CN113955775B - Method for extracting lithium carbonate from lithium-rich clay by acid-base combined method - Google Patents
Method for extracting lithium carbonate from lithium-rich clay by acid-base combined method Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
Abstract
The invention relates to a method for extracting lithium carbonate from lithium-rich clay by an acid-base combination method, which comprises the steps of adding the lithium-rich clay into a sulfuric acid solution with a certain concentration for leaching, and then filtering and separating to obtain acid leaching solution and acid leaching residues; adding a sodium hydroxide solution into the acid leaching residue to carry out alkali leaching, and then filtering and separating to obtain an alkali leaching solution and alkali leaching residue; and (3) introducing carbon dioxide gas into the alkali leaching solution, and filtering when the pH value reaches 8.5-10.5 to obtain lithium carbonate solid and carbonation mother liquor. The method has the advantages of simple process, no special requirement on equipment, low energy consumption, good controllability of process parameters, small residual amount of residues, low production cost and the like, and opens up a new way for developing and utilizing the lithium-rich clay.
Description
Technical Field
The invention relates to a method for extracting lithium carbonate from lithium-rich clay by an acid-base combination method, belonging to the technical field of metallurgy and mineral product utilization.
Background
The lithium element has special physical and electrochemical properties such as low density and high specific energy, is widely applied to the advanced industrial fields such as new energy development, nuclear industry, aerospace, national defense and the like, and has extremely high economic and strategic values. Lithium ore resources in China are relatively rich and account for about 13.8 percent of the total world resource amount. However, due to the continuous increase of the demand of lithium resources and the restriction of the development and utilization technology of lithium ores, the guarantee of lithium resources in China is seriously insufficient, and the external dependence degree is as high as 76%. At present, the lithium deposit resources exploited and utilized all over the world are mainly brine deposits and pegmatite deposits. In recent years, new clay-type lithium ores are gradually discovered and recognized in the southwest area of China (wenhanjie, 2019). If the clay type lithium ore can be efficiently developed and utilized, the situation of shortage of lithium resources in China can be effectively relieved.
At present, the process technology for extracting lithium from lithium ore mainly comprises a limestone roasting method, a sulfate roasting method, a chlorination roasting method and the like, but the methods have some defects more or less, such as large evaporation energy consumption, difficult equipment maintenance, low lithium recovery rate and high generation cost of the limestone roasting method; the sulfate roasting method has long flow and high process energy consumption; the chloridizing roasting method has the advantages of large reagent dosage, difficult LiCl collection and strong furnace gas corrosivity. These lithium extraction processes are suitable for extracting lithium from spodumene and lepidolite. The lithium in the clay mineral is mainly existed in the clay mineral, and the process is not suitable for directly extracting the lithium.
The existing lithium extraction process from the lithium-rich clay ore generally has the problems of high energy consumption, high equipment requirement, large slag yield, high cost and the like. Therefore, aiming at the current situation of lithium-rich clay mineral resources and the defects in the lithium extraction process in China, a new technology for extracting lithium from the lithium-rich clay mineral with high efficiency and energy conservation needs to be researched urgently.
Disclosure of Invention
Technical problem to be solved
In order to solve the above problems in the prior art, the invention provides a method for extracting lithium carbonate from lithium-rich clay by an acid-base combination method, which effectively separates and extracts lithium in the lithium-rich clay and converts the lithium into a lithium carbonate product.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a method for extracting lithium carbonate from lithium-rich clay by an acid-base combination method comprises the following steps:
s1, crushing and grinding the lithium-rich clay to obtain a lithium-rich clay powdery sample;
s2, adding a sulfuric acid solution into the lithium-rich clay powder obtained in the step S1 for leaching, and then filtering and separating to obtain acid leaching solution and acid leaching residues;
s3, adding a sodium hydroxide solution into the acid leaching residue obtained in the step S2 for alkali leaching, and then filtering and separating to obtain an alkali leaching solution and an alkali leaching residue;
s4, introducing carbon dioxide gas into the alkali leaching solution obtained in the step S3, and then filtering to obtain lithium carbonate solid and carbon mother liquor;
s5, adding Ca (OH) into the carbon content mother liquor obtained in the step S32Stirring the solution, filtering, and returning the obtained filtrate as sodium hydroxide solution to step S3 in the next reactionCarrying out alkaline leaching and dissolving out;
s6, concentrating and crystallizing the pickle liquor obtained in the step S2 to obtain ferric sulfate.
In the method for extracting lithium carbonate as described above, preferably, in step S1, the lithium-rich clay is crushed and ground to 100 to 400 mesh.
In the method for extracting lithium carbonate, preferably, in step S2, the concentration of the sulfuric acid solution is 1 to 3mol/L, the leaching is performed at 40 to 100 ℃, the stirring is performed simultaneously during the leaching, the stirring rate is 300 to 500 rpm, and the time is 0.5 to 3 hours.
Further preferably, the concentration of the sulfuric acid solution is 2-3 mol/L.
In the method for extracting lithium carbonate, preferably, in step S2, the sulfuric acid solution is mixed with the lithium-rich clay powder at a liquid-to-solid ratio of 5-10: 1.
In the method for extracting lithium carbonate, in step S3, the mass concentration of the sodium hydroxide solution is preferably 10% to 40%, and the solid-liquid mass ratio of the acid leaching residue to the sodium hydroxide solution is preferably 1:3 to 10.
In the method for extracting lithium carbonate, preferably, in step S3, the temperature of the alkali leaching is maintained at 60-100 ℃, and the leaching time is 0.5-2 h.
In the method for extracting lithium carbonate as described above, preferably, in step S4, the carbon dioxide gas is maintained at a carbon dioxide content of 20% to 40%, and the alkaline leaching solution is heated to 60 to 100 ℃.
In the method for extracting lithium carbonate as described above, preferably, in step S4, when the pH value in the alkali leaching solution is measured to be 8.5 to 10.5, the introduction of carbon dioxide gas is stopped.
In the method for extracting lithium carbonate as described above, preferably, in step S5, Ca (OH)2The mass fraction of the solution is 5 to 30 percent, when no precipitate is generated in the solution, the addition of Ca (OH) is stopped 2And (3) solution.
(III) advantageous effects
The invention has the beneficial effects that:
according to the method for extracting lithium carbonate from lithium-rich clay by using the acid-base combination method, provided by the invention, the lithium in the lithium-rich clay can be effectively separated and extracted by using the acid-base combination method through step-by-step dissolution without roasting, and the lithium is converted into a lithium carbonate product.
The method for extracting lithium carbonate from lithium-rich clay by using the acid-base combination method provided by the invention has the advantages of simple process, low energy consumption, no special requirements on equipment, good controllability of process parameters, small residual amount of residues, low production cost and the like, and opens up a new way for extracting lithium from the lithium-rich clay.
Detailed Description
Through a large number of experiments, researches show that the lithium-rich clay is leached by sulfuric acid with the concentration of 0-4 mol/L, then the content of lithium in the lithium-rich clay is measured by using an electronic probe, and when the sulfuric acid with the concentration of 0-3 mol/L is found, Li in leaching slag2The content of O is not substantially changed, Fe2O3The content of (a) is gradually reduced, and when the concentration of sulfuric acid is 2-3 mol/L, Fe2O3Leaching out most of the water; when the sulfuric acid is 4mol/L, Al in the leaching slag is leached2O3Has a partial leaching, and when the leaching temperature is higher than 100 ℃, Al 2O3And Li2The dissolution rate of O is obviously improved.
The invention provides a method for extracting lithium carbonate from lithium-rich clay by an acid-base combined method, which preferably comprises the following steps:
s1: crushing and grinding the lithium-rich clay to 100-400 meshes to obtain a lithium-rich clay powdery sample;
s2: and (3) mixing the lithium-rich clay powdery sample obtained in the step (1) according to the weight ratio of 5-10: and (3) placing the solution-solid ratio of 1 in a sulfuric acid solution with the concentration of 1-3 mol/L, stirring for 0.5-6 h under a certain temperature condition, and filtering and separating to obtain acid leaching solution and acid leaching residue.
Research shows that when the concentration of the sulfuric acid solution is preferably 1-3 mol/L, most of Fe in the clay2O3The iron sulfate is generated by reaction with sulfuric acid and enters an acid leaching solution, lithium is not dissolved out of a leaching solution and enters acid leaching residues, and the concentration of the sulfuric acid solution is preferably 2-3 mol/L.
S3: and (3) mixing the acid leaching residue obtained in the step (S2) with a sodium hydroxide solution with a certain concentration according to a certain liquid-solid ratio, stirring for 0.5-3 h at the temperature of 60-100 ℃, and filtering to obtain an alkali leaching solution and an alkali leaching residue, wherein the alkali leaching residue mainly comprises impurities such as sodium aluminosilicate, silicon dioxide and the like.
The minerals in the lithium-rich clay mainly comprise aluminosilicate minerals such as muscovite, kaolinite and the like, lithium mainly exists in the minerals, after acid leaching, acid leaching residues mainly contain the aluminosilicate minerals and lithium existing in the aluminosilicate minerals, the aluminosilicate minerals are reacted with a sodium hydroxide solution to mainly produce insoluble sodium aluminosilicate, the lithium existing in the aluminosilicate minerals is converted into lithium hydroxide in the process, and the lithium hydroxide is dissolved in the solution and enters an alkali leaching solution. Preferably, the mass concentration of the sodium hydroxide solution is 10-40%, the dosage ratio of the acid leaching residue to the sodium hydroxide solution is preferably 1: 3-10 by mass of solid-liquid ratio, when the dosage of the sodium hydroxide is too small, lithium cannot be leached completely, and when the dosage of the sodium hydroxide is too large, resource waste is easily caused.
S4: and (3) introducing 10-40% carbon dioxide gas into the alkali extract obtained in the step S3, stopping introducing the carbon dioxide when the pH value of the alkali extract is 8.5-10.5, and filtering to obtain lithium carbonate and carbonation mother liquor.
S5: adding 5 to 30 mass percent of Ca (OH) into the carbon content mother liquor obtained in the step S42(causticizing process), after the precipitate is separated out after stirring, stopping adding Ca (OH) when no precipitate is produced2Filtering the solution, and returning the filtrate to the step S3 as a sodium hydroxide solution to continue the alkaline leaching.
S6: and concentrating and crystallizing the pickle liquor obtained in the step S2 to obtain ferric sulfate. The obtained ferric sulfate can be used as coagulant for water purification and treating agent for sludge, can be used as astringent and hemostatic in medicine, and can be used as coagulant for industrial wastewater.
For a better understanding of the present invention, reference will now be made in detail to the present invention by way of specific embodiments thereof.
Example 1
Of the present embodimentThe main chemical composition SiO in the lithium-rich clay242.85% Fe2O35.38% of Al2O3Content of 36.03%, Li2The O content is 0.98 per mill. The method comprises the following specific steps:
s1: crushing and grinding the lithium-rich clay to 100 meshes to obtain a lithium-rich clay powdery sample;
S2: placing a powdery sample of the lithium-rich clay mineral powder obtained in the step S1 in a sulfuric acid solution with the concentration of 6mol/L according to the mass ratio of 5:1, stirring and dissolving for 0.5h at the temperature of 40 ℃, and filtering and separating to obtain acid leaching solution and acid leaching residue;
s3: mixing the acid leaching residue obtained in S2 with a sodium hydroxide solution with the mass concentration of 10% according to the mass ratio of 1:9, stirring for 3 hours at the temperature of 60 ℃, and filtering to obtain an alkali leaching solution and an alkali leaching residue;
s4: heating the alkali leaching solution obtained in the step S3 to 60 ℃, introducing carbon dioxide gas with the mass concentration of 20%, stopping introducing the carbon dioxide when the pH value of the solution reaches 8.5, and filtering to obtain lithium carbonate and carbonation mother liquor, wherein the recovery rate of the lithium carbonate is 99.17% by calculation;
s5: adding 15% Ca (OH) by mass into the carbon content mother liquor obtained in the step S4 slowly2Continuously stirring, stopping adding Ca (OH) when no precipitate is generated in the solution2Filtering the solution, and returning the filtrate to S3 as sodium hydroxide solution for continuous alkaline leaching dissolution;
s6: and concentrating and crystallizing the pickle liquor obtained in the step S2 to obtain ferric sulfate.
Example 2
The main chemical composition SiO in the lithium-rich clay of this embodiment242.85% Fe2O35.38% of Al 2O3Content of 36.03%, Li2The O content is 0.98 per mill. The method comprises the following specific steps:
s1: crushing and grinding the lithium-rich clay to 400 meshes to obtain a lithium-rich clay powdery sample;
s2: placing the lithium-rich clay mineral powder powdery sample obtained in S1 into a sulfuric acid solution with the concentration of 2mol/L according to the mass ratio of 8:1, stirring and dissolving for 0.5h at the temperature of 100 ℃, and filtering and separating to obtain acid leaching solution and acid leaching residue;
s3: mixing the acid leaching residue obtained in the step S2 with a sodium hydroxide solution with the mass concentration of 40% according to the mass ratio of 1:3.5, stirring for 0.5h at the temperature of 100 ℃, and filtering to obtain an alkali leaching solution and an alkali leaching residue;
s4: heating the alkali leaching solution obtained in the step S3 to 100 ℃, introducing carbon dioxide gas with the mass concentration of 40%, stopping introducing the carbon dioxide when the pH value of the solution reaches 10.5, and filtering to obtain lithium carbonate and carbonation mother liquor, wherein the recovery rate of the lithium carbonate is 97.84% by calculation;
s5: adding 20 percent of Ca (OH) into the carbon content mother liquor obtained in the S42(causticizing process) and stirring, when the precipitate is not generated any more, stopping adding Ca (OH)2The solution was filtered, and the filtrate was returned as a sodium hydroxide solution to step S3 to continue the alkaline leaching.
S6: and concentrating and crystallizing the pickle liquor obtained in the step S2 to obtain ferric sulfate.
Comparative example
This comparative example was conducted on the basis of example 1 except that the sulfuric acid solution was used at a concentration of 6mol/L and the recovery rate of lithium carbonate finally obtained was 87.95%.
Compared with the sulfuric acid roasting method, the method has the advantages of low energy consumption (roasting process is not needed, energy consumption and cost are greatly reduced), low equipment requirement (the sulfuric acid roasting method requires high pressure resistance, high temperature resistance and corrosion resistance of equipment, and large equipment loss), and simple process (the sulfuric acid roasting method has complex process and long period).
Compared with the oxidation roasting-acid leaching method, the method has the advantages of low cost (the oxidation roasting-acid leaching method needs roasting temperature of 600-900 ℃ and does not need roasting), good process controllability (the technology is easy to control, the impurity removal process of the oxidation roasting-acid leaching method is complex), high utilization rate (the recovery rate of lithium extracted by the oxidation roasting-acid leaching method is low), high product quality (the product obtained by the oxidation roasting-acid leaching method is low), and low production cost.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention will still fall within the protection scope of the technical solution of the present invention.
Claims (9)
1. A method for extracting lithium carbonate from lithium-rich clay by an acid-base combined method is characterized by comprising the following steps:
s1, crushing and grinding the lithium-rich clay to obtain a lithium-rich clay powdery sample;
s2, adding a sulfuric acid solution into the lithium-rich clay powder obtained in the step S1 for leaching, and then filtering and separating to obtain acid leaching solution and acid leaching residues;
s3, adding a sodium hydroxide solution into the acid leaching residue obtained in the step S2 for alkali leaching, and then filtering and separating to obtain an alkali leaching solution and an alkali leaching residue;
s4, introducing carbon dioxide gas into the alkali leaching solution obtained in the step S3, and then filtering to obtain lithium carbonate solid and carbon mother liquor;
s5, adding Ca (OH) into the carbon content mother liquor obtained in the step S32Stirring and filtering the solution, and returning the obtained filtrate as a sodium hydroxide solution to the next reaction in step S3 for alkaline leaching dissolution;
s6, concentrating and crystallizing the pickle liquor obtained in the step S2 to obtain ferric sulfate;
in step S2, the concentration of the sulfuric acid solution is 1-3 mol/L, the leaching is carried out at 40-100 ℃, the stirring is carried out simultaneously in the leaching process, the stirring speed is 300-500 r/min, and the time is 0.5-3 h.
2. The method for extracting lithium carbonate according to claim 1, wherein in step S1, the lithium-rich clay is crushed and ground to 100 to 400 mesh.
3. The method for extracting lithium carbonate according to claim 1, wherein the concentration of the sulfuric acid solution is 2 to 3 mol/L.
4. The method for extracting lithium carbonate according to claim 1, wherein in step S2, the ratio of the sulfuric acid solution to the lithium-rich clay powder is 5-10: 1, mixing.
5. The method for extracting lithium carbonate according to claim 1, wherein in the step S3, the mass concentration of the sodium hydroxide solution is 10% to 40%, and the solid-liquid mass ratio of the acid leaching residue to the sodium hydroxide solution is 1:3 to 10.
6. The method for extracting lithium carbonate according to claim 1, wherein in step S3, the temperature of the alkaline leaching is maintained at 60 to 100 ℃, and the leaching time is 0.5 to 2 hours.
7. The method for extracting lithium carbonate according to claim 1, wherein in step S4, the carbon dioxide gas contains carbon dioxide at a concentration of 20% to 40%, and the alkaline leaching solution is heated to 60 ℃ to 100 ℃.
8. The method for extracting lithium carbonate according to claim 1, wherein in step S4, when the pH value in the alkali leaching solution is measured to be 8.5 to 10.5, the introduction of carbon dioxide gas is stopped.
9. The method for extracting lithium carbonate according to claim 1, wherein in step S5, ca (oh) 2The mass fraction of the solution is 5% -30%, when no precipitate is generated in the solution, the addition of Ca (OH) is stopped2And (3) solution.
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| CN114934196B (en) * | 2022-07-12 | 2024-01-19 | 长安大学 | Lithium extraction method for low-aluminum lithium-rich clay |
| CN116477858A (en) * | 2023-02-28 | 2023-07-25 | 四川顺应锂材料科技有限公司 | Method for preparing battery-grade lithium carbonate by pressure leaching of clay lithium ore |
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