CN113753924B - Method for extracting lithium carbonate and co-producing sodium aluminosilicate from lithium-rich clay by activated water dissolution method - Google Patents

Method for extracting lithium carbonate and co-producing sodium aluminosilicate from lithium-rich clay by activated water dissolution method Download PDF

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CN113753924B
CN113753924B CN202111154692.1A CN202111154692A CN113753924B CN 113753924 B CN113753924 B CN 113753924B CN 202111154692 A CN202111154692 A CN 202111154692A CN 113753924 B CN113753924 B CN 113753924B
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lithium
water
sodium
rich clay
filtering
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CN113753924A (en
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潘爱芳
马昱昭
孙悦
马润勇
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Pan Aifang
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00Lithium compounds
    • C01D15/08Carbonates; Bicarbonates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/26Aluminium-containing silicates, i.e. silico-aluminates

Abstract

The invention relates to a method for extracting lithium carbonate and coproducing sodium aluminosilicate from lithium-rich clay by an activated water dissolution method, which comprises the following steps: uniformly mixing the lithium-rich clay with alkali and a leaching agent, grinding the mixture into powder, and roasting to obtain roasted clinker; adding water for reaction, filtering and separating to obtain a first water leaching solution and water leaching slag, adding sodium aluminate or sodium silicate into the first water leaching solution, aging, and filtering to obtain a second water leaching solution and sodium aluminosilicate precipitate; introducing carbon dioxide gas into the second water leaching solution, and then filtering and separating the solution to obtain a lithium carbonate product and a carbon dioxide mother liquor; heating the carbon content mother liquor, and after completely evaporating to dryness, recycling the obtained crystal as alkali. The method provided by the invention has the advantages of simple and easy operation method, no special requirements on equipment, good controllability of process parameters, environmental protection, no wastewater discharge, low cost, high quality of obtained products, good economic benefit and the like, and opens up a new way for the development and utilization of the lithium-rich clay.

Description

Method for extracting lithium carbonate and co-producing sodium aluminosilicate from lithium-rich clay by activated water dissolution method
Technical Field
The invention relates to a method for extracting lithium carbonate and co-producing sodium aluminosilicate from lithium-rich clay by an activated water dissolution method, belonging to the technical field of metallurgy and mineral product utilization.
Background
Lithium, called "high-energy metal", "energy metal" and "metal promoting world progress", is widely used in advanced industrial fields such as new energy development, nuclear industry, aerospace and national defense, and has extremely high economic and strategic values, so that it is listed in key mineral catalogues by China. The lithium mine resources in China are rich, and the resource amount is 54 multiplied by 105t, accounting for about 13.8% of the total world resource. 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 dependency degree is as high as 76%. Currently, the lithium deposit resources exploited and utilized worldwide mainly include pegmatite deposits and brine 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 shortage of lithium resources in China can be effectively relievedThe situation is that.
At present, the process technology for extracting lithium from lithium ore mainly comprises a limestone roasting method, a sulfuric acid method, a limestone method, a soda process and the like. The sulfuric acid method has wide application range, but has high energy consumption and low value of byproducts, so that the process has high cost; the limestone method needs to mix minerals such as lepidolite and the like with limestone according to the mass ratio of about 1:3, lithium in the minerals is converted into a soluble state through high-temperature calcination, and the process needs to input a large amount of calcium-containing materials and has high calcination condition requirements, high reaction energy consumption and high cost; sodium-containing filter residue with low value is generated when lithium is extracted by a soda ash method, so that the recycling availability of the filter residue is poor, a large amount of solid waste which is low in recycling value and difficult to treat is generated when lithium is extracted by the whole process, and the process is not environment-friendly. Therefore, the problems of high energy consumption, high equipment requirement, large slag yield and the like generally exist in the conventional lithium extraction process from the lithium-rich clay ore. And the lithium in the clay mineral is mainly existed in the clay mineral, and obviously, the process can not be directly adopted for extracting the lithium. 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 and co-producing sodium aluminosilicate from lithium-rich clay by an activated water dissolution method, wherein lithium of the lithium-rich clay ore is separated and extracted, a lithium carbonate product is converted, and silicon and aluminum are separated and extracted to form sodium aluminosilicate.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a method for extracting lithium carbonate and co-producing sodium aluminosilicate from lithium-rich clay by an activated water dissolution method comprises the following steps:
step 1: evenly mixing the lithium-rich clay with alkali and a melting agent, grinding to obtain powder of 100-300 meshes to obtain mixed raw material,
and 2, step: roasting the mixed raw material obtained in the step 1 at a high temperature to obtain roasted clinker;
and step 3: placing the roasted clinker obtained in the step 2 into water, filtering and separating after reaction to obtain a first water leaching solution and water leaching slag,
and 4, step 4: adding sodium aluminate or sodium silicate into the first water extract obtained in the step (3) to adjust the concentration of the sodium aluminate and the concentration of the sodium silicate, aging, and filtering to obtain a second water extract and sodium aluminosilicate precipitate;
and 5: introducing carbon dioxide gas into the second water extract obtained in the step (4), adjusting the pH value of the solution to 8.5-10.5, stopping introducing the carbon dioxide, and filtering and separating the solution to obtain a precipitate and a carbon content mother solution;
step 6: heating the carbon content mother liquor obtained in the step 5, and after the carbon content mother liquor is completely evaporated to dryness, taking the obtained crystals as alkali which can be used for returning to the material prepared in the step 1 in the next batch of raw materials so as to reduce the consumption of the raw materials;
and 7: and washing the precipitate with water, and drying to obtain a lithium carbonate product.
In the method, preferably, in step 1, the mass ratio of the lithium-rich clay to the alkali is 1: 0.5-1.5, and the blending is performed, wherein the addition amount of the melting-out agent is 1-10 per mill of the lithium-rich clay.
In the method as described above, preferably, in step 1, the fusing agent is sodium sulfate and the alkali is sodium carbonate.
In the method, preferably, in the step 2, the roasting temperature is 600-1000 ℃, and the roasting time is 20-60 min.
In the method as described above, preferably, in step 3, the solid-to-liquid ratio of the calcined clinker to water is 1: 3-10 times.
In the method as described above, preferably, in step 4, the sodium aluminate or sodium silicate is added in an amount of a difference in the lithium-rich clay such that the amount of the substance containing silicon or aluminum element is equal.
In the method, preferably, in the step 4, the aging temperature is 40-100 ℃, and the aging time is 1-10 h.
In the method as described above, preferably, in step 5, the concentration of the carbon dioxide gas is maintained at 30% to 40%.
In the method, the heating temperature in step 6 is preferably 60-100 ℃.
(III) advantageous effects
The invention has the beneficial effects that:
(1) according to the method for extracting lithium carbonate and co-producing sodium aluminosilicate from lithium-rich clay by the activated water dissolution method, after the lithium-rich clay ore is mixed and roasted with alkali and a melting agent, lithium in the lithium-rich clay can be effectively extracted through dissolution, impurity removal and decomposition processes, and is separated and converted into a lithium carbonate product, and meanwhile, aluminum and silicon in the clay are converted into sodium aluminosilicate.
(2) According to the method for extracting lithium carbonate and co-producing sodium aluminosilicate from lithium-rich clay by the activated water dissolution method, alkali added in the process flow is obtained through the subsequent steps, and recycling can be achieved.
(3) The method for extracting lithium carbonate and co-producing sodium aluminosilicate from the lithium-rich clay by the activated water dissolution method provided by the invention has the advantages of simple and easy operation method, no special requirements on equipment, good controllability of process parameters, environmental friendliness, no wastewater discharge, low cost, high quality of obtained products, good economic benefits and the like, and opens up a new way for development and utilization of the lithium-rich clay.
Detailed Description
The invention provides a method for extracting lithium carbonate and coproducing sodium aluminosilicate from lithium-rich clay by an activated water dissolution method, which comprises the following steps:
step 1: mixing the lithium-rich clay, alkali and a melting agent according to a certain mass ratio, and grinding the mixture to 100-300 meshes to obtain a mixed raw material, wherein the melting agent is sodium sulfate;
step 2: roasting the mixed raw material obtained in the step 1 at 600-1000 ℃ for a certain time to obtain roasted clinker;
the reactions occurring in this step are mainly as follows:
Al2O3+Na2CO3=2NaAlO2+CO2
SiO2+Na2CO3=Na2SiO3+CO2↑;
researches show that the lithium-rich clay is roasted by adding alkali and a melting agent to generate sodium aluminate and sodium silicate, and lithium sulfate is obtained by position conversion.
And step 3: placing the roasted clinker obtained in the step (2) in water, reacting for 5-30 min at normal temperature-90 ℃ according to a certain liquid-solid ratio, and filtering and separating to obtain a first water leaching solution and water leaching slag;
the main reaction of this step is as follows:
Na2SiO3+NaAlO2+H2O=NaAlSiO4↓+2NaOH;
the water leaching residue contains sodium aluminosilicate and iron-containing precipitate, and the first water leaching solution contains lithium ion solution and excessive AlO2 -Or SiO3 2-Ions.
And 4, step 4: adding sodium aluminate or sodium silicate into the first water extract obtained in the step (3) to adjust the concentration of the sodium aluminate and the concentration of the sodium silicate, aging for a certain time at a certain temperature, and filtering to obtain a second water extract and sodium aluminosilicate (NaAlSiO)4) Precipitating;
the reaction in this step mainly takes place as follows:
Na2SiO3+NaAlO2+H2O=NaAlSiO4↓+2NaOH;
adding sodium aluminate or sodium silicate to convert AlO2 -Or SiO3 2-The ions are completely precipitated, only the solution containing lithium and sodium ions remains,
and 5: introducing carbon dioxide gas into the second water extract obtained in the step (4), adjusting the pH of the solution to 8.5-10.5, and filtering and separating to obtain a precipitate and a carbon content mother liquor;
the reactions that mainly occur in this step are as follows:
2LiSO4+CO2=Li2CO3↓+H2SO4
NaOH+CO2=Na2CO3+H2O;
NaOH+H2SO4=Na2SO4+H2O
step 6: and (3) heating the carbon content mother liquor obtained in the step (5), and after the carbon content mother liquor is completely evaporated to dryness, taking the obtained crystals (sodium carbonate) as alkali, and returning the obtained crystals to the step (1) for preparing the raw materials in the next batch to reduce the consumption of the raw materials.
And 7: the precipitate was washed with water and dried to give a lithium carbonate product.
According to the invention, sodium sulfate and alkali are calcined to separate and replace lithium in the lithium-rich clay by adopting high-temperature sintering, the clay structure is changed from compact to loose, the reaction is easy, then the roasted product is subjected to water leaching, solid-liquid separation is carried out, carbon dioxide gas is introduced into the filtrate to generate precipitation, lithium carbonate and carbon content mother liquor are obtained by filtration and separation, and lithium is effectively separated from the lithium-rich clay to obtain a lithium carbonate product.
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
The main component of the lithium-rich clay in this embodiment is SiO242.85% Fe2O35.38% of Al2O3Content of 36.03%, Li2The O content is 0.98 per mill. The method comprises the following specific steps:
step 1: mixing and uniformly mixing the lithium-rich clay, sodium carbonate and a melting agent according to the mass ratio of 1:0.5:0.001, and grinding the mixture to 100 meshes to obtain a mixed raw material; the fusing agent adopts sodium sulfate;
step 2: roasting the mixed raw material obtained in the step 1 for 60min at 850 ℃ to obtain roasted clinker;
and step 3: placing the roasted clinker obtained in the step 2 into water, wherein the water consumption is 3: 1, adding water, stirring and dissolving for 30min at normal temperature, and filtering and separating to obtain a first water extract and water extract residues;
and 4, step 4: adding sodium aluminate into the first water leaching solution, wherein the adding amount of the sodium aluminate is equal to the amount of the residual sodium silicate in the first water leaching solution, aging for 10 hours at the temperature of 40 ℃, filtering to obtain a second water leaching solution and a sodium aluminosilicate precipitate, and calculating the recovery rate of the sodium aluminosilicate to be 94.57%;
and 5: and (4) introducing carbon dioxide gas with the mass concentration of 20% into the second water extract obtained in the step (4), stopping introducing the carbon dioxide when the pH value in the solution is 8.5, and filtering and separating to obtain a precipitate and a carbon content mother liquor.
Step 6: and (3) heating the carbon content mother liquor obtained in the step (5) to 80 ℃, and after the carbon content mother liquor is completely evaporated to dryness, taking the obtained crystal as sodium carbonate, wherein the sodium carbonate can be used for material preparation in the step (1) in a new batch of lithium-rich clay to reduce raw material consumption.
And 7: the precipitate is washed once with water and dried to form the lithium carbonate product. The calculated recovery rate of lithium can reach 98.93%.
Example 2
SiO in the lithium-rich clay of the embodiment240.53% Fe2O35.57% of Al2O3Content of 38.37% Li2The O content is 1.02 per mill. The method comprises the following specific steps:
step 1: mixing the lithium-rich clay, sodium carbonate and a melting agent uniformly according to the proportion of 1:1.5:0.01, and grinding to 200 meshes to obtain a mixed raw material;
step 2: roasting the mixed raw material obtained in the step 1 for 20min at 980 ℃ to obtain roasted clinker;
and step 3: placing the roasted clinker obtained in the step 2 into water, wherein the water consumption is as follows according to the liquid-solid ratio of 10: 1, adding water, stirring and dissolving for 5min at the temperature of 90 ℃, and then filtering and separating to obtain a first water extract and water extract residues;
and 4, step 4: adding sodium silicate into the first water leaching solution obtained in the step 3, wherein the adding amount of the sodium silicate enables the amount of the sodium silicate to be equal to that of the residual sodium aluminate in the first water leaching solution, aging for 1 hour at the temperature of 100 ℃, and filtering to obtain a second water leaching solution and sodium aluminosilicate, wherein the recovery rate of the sodium aluminosilicate is 94.64% by calculation;
and 5: introducing carbon dioxide gas with the mass concentration of 40% into the second water extract obtained in the step (4), stopping introducing the carbon dioxide when the pH value in the solution is 8.5, and filtering and separating to obtain carbon-neutral mother liquor;
step 6; and (3) heating the carbon content mother liquor obtained in the step (5) to 100 ℃, and after the carbon content mother liquor is completely evaporated to dryness, taking the obtained crystals as sodium carbonate to return to the mixture obtained in the step (1) so as to reduce the consumption of raw materials.
And 7: the precipitate is washed once with water and dried to form the lithium carbonate product. The calculated lithium recovery rate can reach 98.22 percent
Compared with the direct acid dissolution method in the prior art, the method has the advantages of high comprehensive utilization rate, capability of fully recovering the components such as aluminum, silicon, lithium and the like in the lithium-rich clay, capability of reducing the loss of raw materials such as auxiliaries and the like to the greatest extent, environmental friendliness, no waste water discharge (a large amount of acid solution is required for the discharge of the direct acid dissolution method in the prior art), and no special requirements on equipment (the direct acid dissolution method generally requires high pressure and high temperature resistance of the equipment).
Compared with the sulfate roasting-acid leaching method in the prior art, the method has the advantages that the auxiliary agent can be recycled, the roasting auxiliary agent is difficult to recover and seriously wasted in the sulfate roasting-acid leaching method in the prior art, and the obtained product has large residual quantity of the roasting auxiliary agent, so that the method is not economical and practical. Therefore, the method has the advantages of low cost, high quality of obtained products, good economic benefit, various products obtained by the method, high added value products and the like.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art can change or modify the technical content disclosed above into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (3)

1. A method for extracting lithium carbonate and co-producing sodium aluminosilicate from lithium-rich clay by an activated water dissolution method is characterized by comprising the following steps:
step 1: evenly mixing the lithium-rich clay with alkali and a melting agent, grinding the mixture to 100-300 meshes to obtain a mixed raw material,
step 2: roasting the mixed raw material obtained in the step 1 at a high temperature to obtain roasted clinker;
and step 3: placing the roasted clinker obtained in the step 2 into water, filtering and separating after reaction to obtain a first water leaching solution and water leaching slag,
and 4, step 4: adding sodium aluminate or sodium silicate into the first water extract obtained in the step (3) to adjust the concentration of the sodium aluminate and the concentration of the sodium silicate, aging, and filtering to obtain a second water extract and a sodium aluminosilicate precipitate;
and 5: introducing carbon dioxide gas into the second water extract obtained in the step (4), adjusting the pH value of the solution to 8.5-10.5, stopping introducing the carbon dioxide, and filtering and separating the solution to obtain a precipitate and a carbon content mother solution;
and 6: heating the carbon content mother liquor obtained in the step 5, and after the carbon content mother liquor is completely evaporated to dryness, taking the obtained crystals as alkali which can be used for returning to the material prepared in the step 1 in the next batch of raw materials so as to reduce the consumption of the raw materials;
and 7: washing the precipitate with water, and drying to obtain a lithium carbonate product;
in the step 1, the mass ratio of the lithium-rich clay to the alkali is 1: 0.5-1.5, blending is carried out, and the addition amount of the melting-out agent is 1-10 per mill of the lithium-rich clay;
the fusing agent is sodium sulfate, and the alkali is sodium carbonate;
in the step 2, the roasting temperature is 600-1000 ℃, and the roasting time is 20-60 min;
in step 3, the solid-to-liquid ratio of the roasting clinker to water is 1: 3-10 times of the steps;
in step 4, the sodium aluminate or sodium silicate is added in a difference amount which enables the substances containing silicon or aluminum elements to be equal in amount in the lithium-rich clay;
in the step 4, the aging temperature is 40-100 ℃, and the aging time is 1-10 h.
2. The method of claim 1, wherein the concentration of the carbon dioxide gas is maintained at 30% to 40% in step 5.
3. The method according to claim 1, wherein the heating temperature in step 6 is 60 to 100 ℃.
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