CN110563009A - Method for preparing battery-grade lithium carbonate from fly ash by carbonization decomposition method - Google Patents
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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
- C01D15/08—Carbonates; Bicarbonates
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- C01—INORGANIC CHEMISTRY
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Abstract
The invention discloses a method for preparing battery-grade lithium carbonate by using a lithium-containing solution in a fly ash aluminum extraction process, which relates to the technical field of lithium extraction by an adsorption method and the technical field of battery-grade lithium carbonate preparation, and is implemented based on the adsorption separation of lithium in the lithium-containing solution and the preparation of the battery-grade lithium carbonate obtained in the fly ash aluminum extraction process, and comprises the following steps: adsorbing and extracting lithium, concentrating, carbonating and precipitating, carbonizing and removing impurities, heating and decomposing, and crushing. The method can effectively extract lithium in the fly ash, prepare battery-grade lithium carbonate, provide a new idea for comprehensive utilization of the fly ash, and improve economic benefits.
Description
Technical Field
the invention relates to a preparation method of lithium carbonate, in particular to a method for preparing battery-grade lithium carbonate by utilizing fly ash
Background
lithium is the lightest metal element in nature, is a very active alkali metal element, is widely applied to the metallurgical industry and is generally used as a deoxidizer and a desulfurizer. In addition, with the rapid development of the battery industry and new energy automobiles, the utilization value of lithium even exceeds that of precious metals, and the lithium becomes an "energy metal" in the 21 st century, so that the demand of lithium is continuously increased.
Lithium resources in nature are mainly stored in lithium ores, salt lake brine and seawater. Lithium extraction from lithium ore is the first method adopted and developed, including high-temperature high-pressure acid leaching method, high-temperature roasting method, etc., and these methods have the problems of high energy consumption, high equipment requirement, etc. The technological process of extracting lithium from salt lake bittern in sea water includes mainly evaporation and crystallization separation, salting out, selective semi-permeable membrane process, calcination and leaching, precipitation, solvent extraction, ion exchange, adsorption, etc. The extraction of lithium from brine is mainly limited by impurities such as magnesium, calcium, boron and the like in the brine, and the content of the impurities increases the extraction difficulty of lithium.
China takes coal as basic fuel for power production, and the discharge amount of fly ash is increased rapidly along with the rapid development of the power industry in China. The fly ash is used as a potential urban mineral resource, the chemical composition of the fly ash is relatively complex, and the main substance comprises SiO2、A12O3、Fe2O3、CaO、MgO、K2O、Na2O、P2O5、TiO2、MnO、SO3Etc. of SiO2About 35.6-57.2% by mass of A12O3The mass fraction is about 18.8% to 55.0%, and is a typical aluminosilicate mineral. Therefore, the fly ash is mostly used for preparing aluminum-silicon products, the current methods for treating the fly ash are mainly divided into an acid method and an alkali method, lithium can be enriched in different forms in different methods, and the problems of low extraction rate and low product purity exist in the current stage of the method for extracting lithium from fly ash. Patent CN107758714 discloses a method for 'a combined method for extracting aluminum, silicon, lithium and gallium from fly ash synergistically', which is a process method for extracting aluminum oxide by using Bayer process. The method is based on a certain fly ash reinforced desiliconization-mild alkaline process aluminum lithium gallium synergistic extraction process, extracts lithium and prepares battery-grade lithium carbonate, and improves the comprehensive utilization level of the fly ash.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide an extraction method of lithium in a synergistic extraction process of aluminum, lithium and gallium based on certain fly ash enhanced desiliconization-mild alkaline method.
The technical scheme of the invention is that the method for preparing battery-grade lithium carbonate from fly ash by using a carbonization decomposition method comprises the following steps of:
(1) absorbing and extracting lithium: carrying out lithium ion adsorption by using a lithium ion adsorbent and a lithium-containing solution generated by a fly ash aluminum extraction process, and desorbing by using a desorption solution and the adsorbent subjected to the lithium ion adsorption to obtain a desorption solution; the adsorption temperature is 10-80 ℃, and the using amount of the purifying liquid is 1-30 BV; the desorption temperature is 10-80 ℃, and the dosage of the desorbent is 1-30 BV;
(2) Concentration: concentrating the desorption solution obtained in the step (1) to obtain a concentrated solution, and filtering the concentrated solution to obtain a filtrate, wherein the content of suspended substances in the filtered filtrate is lower than 0.01 g/L;
(3) carbonation and precipitation: adding a carbonate solution into the filtrate obtained in the step (2) at the speed of 0.5-5L/h, stirring, carrying out precipitation reaction at the temperature of 40-120 ℃, filtering the obtained precipitate, and drying to obtain a primary lithium carbonate product; the dosage of the carbonate solution is 1-3 times of the theoretical dosage of lithium ions by mole;
(4) And (3) carbonization and impurity removal: mixing the primary lithium carbonate product obtained in the step (3) with water, introducing carbon dioxide gas, stirring, and filtering after the reaction is finished to obtain a lithium bicarbonate solution;
(5) Heating and decomposing: heating and decomposing the lithium bicarbonate solution in the step (4) to obtain a product lithium carbonate, wherein the decomposition temperature of the lithium bicarbonate solution is 60-150 ℃;
(6) Crushing: and (5) further crushing the lithium carbonate product in the step (5) to obtain battery-grade lithium carbonate meeting the requirements.
According to the method for preparing battery-grade lithium carbonate from fly ash by using the carbonization decomposition method, in the step (1), preferably, the lithium-containing solution in the process of extracting lithium from fly ash comprises a pre-desilication solution, a circulating solution, a crude solution, a seed precipitation solution, a carbon distillation mother solution and a carbon distillation raw solution.
The fly ash aluminum extraction process refers to a fly ash reinforced desilication-mild alkaline method aluminum lithium gallium synergistic extraction process.
The amount of carbonate added affects the yield of the product; the temperature of the precipitation reaction affects the yield and purity of the product; the thermal decomposition temperature affects the yield of the product.
According to the method for preparing battery-grade lithium carbonate from fly ash by using the carbonization decomposition method, in the step (1), the lithium ion adsorbent is preferably selected from any one or more of manganese ion sieves, titanium ion sieves, niobium ion sieves, zirconium ion sieves, aluminum salt adsorbents, nickel adsorption resins or chelating resins;
preferably, the desorbent used in the step (1) is one or more of water, lithium chloride solution, dilute hydrochloric acid and dilute sulfuric acid.
According to the method for preparing the battery-grade lithium carbonate from the fly ash by the carbonization decomposition method, the lithium-containing solution passes through a packed column loaded with an adsorbent at a flow rate of 1-10BV/h during adsorption in the step (1);
Preferably, the desorbent flows through the packed column at a flow rate of 1-10BV/h during desorption in step (1).
according to the method for preparing battery-grade lithium carbonate from fly ash by using the carbonization decomposition method, in the step (2), the lithium ion concentration in the concentrated solution after concentration is preferably 1-30 g/L.
more preferably, in the step (2), the concentration of lithium ions in the concentrated solution after concentration is 15 to 30 g/L.
according to the method for preparing battery grade lithium carbonate from fly ash by carbonization decomposition, the carbonate used in the step (3) is preferably selected from sodium carbonate or potassium carbonate; the concentration of the carbonate in the step (3) is 5-40% by mass concentration.
According to the method for preparing battery-grade lithium carbonate from fly ash by using the carbonization decomposition method, the stirring in the reaction process in the step (3) is preferably carried out by using a stirrer, and the stirring speed is 200-1200 r/min; after the dropwise addition of the carbonate solution in the step (3) is finished, continuously stirring and reacting for 0.5-10h, and then filtering;
preferably, the precipitate in step (3) is filtered and washed before drying. I.e. it may not be washed.
Further, the washing is that the product is washed with hot water.
Further, it means washing with hot water at 50-100 deg.C for 1-6 times. The amount of hot water is 50-300ml each time.
according to the method for preparing battery grade lithium carbonate from fly ash by the carbonization decomposition method, the primary lithium carbonate product and water in the step (4) are preferably mixed according to the liquid-solid ratio (1-50): 1, mixing;
preferably, the flow rate of the carbon dioxide gas in the step (4) is 1-10BV/h, and the reaction time is 1-20 h. The expression gas flow rate is only applicable to the experimental set-up, as the case may be if industrialization is required, where BV is a multiple of the reactor volume.
preferably, in the step (4), a stirrer is adopted for stirring, and the stirring speed is 200-1200 r/min.
According to the method for preparing the battery-grade lithium carbonate from the fly ash by the carbonization decomposition method, the reaction time of the step (5) is preferably 1-20 h.
According to the method for preparing battery-grade lithium carbonate from fly ash by using the carbonization decomposition method, the crushing device used in the step (6) is preferably one or more selected from a box-type crusher, a gas flow crusher, a superfine crusher, a freezing crusher, a low-temperature crusher, a turbine crusher and a superfine crusher.
Has the advantages that:
The method mainly aims at the technological process of fly ash reinforced desiliconization-mild alkaline process aluminum lithium gallium synergistic extraction, selects a resin adsorption method to remove impurity ions, and further uses a carbonization decomposition method to deeply remove impurities. The method is beneficial to extracting lithium from the strong alkaline solution and preparing the battery-grade lithium carbonate product, the total energy consumption is low, the product yield is over 80 percent, and the purity granularity meets the requirement of the battery-grade lithium carbonate.
Drawings
FIG. 1 is a flow chart of a synergistic extraction process of aluminum, lithium and gallium by a fly ash reinforced desilication-mild alkaline method;
FIG. 2 is a flow chart of an embodiment of the present invention;
FIG. 3 is a curve showing the variation of the concentration of lithium ions in the effluent of the adsorption column with the amount of the purification solution;
Fig. 4 is a graph of the effect of operating temperature on lithium bicarbonate decomposition.
Detailed Description
the present invention is described with reference to the accompanying drawings and detailed description so that the advantages and features of the invention will be more readily understood by those skilled in the art, and the scope of the invention will be more clearly defined.
the invention is described in detail below with reference to the figures and the embodiments. The following examples are only illustrative of the present invention, and the scope of the present invention shall include the full contents of the claims, and not be limited to the following examples.
The lithium extraction raw material is taken from a lithium-containing solution in each working section of a certain fly ash aluminum extraction process, and the parameters are shown in table 1.
TABLE 1 lithium-containing solution parameters for each section
example 1:
(1) Passing the pre-desiliconized solution through an adsorption column loaded with an aluminum salt adsorbent at the flow rate of 5BV/h to perform lithium ion adsorption, wherein the adsorption temperature is 60 ℃, and the using amount of a purifying solution is 5 BV;
(2) desorbing the adsorbent subjected to lithium ion adsorption by using a lithium chloride solution with the concentration of 150ppm, wherein the flow rate of the lithium chloride solution is 5BV/h during desorption, the desorption temperature is 25 ℃, and the using amount of the desorption agent is 5BV, so as to obtain a desorption solution.
(3) and transferring the desorption solution into evaporation concentration equipment, and concentrating until the concentration of lithium ions in the concentrated solution is 25g/L to obtain a concentrated solution. The concentrate was filtered to a suspended matter content of less than 0.01 g/L.
(4) Heating 200mL of concentrated solution to 80 ℃, adding 200mL of sodium carbonate solution with the mass fraction of 30% into the solution at the speed of 1L/h, stirring and reacting for 1h after dropwise addition, filtering, and washing a filter cake for 0-3 times by using hot water at the temperature of 75 ℃, wherein the dosage is 150mL each time. The results are shown in Table 2.
(5) mixing the product with water at a liquid-solid ratio of 20:1, introducing carbon dioxide at a gas speed of 1L/h, stirring and reacting at normal temperature for 100min, and heating the filtered lithium bicarbonate solution at 70 ℃ for 5h to obtain the product.
(6) And (4) crushing the product by using a jet mill to meet the requirement of the granularity of the battery-grade lithium carbonate.
TABLE 2 influence of washing times on purity and yield of lithium carbonate
Since lithium carbonate has a slight solubility in water, a small amount of lithium carbonate dissolves when washed with water, and the yield is lowered.
example 2:
(1) enabling the circulating liquid to pass through an adsorption column loaded with nickel adsorption resin at the flow rate of 3BV/h for lithium ion adsorption, wherein the adsorption temperature is 50 ℃, and the using amount of the purifying liquid is 20 BV;
(2) Desorbing the adsorbent subjected to lithium ion adsorption by using hydrochloric acid with the concentration of 2moL/L, wherein the flow rate of the hydrochloric acid is 3BV/h, the desorption temperature is 30 ℃, and the using amount of the desorbent is 5BV, so as to obtain desorption liquid.
(3) And transferring the desorption solution into evaporation concentration equipment, and concentrating until the concentration of lithium ions in the concentrated solution is 20g/L to obtain a concentrated solution. The concentrate was filtered to a suspended matter content of less than 0.01 g/L.
(4) Heating 200mL of concentrated solution to 80 ℃, introducing 180mL of sodium carbonate solution with the mass fraction of 30% into the solution at the speed of 2L/h, stirring and reacting for 1h after the dropwise addition is finished, then aging for 1h, filtering, and washing a filter cake for 4 times by using hot water at 80 ℃ with the dosage of 150mL each time. The weight after drying was 33.17 g.
(5) and mixing the product with water at a liquid-solid ratio of 30:1, introducing carbon dioxide at a gas speed of 2BV/h, stirring and reacting for 80min at normal temperature, heating the filtered lithium bicarbonate solution at 80 ℃ for 6h, and drying to obtain a lithium carbonate product, wherein the product yield is 82.3%, and the purity is 99.6%.
(6) and (4) crushing the product by using a jet mill to meet the requirement of the granularity of the battery-grade lithium carbonate.
Example 3:
(1) enabling the carbon evaporation mother liquor to pass through an adsorption column loaded with chelating resin at the flow rate of 5BV/h, and performing lithium ion adsorption, wherein the adsorption temperature is 40 ℃, and the using amount of a purifying solution is 5 BV;
(2) desorbing the adsorbent subjected to lithium ion adsorption by using hydrochloric acid with the concentration of 0.5moL/L, wherein the flow rate of the hydrochloric acid during desorption is 5BV/h, the desorption temperature is 40 ℃, and the using amount of the desorbent is 10BV, so as to obtain desorption liquid.
(3) Transferring the desorption solution into evaporation concentration equipment, concentrating until the concentration of lithium ions in the concentrated solution is 15g/L, and filtering the concentrated solution to ensure that the content of suspended matters is lower than 0.01 g/L.
(4) Heating 200mL of concentrated solution to 90 ℃, introducing 500mL of sodium carbonate solution with the mass fraction of 15% into the solution at the speed of 5L/h, stirring and reacting for 1h after the dropwise addition is finished, then aging for 1h, filtering, and washing a filter cake for 5 times by using hot water at the temperature of 75 ℃, wherein the dosage of each time is 120 mL. The weight after drying was 31.06 g.
(5) And mixing the product with water at a liquid-solid ratio of 25:1, introducing carbon dioxide at a gas speed of 2L/h, stirring and reacting for 120min at normal temperature, heating the filtered lithium bicarbonate solution at 90 ℃ for 5h, and drying to obtain a lithium carbonate product, wherein the product yield is 81.6%, and the purity is 99.7%. The product results are analyzed in Table 3.
(6) and (4) crushing the product by using a jet mill to meet the requirement of the granularity of the battery-grade lithium carbonate.
TABLE 3 analysis of the product lithium carbonate
Example 4:
(1) Allowing the carbon evaporation stock solution to pass through an adsorption column loaded with chelating resin at the flow rate of 1BV/h for lithium ion adsorption, wherein the adsorption temperature is 20 ℃, and the using amount of a purifying solution is 6 BV;
(2) Desorbing the adsorbent subjected to lithium ion adsorption by using hydrochloric acid with the concentration of 1moL/L, wherein the flow rate of the hydrochloric acid is 1BV/h, the desorption temperature is 20 ℃, and the using amount of the desorbent is 2BV, so as to obtain desorption liquid.
(3) and transferring the desorption solution into evaporation concentration equipment, and concentrating until the concentration of lithium ions in the concentrated solution is 35g/L to obtain concentrated solution. The concentrate was filtered to a suspended matter content of less than 0.01 g/L.
(4) heating 200mL of concentrated solution to 90 ℃, introducing 250mL of sodium carbonate solution with the mass fraction of 30% into the solution at the speed of 4L/h, stirring and reacting for 1h after dropwise addition, filtering, washing a filter cake for 6 times by hot water at the temperature of 80 ℃, and using 120mL of the hot water each time. The weight after drying was 30.25 g.
(5) and mixing the product with water at a liquid-solid ratio of 30:1, introducing carbon dioxide at a gas speed of 2.5L/h, stirring and reacting for 100min at normal temperature, heating the filtered lithium bicarbonate solution at 80 ℃ for 6h, and drying to obtain a lithium carbonate product, wherein the product yield is 81.9%, and the product purity is 99.6%.
(6) And (4) crushing the product by using a freezing crusher to meet the requirement of the granularity of the battery-grade lithium carbonate.
The method is beneficial to extracting lithium from the strong alkaline solution and preparing the battery-grade lithium carbonate product, the total energy consumption is low, the product yield is over 80 percent, and the purity granularity meets the requirement of the battery-grade lithium carbonate.
Claims (10)
1. a method for preparing battery-grade lithium carbonate from fly ash by a carbonization decomposition method comprises adsorption and is characterized in that: the method comprises the following steps:
(1) Absorbing and extracting lithium: carrying out lithium ion adsorption by using a lithium ion adsorbent and a lithium-containing solution generated by a fly ash aluminum extraction process, and desorbing by using a desorption solution and the adsorbent subjected to the lithium ion adsorption to obtain a desorption solution; the adsorption temperature is 10-80 ℃, and the using amount of the purifying liquid is 1-30 BV; the desorption temperature is 10-80 ℃, and the dosage of the desorbent is 1-30 BV;
(2) concentration: concentrating the desorption solution obtained in the step (1) to obtain a concentrated solution, and filtering the concentrated solution to obtain a filtrate, wherein the content of suspended substances in the filtered filtrate is lower than 0.01 g/L;
(3) Carbonation and precipitation: adding a carbonate solution into the filtrate obtained in the step (2) at the speed of 0.5-5L/h, stirring, carrying out precipitation reaction at the temperature of 40-120 ℃, filtering the obtained precipitate, and drying to obtain a primary lithium carbonate product; the dosage of the carbonate solution is 1-3 times of the theoretical dosage of lithium ions by mole;
(4) And (3) carbonization and impurity removal: mixing the primary lithium carbonate product obtained in the step (3) with water, introducing carbon dioxide gas, stirring, and filtering after the reaction is finished to obtain a lithium bicarbonate solution;
(5) Heating and decomposing: heating and decomposing the lithium bicarbonate solution in the step (4) to obtain a product lithium carbonate, wherein the decomposition temperature of the lithium bicarbonate solution is 60-150 ℃;
(6) Crushing: and (5) further crushing the lithium carbonate product in the step (5) to obtain battery-grade lithium carbonate meeting the requirements.
2. the method for preparing battery-grade lithium carbonate from fly ash by using the carbonization decomposition method according to claim 1, wherein in the step (1), the lithium-containing solution in the process for extracting lithium from fly ash comprises a pre-desilication solution, a recycle solution, a crude solution, a seed precipitation solution, a carbon distillation mother solution and a carbon distillation raw solution.
3. The method for preparing battery-grade lithium carbonate from fly ash by carbonization decomposition according to claim 1, wherein in the step (1), the lithium ion adsorbent is selected from any one or more of manganese ion sieve, titanium ion sieve, niobium ion sieve, zirconium ion sieve, aluminum salt adsorbent, nickel adsorbent resin and chelate resin;
The desorbent used in the step (1) is one or more of water, a lithium chloride solution, dilute hydrochloric acid or dilute sulfuric acid.
4. The method for preparing battery-grade lithium carbonate from fly ash by the carbonization decomposition method according to claim 1, wherein the lithium-containing solution during the adsorption in the step (1) passes through a packed column loaded with an adsorbent at a flow rate of 1-10 BV/h;
And (2) flowing the desorbent through the packed column at the flow rate of 1-10BV/h during desorption in the step (1).
5. The method for preparing battery-grade lithium carbonate from fly ash by virtue of carbonization decomposition according to claim 1, wherein in the step (2), the concentration of lithium ions in the concentrated solution after concentration is 1-30 g/L.
6. The method for preparing battery-grade lithium carbonate from fly ash by using carbonization decomposition method according to claim 1, wherein in the step (3), the carbonate is selected from sodium carbonate or potassium carbonate; the concentration of the carbonate in the step (3) is 5-40% by mass concentration.
7. The method for preparing battery-grade lithium carbonate from fly ash by the carbonization decomposition method according to claim 1, wherein the stirring in the reaction process in the step (3) is performed by a stirrer, and the stirring speed is 200-1200 r/min; after the dropwise addition of the carbonate solution in the step (3) is finished, continuously stirring and reacting for 0.5-10h, and then filtering;
and (3) after filtering the precipitate, washing the precipitate before drying.
8. The method for preparing battery-grade lithium carbonate from fly ash by carbonization decomposition according to claim 1, wherein the primary lithium carbonate product and water in the step (4) are mixed according to a liquid-solid ratio (1-50): 1, mixing;
The flow rate of the carbon dioxide gas in the step (4) is 1-10BV/h, and the reaction time is 1-20 h;
And (4) stirring by using a stirrer at the stirring speed of 200-1200 r/min.
9. The method for preparing battery-grade lithium carbonate from fly ash by using carbonization decomposition method according to claim 1, wherein the reaction time in step (5) is 1-20 h.
10. The method for preparing battery-grade lithium carbonate from fly ash by using carbonization decomposition method according to claim 1, wherein the pulverizing device used in the step (6) is one or more selected from a box-type pulverizer, a jet mill, a super-fine pulverizer, a freezing pulverizer, a low-temperature pulverizer, a turbine pulverizer and a super-fine pulverizer.
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Application publication date: 20191213 |