precipitation method, so that the alkali consumption for precipitation is high, and the economic value is not high. The novel extraction method, namely neutral phosphonate extraction, is feasible, and is used for preliminarily separating magnesium and lithium to a certain degree to greatly reduce the magnesium-lithium ratio of the separated brine, then removing magnesium by alkali precipitation and further extracting lithium. At present, the salt lake lithium extraction technology successfully applied by salt lake lithium extraction enterprises in Qinghai regions mainly adopts the development idea of electrodialysis method, adsorption method and the like.
In essence, in the novel extraction method, besides the lithium ion concentration, different pH values of raw material brine are an important reaction power in the extraction and back extraction reaction processes, namely alkaline brine is favorable for the extraction reaction process, and acidic water or solution can be favorable for the back extraction reaction process, so that the novel extraction method is suitable for carbonate salt lakes, and for sulfate salt lake brine and chloride salt lake brine, the novel extractant has low capability of extracting lithium ions and cannot efficiently extract lithium ions.
Disclosure of Invention
Aiming at the problems that the existing extraction technology is suitable for carbonate salt lakes, and the extraction effect is poor for sulfate salt lake brine and chloride salt lake brine, the invention provides a method for extracting and preparing lithium carbonate from sulfate salt lake brine and chloride salt lake brine. The method is organically linked with a novel extracting agent extraction method by changing the pH value of the brine at reasonable cost, expands the adaptability of the novel extraction technology to extracting lithium from various salt lakes, and has positive significance for effectively utilizing the brine resources of the salt lakes of Qinghai and Tibet, perfecting the industrial chain of new energy resources and developing local economy.
The invention is realized by the following technical scheme:
a method for extracting and preparing lithium carbonate from sulfate type and chloride type salt lake brine comprises the following steps:
(1) concentrating salt lake brine to appropriate L i+Adding an alkali solution to adjust the pH value of the brine to be neutral or slightly alkaline according to the condition that magnesium ions in the raw material brine are not separated out or are separated out in a small amount, wherein the magnesium-lithium ratio is not higher than 1000: 1;
(2) introducing neutral extractant into salt lake brine according to a certain proportion, adding diluent, stirring thoroughly, mixing uniformly, extracting for 2-8 min, and repeatedly extracting for 1-5 times to obtain L i-containing extract+And a small amount of Mg+2The organic phase of (a);
(3) the obtained organic phase enters a mixer, and CO is introduced into the mixer2And pure water as stripping agent, stripping agent CO2And H2H produced by hydrolysis of O+Displacement extraction of L i from the organic phase+L iHCO is obtained3And Mg (HCO)3)2Dissolving in waterAnd (3) reducing the magnesium-lithium reduction ratio in the stripping solution to the level of economically producing lithium carbonate 2: 1-4: 1, if necessary, the requirement of low magnesium-lithium ratio is met by multi-stage operation of further extraction and back extraction after adjusting the pH of a back extraction solution;
(4) adding alkali into the stripping solution to remove a small amount of magnesium ions in the form of magnesium hydroxide precipitate;
(5) l iHCO obtained after demagging3Heating the aqueous solution to decompose the aqueous solution to form L i slightly soluble in water2CO3，Li2CO3Crystallizing, separating precipitate, washing and drying to obtain L i2CO3And (4) crystals.
Further, the alkali solution in the step (1) is a sodium hydroxide solution, a potassium hydroxide solution, ammonia water, a sodium carbonate solution or a calcium hydroxide solution.
Further, the pH value of the alkalescence of the step (1) is less than or equal to 8.
Further, the neutral extractant in the step (2) is neutral phosphonate or fluorinated neutral phosphonate. Further preferred is tributylphosphine oxide or fluorinated trioctylphosphine oxide. The extraction of the extractant is sequentially as follows: hydrogen ion lithium ion sodium ion potassium ion. In the absence of hydrogen ions in an alkaline environment, the extractant first extracts lithium ions.
The invention has the beneficial effects that: (1) according to the invention, the low-cost alkali or alkali solution is used as the pH regulator of the concentrated brine, so that the pH value of the brine is more than 7, the brine is slightly alkaline, magnesium hydroxide is not precipitated or is precipitated in a small amount in the pH value range, a neutral extractant is adopted to selectively extract lithium ions, and based on the chelating action force of the extractant and the lithium ions, the target lithium ions are efficiently screened, so that the better magnesium-lithium separation is realized, and the magnesium-lithium ratio is reduced; (2) the pH value of concentrated brine of sulfate type and chloride type salt lakes is adjusted, so that the connection of raw materials and an extraction technology is realized, and the adaptability of the novel extraction technology to lithium extraction of various salt lakes is expanded.
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FIG. 1 is a flow chart of a process for preparing lithium carbonate by extracting from a sulfate type or chloride type salt lake brine.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments and the accompanying drawings.
During the evaporation and concentration process of the carbonate salt lake brine in the salt pan, the pH value of the brine tends to rise along with the evaporation. After the sulfate salt lake brine and the chloride salt lake brine are subjected to controlled concentration by the salt field technology, a large amount of other ions are crystallized and separated out in the form of salt field minerals and are separated from the brine, the water-salt system of the brine which is continuously concentrated is greatly simplified, lithium ions are not crystallized and separated out in the form of the salt field minerals in the concentration process and are enriched in the brine, and the pH value is in a descending trend.
Taking the sulfate type salt lake brine of Qinghai as an example, the physicochemical properties of the original brine and the concentrated brine (old brine) are shown in the following table:
TABLE 1 physicochemical Properties of sulfate type salt lake brine and aged brine
Figure BDA0002502072390000031
I.e., the pH increased from 6.51 in the raw brine to 2.86 in the old brine stage during the concentration by evaporation. Some chloride type salt lake brine can be reduced to about pH 4 in the process of evaporation and concentration.
From the water salt system of the brine, the magnesium ions in the brine are highly concentrated and enriched except the lithium ions, the magnesium-lithium ratio of the brine is higher, and the magnesium-ion ratio of the concentrated brine of the salt lake reaches:
Mg2+：Li+8.98: 0.4: 22.45: 1. At the same time, a large number of K+、Na+Ions are removed in the salt pan evaporation process in the form of salt pan crystallized ore.
Na can be used for adjusting pH of concentrated brine2CO3NaOH, KOH, etc., Na+、K+Is the ions contained in the brine system, so that other impurity ions can not be introduced.
Na2CO3The solubility of saturated sodium carbonate at 20 ℃ is 21.5g/100g of water,calculated mass fraction Wt% 17.70%, calculated mass concentration of substance 1.987 mol/L, Ka2＝4.7×10-11，CO3 2-Hydrolysis constant Kh-Kw/Ka 2-2.13 x10-4，COH -(C × Kh)0.5 ═ 0.02, and the density was measured to be 1.19g/m L ═ 12.3, i.e., C (Na)2CO3)OH＝10-(14-12.3)＝10-1.7mol/L compared with NaOH, the solubility of NaOH at 20 ℃ is 109g/100g water, 102g/100g (in the production process, the time for preparing completely saturated solution is longer) of unsaturated NaOH solution has the density of 1.530g/cm3, the mass fraction is 50.5%, the mol concentration is 19.310 mol/L, namely the concentration of C (NaOH) OH is 19.310 mol/L, namely C (NaOH) which is close to saturated NaOH solution at the same temperatureOHWith saturated Na2CO3C (Na) of solution2CO3)OHThe ratio of the components is as follows:
C(NaOH)OH：C(Na2CO3)＝19.310:10-1.7
namely, the pH value regulating capacity of NaOH is far greater than that of Na2CO3The pH value regulating ability of the composition. Therefore, NaOH solution can be selected as the pH regulator of the concentrated brine.
During this conditioning, theoretically, two chemical reactions occur in the solution:
a first reaction: h + in low pH brine and OH in added NaOH solution-Reaction is carried out:
H++OH-＝H2O
in this reaction, H in brine at pH 7+All the reaction is continued, NaOH is added continuously, OH in solution-In excess, resulting in a gradual rise in the pH of the brine.
Required NaOH dosage:
setting the temperature to be 20 ℃;
brine volume Lbrine1000, density Dbrine＝1.376g/cm3PH 3, namely C (OH-)brine＝10-(14-3)＝10-11mol/L；
NaOH solutionLiquid volume LNaOH10L, Density DNaOH＝1.331g/cm3，C(OH-)NaOH＝19.310mol/L；
Adjusted mother liquor volume LliquidDensity 1010Lliquid1.375g/cm3, pH 8, i.e. C (OH)-)liquid＝10-(14-8)＝10-6mol/L；
And (3) a second reaction:
Mg2++2OH-＝Mg(OH)2(precipitation)
The two reactions are carried out alternately, and the pH value can be adjusted within 8 to Mg (OH)2The method does not generate precipitation reaction or generates slight degree, and the method can be organically linked with a novel extractant extraction method by changing the pH value of brine at reasonable cost.
And (4) if the strip liquor after back extraction is subjected to pH value adjustment and further re-extraction and back extraction, the strip liquor with lower magnesium-lithium ratio can be obtained, and the subsequent lithium extraction processing is facilitated.
The following specific examples all refer to the process flow diagram of figure 1.
EXAMPLE 1 extraction of lithium from sulfate type salt lake brine
(1) Salt lake brine (L i) with magnesium-lithium ratio of 60:1+0.15 g/L) is added slowly into NaOH saturated solution under stirring to adjust the pH value of the brine to 7.68;
(2) introducing tributylphosphine oxide extractant of 500m L matched with sulfonated kerosene (30%, v/v) into 1000m L salt lake brine according to the proportion of 1: 2, fully stirring and uniformly mixing, extracting for 5 minutes, and repeatedly extracting for 2 times to obtain extract containing L i+And a small amount of Mg+2The extractant organic phase of (1);
(3) the obtained organic phase was fed into a mixer into which 3000m L CO was introduced2And 150m L pure water, H produced by carbonic acid in stripping agent+Displacement extraction of L i from the organic phase+And a small amount of Mg+2L iHCO is obtained3And Mg (HCO)3)2And (3) an aqueous solution, wherein the magnesium-lithium ratio in the stripping solution is 12: 1, adjusting the pH of a stripping solution, and then carrying out further extraction and back extraction to achieve a low magnesium-lithium ratio of 4: 1;
(4) adding sodium hydroxide into the stripping solution to remove a small amount of magnesium ions in the form of magnesium hydroxide precipitate;
(5) l iHCO obtained after demagging3The aqueous solution is heated and decomposed to form L i which is slightly soluble in water2CO3(0.17 mol/L, 25 ℃) and CO2Gas, CO2Recycling of gas, L i2CO3Crystallizing, separating precipitate, washing and drying to obtain L i2CO3Crystal 0.698g L i+The extraction yield was 88.1%.
EXAMPLE 2 extraction of lithium from chloride-type salt lake brine
(1) Salt lake brine (L i) with magnesium-lithium ratio of 52:1+Concentration of 2 g/L), slowly adding NaOH saturated solution under stirring, and adjusting the pH value of the brine to 8.0;
(2) introducing 1000m L and sulfonated kerosene (30%, v/v) matched fluorinated trioctylphosphine oxide extractant into 1000m L salt lake brine according to a certain ratio (1: 1), fully stirring and uniformly mixing, extracting for 3 minutes, and repeatedly extracting for 2 times to obtain extract containing L i+And a small amount of Mg+2Obtaining an extractant organic phase;
(3) the obtained organic phase of the extractant enters a pipeline mixer, and 3000m L CO is introduced into the pipeline mixer2And 200m L pure water, H produced by carbonic acid in stripping agent+Displacement extraction of L i from the organic phase+And a small amount of Mg+2L iHCO is obtained3And Mg (HCO)3)2And (3) an aqueous solution, wherein the magnesium-lithium ratio in the stripping solution is 15: 1, adjusting the pH of a stripping solution, and then carrying out further extraction and back extraction to achieve a low magnesium-lithium ratio of 2: 1;
(4) adding sodium hydroxide into the stripping solution to remove a small amount of magnesium ions in the form of magnesium hydroxide precipitate;
(5) l iHCO obtained after demagging3The aqueous solution is heated and decomposed to form L i which is slightly soluble in water2CO3(0.17 mol/L, 25 ℃) and CO2Gas, CO2Recycling of gas, L i2CO3Crystallizing, separating precipitate, washing and drying to obtain L i2CO3Crystal 9.07g, L i+The extraction yield was 85.9%.
Comparative example extraction of lithium from sulfate type salt lake brine
(1) Adding an extractant tributylphosphine oxide into diluent sulfonated kerosene (30 percent, v/v), preparing 1000m L, introducing 2000m L Qinghai (the altitude is 3000m, the perennial temperature is 10 ℃) salt lake brine according to the volume ratio of 1: 2, wherein the content of the brine L i + is 1000ppm, the pH value of the brine is 4.5, fully stirring and uniformly mixing the brine, the extraction time is 10 minutes, and repeatedly extracting for 2 times to obtain the sulfonated kerosene containing L i+Extracted organic phase with an ion content of 520 ppm.
(2) The prepared stripping agent (CO)2Gas and water) are mixed with the lithium-containing organic phase obtained after extraction according to the proportion of 5:1, the back extraction temperature is controlled to be 25 ℃, stirring and oscillation are carried out, the back extraction time is 10min, the back extraction pressure is 0.2MPa, and extraction is repeated for 3 times to obtain a lithium bicarbonate aqueous solution containing a small amount of bicarbonate impurities;
(3) heating the stripping solution, controlling the temperature at 100 ℃, the pressure at-0.05 MPa and the stirring speed at 800rpm, and stirring properly until the lithium bicarbonate is completely decomposed to obtain lithium carbonate;
(4) l i in the phase separation crystallization pool which is slightly soluble in water2CO3The lithium carbonate is crystallized and separated out when the saturated concentration (1.43 g/L, 10 ℃) is reached, the precipitate is separated and washed and dried to obtain 5g of lithium carbonate crystals, and the extraction yield of L i + is 47.5%.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.

Claims (4)

1. A method for extracting and preparing lithium carbonate from sulfate type and chloride type salt lake brine is characterized by comprising the following steps:
(1) concentrating salt lake brine to appropriate L i+Adding an alkali solution to adjust the pH value of the brine to be neutral or slightly alkaline according to the condition that magnesium ions in the raw material brine are not separated out or are separated out in a small amount, wherein the magnesium-lithium ratio is not higher than 1000: 1;
(2) introducing an extracting agent into salt lake brine according to a certain proportion, adding a diluent, fully stirring and uniformly mixing, extracting for 2-8 minutes, repeatedly extracting for 1-5 times to obtain L i-containing solution+And a small amount of Mg+2The organic phase of (a);
(3) the obtained organic phase enters a mixer, and CO is introduced into the mixer2And pure water as stripping agent, stripping agent CO2And H2H produced by hydrolysis of O+Displacement extraction of L i from the organic phase+L iHCO is obtained3And Mg (HCO)3)2And (3) reducing the magnesium-lithium reduction ratio in the stripping solution to the level of economically producing lithium carbonate by using the aqueous solution, wherein the magnesium-lithium reduction ratio is 2: 1-4: 1, if necessary, the requirement of low magnesium-lithium ratio is met through multi-stage operation of further extraction and back extraction after the pH value of a back extraction solution is adjusted;
(4) adding alkali into the stripping solution to remove a small amount of magnesium ions in the form of magnesium hydroxide precipitate;
(5) l iHCO obtained after demagging3Heating the aqueous solution to decompose the aqueous solution to form L i slightly soluble in water2CO3，Li2CO3Crystallizing, separating precipitate, washing and drying to obtain L i2CO3And (4) crystals.
2. The method according to claim 1, wherein the alkali solution in step (1) is sodium hydroxide solution, potassium hydroxide solution, ammonia water, sodium carbonate solution or calcium hydroxide solution.
3. The method according to claim 1, wherein the step (1) is slightly alkaline with a pH value of 8 or less.
4. The method of claim 1, wherein the step (2) extractant is a neutral phosphonate or a fluorinated neutral phosphonate.
CN202010435418.0A 2020-05-21 2020-05-21 Method for extracting and preparing lithium carbonate from brine of sulfate type salt lake and chloride type salt lake Withdrawn CN111424183A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115637327A (en) * 2022-10-28 2023-01-24 昆明理工大学 Coupling device assisting in lithium extraction in salt lake based on ultrasound and use method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115637327A (en) * 2022-10-28 2023-01-24 昆明理工大学 Coupling device assisting in lithium extraction in salt lake based on ultrasound and use method thereof
CN115637327B (en) * 2022-10-28 2024-06-04 昆明理工大学 Coupling device for extracting lithium from salt lake based on ultrasonic assistance and application method thereof

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