CN110592383A - Method for extracting lithium from fly ash by adsorption method - Google Patents
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- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
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- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
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- C22B26/12—Obtaining lithium
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Abstract
The invention belongs to the technical field of rare and noble metal extraction, and particularly relates to a method for extracting lithium from fly ash by an adsorption method. The implementation of the method is based on a fly ash reinforced desilication-mild alkali method aluminum lithium gallium synergistic extraction process, mainly comprises a lithium extraction method of lithium-containing solution fine filtration purification, adsorption and desorption, so that the separation and extraction of lithium in the fly ash are realized, the obtained product liquid can be directly used for a subsequent refining impurity removal process of a lithium carbonate product, the comprehensive utilization of the fly ash is realized, and the economic benefit is improved.
Description
Technical Field
The invention relates to a method for extracting lithium from fly ash, in particular to a method for extracting lithium from fly ash by an adsorption method.
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 is a big coal-producing country and takes coal as basic fuel for power production. According to statistics, the thermal power yield reaches 44371 hundred million kilowatt hours in 2016 years in China, and accounts for 72.24 percent of the total production. With the rapid development of the electric power industry in China, the discharge amount of the fly ash is increased rapidly. The fly ash is a potential 'urban mineral' resource, the chemical composition of the fly ash is relatively complex, and the main substances comprise SiO2, A12O3, Fe2O3, CaO, MgO, K2O, Na2O, P2O5, TiO2, MnO2, SO3 and the like, wherein the mass fraction of SiO2 is about 35.6-57.2%, and the mass fraction of A12O3 is about 18.8-55.0%, and the fly ash 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 comprehensive utilization level of the fly ash can be improved by extracting and utilizing other rare metals while preparing the aluminum-silicon products.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a method for extracting lithium from fly ash, which is suitable for a strong alkaline environment and has a simple process.
The technical scheme of the invention is that a method for extracting lithium from fly ash by an adsorption method comprises the following steps:
(1) fine filtering and purifying lithium-containing solution: finely filtering a lithium-containing solution in the fly ash aluminum extraction process to obtain a purified solution;
(2) adsorption: mixing a lithium ion adsorbent with the purified liquid obtained in the step (1) to adsorb lithium ions, wherein the adsorption temperature is 10-80 ℃, and the using amount of the purified liquid is 1-30 BV;
(3) desorbing: and (3) desorbing the adsorbent subjected to lithium ion adsorption in the step (2) by using desorption liquid to obtain desorption liquid, wherein the desorption temperature is 10-80 ℃, and the consumption of the desorption agent is 1-30 BV.
BV refers to the multiple of the total volume of the adsorbent.
According to the method for extracting lithium from fly ash by using the adsorption method, preferably, in the step (1), the lithium-containing solution in the fly ash aluminum extraction process comprises a pre-desiliconization solution, a circulating solution, a crude solution, a seed precipitation mother solution, a carbon distillation mother solution and a carbon distillation raw solution.
According to the method for extracting lithium from fly ash by using the adsorption method, preferably, the fly ash aluminum extraction process refers to a fly ash reinforced desiliconization-mild alkaline method aluminum lithium gallium synergistic extraction process.
Preferably, the fine filtration in the step (1) adopts a fine filtration filter or liquid filtration equipment; the content of suspended substances in the purifying liquid is lower than 0.01 g/L.
In the method for extracting lithium from fly ash by the adsorption method according to the present invention, in the step (2), the lithium ion adsorbent is preferably one or more selected from a manganese ion sieve, a titanium ion sieve, a niobium ion sieve, a zirconium ion sieve, an aluminum salt adsorbent, a nickel adsorbent resin, and a chelate resin.
According to the method for extracting lithium from fly ash by the adsorption method, the purifying liquid passes through an adsorption column loaded with an adsorbent at a flow rate of 1-10BV/h during adsorption in the step (2). The flow rate is higher than 1BV/h, the retention time is prolonged due to too low flow rate, the adsorption column is easy to be blocked by the adsorption liquid containing aluminum silicon, and the efficiency is reduced. The flow rate is lower than 10BV/h, and the impact force on the adsorbent due to overhigh flow rate can cause the unstable bed layer structure and easily damage the adsorbent.
More preferably, the flow rate of the purified liquid during the adsorption is 2-3 BV/h.
According to the method for extracting lithium from fly ash by the adsorption method, the desorbent in the step (3) is preferably one or more of water, a lithium chloride solution, diluted hydrochloric acid or diluted sulfuric acid.
Corresponding desorbents are required for different adsorbents in the method, and the desorbents are subjected to desorption processes through ion exchange or concentration gradient.
According to the method for extracting lithium from the fly ash by the adsorption method, the desorbent passes through a desorption column loaded with the adsorbent subjected to lithium ion adsorption at a flow rate of 1-10BV/h during desorption in the step (3). The flow rate is higher than 1BV/h, the flow rate is reduced, the desorption time is doubled, and the cost is increased. The flow rate is lower than 10BV/h, the retention time is short when the flow rate is too high, the ion exchange is insufficient, the efficiency is reduced, and the impact force of the high flow rate on the adsorbent is too large, so that the bed layer structure is unstable and the adsorbent is easy to damage.
More preferably, the flow rate of the desorbent during desorption is 2-3 BV/h.
According to the method for extracting lithium from fly ash by the adsorption method, the adsorption temperature in the step (2) is preferably 20-60 ℃, and the using amount of the purifying liquid is preferably 5-20 BV.
According to the method for extracting lithium from fly ash by the adsorption method, the desorption temperature in the step (3) is preferably 20-60 ℃, and the dosage of the desorbent is 5-20 BV.
According to the method for extracting lithium from fly ash by adsorption method of the invention, preferably, after the step (2) uses the adsorbent to perform lithium ion adsorption reaction with the purified liquid of the step (1), residual adsorption raffinate which is not completely adsorbed is used as silicon-containing solution for producing silicon-containing material.
The invention has the beneficial effects that:
the method is suitable for a strong alkaline environment, has the advantages of saving the regeneration process of the adsorbent, being simple in process, mild in condition, low in energy consumption, low in equipment requirement and low in price, effectively realizing the recycling of lithium in the fly ash, simultaneously ensuring the subsequent effective utilization of fly ash residues and adsorption residual liquid generated in the process, realizing the zero discharge of waste in the whole process flow, and having good industrial application prospect.
Drawings
FIG. 1 is a schematic view of a process flow of a method for extracting lithium from fly ash by an adsorption method according to the present invention;
FIG. 2 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. 3 is a graph showing the effect of purge flow rate on the adsorption process;
figure 4 is a plot of the effect of desorbent flow rate on desorption process.
Detailed Description
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 the various sections
Example 1:
(1) fine filtering the pre-desiliconized solution to obtain a purified solution;
(2) enabling the purified liquid to pass through an adsorption column loaded with an aluminum salt adsorbent at the flow rate of 5BV/h for lithium ion adsorption, wherein the adsorption temperature is 60 ℃, and the using amount of the purified liquid is 5 BV;
(3) 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.
And (3) after the adsorbent in the step (2) and the purified liquid in the step (1) are subjected to lithium ion adsorption reaction, residual adsorption raffinate which is not completely adsorbed is remained, and the adsorption raffinate can be used as a silicon-containing solution for producing white carbon black and a calcium silicate silicon-containing material, so that zero waste emission of the whole process flow is realized.
Example 2:
(1) fine filtering the circulating liquid to obtain a purified liquid;
(2) enabling the purifying solution 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 solution is 20 BV;
(3) 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.
And (3) after the adsorbent in the step (2) and the purified liquid in the step (1) are subjected to lithium ion adsorption reaction, residual adsorption raffinate which is not completely adsorbed is remained, and the adsorption raffinate can be used as a silicon-containing solution for producing white carbon black and a calcium silicate silicon-containing material, so that zero waste emission of the whole process flow is realized.
Example 3:
(1) finely filtering the carbon evaporation mother liquor to obtain a purified solution;
(2) the purifying liquid passes through an adsorption column loaded with chelating resin at the flow rate of 5BV/h to carry out lithium ion adsorption, mainly using weak acid type macroporous cation exchange resin chelated with diacetoxyl imino, wherein the adsorption temperature is 40 ℃, and the using amount of the purifying liquid is 5 BV;
(3) 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.
And (3) after the adsorbent in the step (2) and the purified liquid in the step (1) are subjected to lithium ion adsorption reaction, residual adsorption raffinate which is not completely adsorbed is remained, and the adsorption raffinate can be used as a silicon-containing solution for producing white carbon black and a calcium silicate silicon-containing material, so that zero waste emission of the whole process flow is realized.
Example 4:
(1) finely filtering the carbon evaporation stock solution to obtain a purified solution;
(2) the purifying liquid passes through an adsorption column loaded with chelating resin at the flow rate of 1BV/h to carry out lithium ion adsorption, mainly using weak acid type macroporous cation exchange resin chelated with diacetoxyl imino, wherein the adsorption temperature is 20 ℃, and the using amount of the purifying liquid is 6 BV;
(3) 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.
And (3) after the adsorbent in the step (2) and the purified liquid in the step (1) are subjected to lithium ion adsorption reaction, residual adsorption raffinate which is not completely adsorbed is remained, and the adsorption raffinate can be used as a silicon-containing solution for producing white carbon black and a calcium silicate silicon-containing material, so that zero waste emission of the whole process flow is realized.
Example 5:
(1) fine filtering the pre-desiliconized solution to obtain a purified solution;
(2) the purifying liquid sequentially passes through an adsorption column loaded with a manganese ion sieve and a titanium ion sieve at the flow rate of 2BV/h to carry out lithium ion adsorption, the adsorption temperature is 20 ℃, and the using amount of the purifying liquid is 5 BV;
(3) and (3) eluting the adsorbent subjected to lithium ion adsorption by using water, wherein the flow rate of the water during elution is 2BV/h, the elution temperature is 20 ℃, and the using amount of the water is 5 BV. After elution is finished, dilute sulfuric acid with the concentration of 1moL/L is used for desorption, the flow rate during desorption is 2BV/h, the desorption temperature is 20 ℃, the consumption of the resolving agent is 5BV, and desorption liquid is obtained by mixing.
And (3) after the adsorbent in the step (2) and the purified liquid in the step (1) are subjected to lithium ion adsorption reaction, residual adsorption raffinate which is not completely adsorbed is remained, and the adsorption raffinate can be used as a silicon-containing solution for producing white carbon black and a calcium silicate silicon-containing material, so that zero waste emission of the whole process flow is realized.
Example 6:
(1) finely filtering the carbon evaporation stock solution to obtain a purified solution;
(2) the purifying liquid passes through an adsorption column loaded with a zirconium ion sieve at the flow rate of 1BV/h to carry out lithium ion adsorption, the adsorption temperature is 20 ℃, and the using amount of the purifying liquid is 3 BV;
(3) desorbing the adsorbent subjected to lithium ion adsorption by using dilute sulfuric acid with the concentration of 1moL/L, wherein the flow rate of the sulfuric acid is 2BV/h, the desorption temperature is 20 ℃, and the using amount of the desorbent is 2BV, so as to obtain desorption liquid.
And (3) after the adsorbent in the step (2) and the purified liquid in the step (1) are subjected to lithium ion adsorption reaction, residual adsorption raffinate which is not completely adsorbed is remained, and the adsorption raffinate can be used as a silicon-containing solution for producing white carbon black and a calcium silicate silicon-containing material, so that zero waste emission of the whole process flow is realized.
Example 7:
(1) finely filtering the carbon evaporation mother liquor to obtain a purified solution;
(2) the purifying liquid passes through an adsorption column loaded with a niobium ion sieve at the flow rate of 1BV/h to carry out lithium ion adsorption, the adsorption temperature is 20 ℃, and the using amount of the purifying liquid is 3 BV;
(3) 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.
And (3) after the adsorbent in the step (2) and the purified liquid in the step (1) are subjected to lithium ion adsorption reaction, residual adsorption raffinate which is not completely adsorbed is remained, and the adsorption raffinate can be used as a silicon-containing solution for producing white carbon black and a calcium silicate silicon-containing material, so that zero waste emission of the whole process flow is realized.
TABLE 2 stripping liquid composition in each example
The extraction rate of lithium is greatly influenced by the nature of the solution. The lithium extraction ratio of the solutions of each section is shown in table 3.
TABLE 3 extraction ratio of lithium from solutions of each section
The method provided by the invention is mainly used for extracting lithium in the fly ash reinforced desilication-mild alkaline process aluminum lithium gallium synergistic extraction process, and is suitable for a strong alkaline environment. The method has the advantages of omitting the regeneration process of the adsorbent, simplifying the steps and reducing the cost.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A method for extracting lithium from fly ash by an adsorption method is characterized by comprising the following steps: the method comprises the following steps:
(1) fine filtering and purifying lithium-containing solution: finely filtering a lithium-containing solution in the fly ash aluminum extraction process to obtain a purified solution;
(2) adsorption: mixing a lithium ion adsorbent with the purified liquid obtained in the step (1) to adsorb lithium ions, wherein the adsorption temperature is 10-80 ℃, and the using amount of the purified liquid is 1-30 BV;
(3) desorbing: and (3) desorbing the adsorbent subjected to lithium ion adsorption in the step (2) by using desorption liquid to obtain desorption liquid, wherein the desorption temperature is 10-80 ℃, and the consumption of the desorption agent is 1-30 BV.
2. The method for extracting lithium from fly ash by adsorption according to claim 1, wherein in the step (1), the lithium-containing solution in the fly ash aluminum extraction process comprises a pre-desilication solution, a recycle solution, a crude solution, a seed precipitation mother solution, a carbon distillation mother solution and a carbon distillation raw solution.
3. The method for extracting lithium from fly ash by using the adsorption method according to claim 1, wherein the fly ash aluminum extraction process is a fly ash reinforced desilication-mild alkaline process aluminum lithium gallium synergistic extraction process.
4. The method for extracting lithium from fly ash by adsorption according to claim 1, wherein the fine filtration in step (1) is performed by using a fine filtration filter or a liquid filtration device; the content of suspended substances in the purifying liquid is lower than 0.01 g/L.
5. The method according to claim 1, wherein in the step (2), the lithium ion adsorbent is one or more selected from a manganese ion sieve, a titanium ion sieve, a niobium ion sieve, a zirconium ion sieve, an aluminum salt adsorbent, a nickel adsorbent resin, and a chelate resin.
6. The method for extracting lithium from fly ash by adsorption according to claim 1, wherein the purifying liquid passes through the adsorption column loaded with the adsorbent at a flow rate of 1-10BV/h during adsorption in the step (2).
7. The method for extracting lithium from fly ash by adsorption according to claim 1, wherein the desorbent in step (3) is one or more of water, lithium chloride solution, dilute hydrochloric acid or dilute sulfuric acid.
8. The method for extracting lithium from fly ash by adsorption according to claim 1, wherein the desorbent in the desorption in the step (3) passes through a desorption column loaded with the adsorbent which has been subjected to lithium ion adsorption at a flow rate of 1-10 BV/h.
9. The method for extracting lithium from fly ash by adsorption according to claim 1, wherein the adsorption temperature in the step (2) is 20-60 ℃, and the using amount of the purifying solution is 5-20 BV; the desorption temperature in the step (3) is 20-60 ℃, and the dosage of the desorbent is 5-20 BV.
10. The method for extracting lithium from fly ash by adsorption according to claim 1, wherein after the step (2) of performing lithium ion adsorption reaction on the adsorbent and the purified liquid obtained in the step (1), residual adsorption raffinate which is not completely adsorbed is used as a silicon-containing solution for producing a silicon-containing material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113333036A (en) * | 2021-05-26 | 2021-09-03 | 华东理工大学 | Preparation method and application of niobium modified hydrophobic acidic cation exchange resin |
| CN114540636A (en) * | 2022-02-24 | 2022-05-27 | 北京工业大学 | Method for recovering metal elements from metal-containing fluid |
| CN115029564A (en) * | 2022-08-12 | 2022-09-09 | 矿冶科技集团有限公司 | Co-production process for extracting lithium from salt lake brine and preparing acid from sulfur-containing material and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107758714A (en) * | 2016-08-17 | 2018-03-06 | 中国科学院过程工程研究所 | A kind of method of aluminium silicon lithium gallium combination method collaboration extraction in flyash |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107758714A (en) * | 2016-08-17 | 2018-03-06 | 中国科学院过程工程研究所 | A kind of method of aluminium silicon lithium gallium combination method collaboration extraction in flyash |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113333036A (en) * | 2021-05-26 | 2021-09-03 | 华东理工大学 | Preparation method and application of niobium modified hydrophobic acidic cation exchange resin |
| CN114540636A (en) * | 2022-02-24 | 2022-05-27 | 北京工业大学 | Method for recovering metal elements from metal-containing fluid |
| CN114540636B (en) * | 2022-02-24 | 2024-05-28 | 北京工业大学 | Method for recovering metal elements from metal-containing fluid |
| CN115029564A (en) * | 2022-08-12 | 2022-09-09 | 矿冶科技集团有限公司 | Co-production process for extracting lithium from salt lake brine and preparing acid from sulfur-containing material and application |
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Application publication date: 20191220 |