CN114990357A - Lithium extraction method for high-sulfur high-alkali lepidolite concentrate smelting slag - Google Patents
Lithium extraction method for high-sulfur high-alkali lepidolite concentrate smelting slag Download PDFInfo
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- CN114990357A CN114990357A CN202210740704.7A CN202210740704A CN114990357A CN 114990357 A CN114990357 A CN 114990357A CN 202210740704 A CN202210740704 A CN 202210740704A CN 114990357 A CN114990357 A CN 114990357A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/08—Chloridising roasting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a lithium extraction method of high-sulfur high-alkali lepidolite concentrate smelting slag, which comprises the following steps: fully and uniformly mixing a certain amount of combined medicament with the lithium slag, roasting in a roasting furnace, heating, stirring and leaching by using tap water after roasting is finished, and filtering to obtain a leaching solution and leaching slag after leaching; the leaching solution is lithium-containing solution, and can be used for subsequent lithium extraction process, and the leaching residue can be used as building material. The method for treating the lithium slag is simple, the comprehensive utilization rate of the lithium slag is high, and the method is suitable for industrial application. Specifically, lithium, rubidium and cesium in the lithium slag are leached into the solution through roasting and leaching, so that the content of potassium, sodium and sulfur in the lithium slag is reduced, and the requirement of the lithium slag as a building material is met.
Description
Technical Field
The invention relates to the field of comprehensive utilization of smelting process solid wastes, in particular to comprehensive utilization of lithium slag.
Background
The lepidolite is a main lithium extraction mineral and has great comprehensive utilization value. At present, the process for extracting lithium carbonate from lepidolite is mainly divided into a limestone sintering method, a sulfate roasting method, a pressure boiling method, a chlorination roasting method, a sulfuric acid method and the like. The sulfate roasting method generates a large amount of lepidolite leaching residues after extracting lithium carbonate, the large amount of stacking of the lepidolite leaching residues not only occupies land, but also easily causes environmental pollution, and meanwhile, the lepidolite also contains a small amount of valuable elements such as lithium, rubidium and cesium, and is not recycled, so that resource waste is easily generated. Therefore, a high-efficiency and environment-friendly treatment method with little environmental pollution is urgently needed, the problem of lithium slag piling is solved, and the comprehensive utilization of the lithium slag is realized.
At present, patents on recycling of lithium slag mainly focus on the aspect of preparing cement and concrete by using lithium slag, and part of preparation materials are replaced by the lithium slag to realize recycling of the lithium slag, for example, cement is prepared by using the lithium slag, limestone, iron slag, silica fume and the like in Nanxianxi and the like, and concrete is prepared by using the lithium slag, the cement, an auxiliary cementing material, sandstone and water in plum brightening and the like. However, such a treatment method cannot recover valuable metals in the lithium slag, resulting in resource loss. Some patents can recover valuable metals such as lithium, rubidium, cesium and the like in the lithium slag, but the recovery process is complex, and great danger exists in the process operation. If Zhangxiufeng and the like adopt sulfuric acid solution to leach lithium slag, the sulfuric acid solution with higher concentration is used in the leaching process, the cost is higher, the risk coefficient is larger, and the whole process flow is more complicated.
Disclosure of Invention
The invention aims to provide a building material prepared from lithium slag with high efficiency, environmental protection and high comprehensive utilization rate and a lithium extraction process.
The invention is realized by the following steps:
a method for extracting lithium from high-sulfur high-alkali lepidolite concentrate smelting slag comprises the following steps:
(1) accurately weighing a certain amount of lithium slag and a combined medicament, fully and uniformly mixing the lithium slag and the combined medicament, and roasting.
(2) After the roasted product is cooled, the roasted product is ground into fine particles, and then a certain amount of tap water is added to carry out magnetic stirring leaching.
(3) And filtering after stirring and leaching to obtain filter residue and filtrate.
According to the lithium extraction method, the mass ratio of the lithium slag to the combined medicament is 1: 1.
According to the lithium extraction method, the combined medicament is a mixture of calcium chloride and ammonium chloride.
According to the lithium extraction method, the mass ratio of the combined medicament is 1: 1-1.5.
According to the lithium extraction method, the roasting temperature is 800-900 ℃ in the roasting process, and the roasting time is 1-2 h.
According to the lithium extraction method, the solid-to-liquid ratio of the leaching solution in the leaching process is 10:1-12.5:1, the leaching time is 1-2 h, the leaching temperature is 40-60 ℃, and the magnetic stirring speed is 400 r/min.
According to the lithium extraction method, the content of lithium ions in the leachate is 0.20-0.23 g/L.
The invention has the characteristics that:
aiming at the problems of low utilization rate of lithium slag resources, complex flow, high cost and large safety factors in the prior art, the method has simple steps, only needs simple roasting and leaching, adopts tap water in the leaching process, is safe and environment-friendly, has low cost and is beneficial to industrial production. In this patent, calcium among the calcium chloride can be effectual exchanges out with the lithium in the lithium sediment, turns into the lithium chloride of soluble with the insoluble lithium mineral in the lithium sediment, and the ammonium chloride volatilizees easily when the calcination, causes the loose porosity of lithium sediment, and the calcination reaction is more complete, and the leaching rate is higher.
(1) The method for treating the lithium slag is simple, the comprehensive utilization rate of the lithium slag is high, and the method is suitable for industrial application.
(2) Valuable elements such as lithium, rubidium, cesium and the like are enriched to obtain enrichment liquid, and the enrichment liquid can be used as a raw material of a lithium extraction process to extract lithium carbonate again, so that the aim of resource utilization from lithium slag to a greater extent is fulfilled.
(3) By adopting the treatment method, the content of potassium, sodium, sulfur and other elements in the regenerated lithium slag can be effectively reduced, so that the lithium slag reaches the standard of building raw materials, the hidden danger of land occupation and environmental pollution caused by lithium slag piling is eliminated, the environmental benefit is remarkable, and certain economic benefit can be generated.
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FIG. 1 is a process flow diagram of a lithium extraction process of high-sulfur high-alkali lepidolite concentrate smelting slag according to the present invention;
Detailed Description
The present invention will be described in detail with reference to specific examples.
Accurately weighing a certain amount of lepidolite leaching residues, weighing the combined medicament with the same mass, and roasting after fully and uniformly mixing the lepidolite leaching residues and the combined medicament to obtain a roasted product. Grinding the roasted product into powder, adding water, heating, stirring and leaching in a magnetic stirrer, and filtering to obtain a lithium-containing leaching solution and leaching residues.
The lithium slag in this example is the residue left after lithium carbonate extraction from lepidolite ore in lichun, jiang xi, the chemical composition of the used lithium slag is the same, the main element composition is shown in table 1, the lithium slag in examples 1 and 3 is the lithium slag of li-electricity generation company, nan, in lichun, and the lithium slag in examples 3 and 4 is the lithium slag of fengxuan company, in lichun, nation.
TABLE 1 lithium slag Primary element composition (wt%)
| Lithium slag | Li | Na | K | S | Rb | Cs |
| Examples 1 and 3 | 0.34 | 5.7 | 6.62 | 7.89 | 0.6 | 0.12 |
| Examples 2 and 4 | 0.21 | 3.13 | 3.86 | 8.40 | 0.32 | 0.07 |
Example 1
A method for treating lithium slag comprises the following steps:
1. weighing the lithium slag and the combined medicament with the same mass, wherein the mass ratio of the combined medicament calcium chloride to the ammonium chloride is 1:1, fully and uniformly mixing, and roasting in a roasting furnace at 900 ℃ for 2 hours.
2. Grinding the roasted product to fine particles, and then carrying out stirring leaching in a magnetic stirring water bath kettle for 1 hour at the leaching temperature of 40 ℃, wherein the leaching solution is tap water, the liquid-solid ratio of the tap water to the lithium slag is 10:1, and the stirring speed is 400 r/min.
3. Filtering after leaching to obtain residue and lithium-containing leaching solution.
TABLE 2 Leaching Rate and Leaching residue element content (wt%)
Example 2
A method for treating lithium slag comprises the following steps:
1. weighing the same mass of the lithium slag and the combined medicament, wherein the ratio of the combined medicament calcium chloride to the ammonium chloride is 2:3, fully and uniformly mixing, and roasting in a roasting furnace at 900 ℃ for 2 hours.
2. Grinding the roasted product to fine particles, and then carrying out stirring leaching in a magnetic stirring water bath kettle for 1 hour at the leaching temperature of 40 ℃, wherein the leaching solution is tap water, the liquid-solid ratio of the tap water to the lithium slag is 10:1, and the stirring speed is 400 r/min.
3. Filtering after leaching to obtain residue and lithium-containing leaching solution.
TABLE 3 Leaching residue content (wt%)
Example 3
A method for treating lithium slag comprises the following steps:
1. weighing the same mass of lithium slag and the combined medicament, wherein the ratio of the combined medicament calcium chloride to the combined medicament ammonium chloride is 1:1, fully and uniformly mixing, and roasting in a roasting furnace at 900 ℃ for 2 hours.
2. Grinding the roasted product to fine particles, and then carrying out stirring leaching in a magnetic stirring water bath kettle for 1.5 hours at the leaching temperature of 45 ℃, wherein the leaching solution is tap water, the liquid-solid ratio of the tap water to the lithium slag is 10:1, and the stirring speed is 400 r/min.
3. Filtering after leaching to obtain residue and lithium-containing leaching solution.
TABLE 4 Leaching residue content (wt,%)
Example 4
A method for treating lithium slag comprises the following steps:
1. weighing the same mass of the lithium slag and the combined medicament, wherein the ratio of the combined medicament calcium chloride to the ammonium chloride is 2:3, fully and uniformly mixing, and roasting in a roasting furnace at 850 ℃ for 1 hour.
2. Grinding the roasted product to fine particles, and then stirring and leaching for 1 hour in a magnetic stirring water bath kettle at the leaching temperature of 50 ℃, wherein the leaching solution is tap water, the liquid-solid ratio of the tap water to the lithium slag is 10:1, and the stirring speed is 400 r/min.
3. Filtering after leaching to obtain residue and lithium-containing leaching solution.
TABLE 5 Leaching residue content (wt%)
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (7)
1. A lithium extraction method of high-sulfur high-alkali lepidolite concentrate smelting slag is characterized by comprising the following steps:
(1) accurately weighing a certain amount of lithium slag and a combined medicament, fully and uniformly mixing the lithium slag and the combined medicament, and roasting.
(2) After the roasted product is cooled, the roasted product is ground into fine particles, and then a certain amount of tap water is added to carry out magnetic stirring leaching.
(3) And filtering after stirring and leaching to obtain filter residue and filtrate.
2. The method for extracting lithium from high-sulfur high-alkali lepidolite concentrate smelting slag according to claim 1, wherein the dosage-mass ratio of the lithium slag to the combined medicament is 1: 1.
3. The method for extracting lithium from the smelting slag of the high-sulfur high-alkali lepidolite ore concentrate as claimed in claim 1, wherein the combined agent is a mixture of calcium chloride and ammonium chloride.
4. The method for extracting lithium from the high-sulfur high-alkali lepidolite concentrate smelting slag according to claim 3, wherein the mass ratio of the combined medicament is 1: 1-1.5.
5. The method for extracting lithium from the high-sulfur high-alkali lepidolite concentrate smelting slag according to claim 1, wherein the roasting temperature is 800-900 ℃ and the roasting time is 1-2 h in the roasting process.
6. The method for extracting lithium from high-sulfur and high-alkali lepidolite concentrate smelting slag according to claim 1, wherein the solid-to-liquid ratio of a leaching solution in the leaching process is 10:1-12.5:1, the leaching time is 1h-2h, the leaching temperature is 40-60 ℃, and the magnetic stirring speed is 400 r/min.
7. The method for extracting lithium from the smelting slag of the high-sulfur and high-alkali lepidolite ore concentrate according to claim 1, wherein the content of lithium ions in the leaching solution is 0.20 to 0.23 g/L.
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| CN202210740704.7A CN114990357A (en) | 2022-06-27 | 2022-06-27 | Lithium extraction method for high-sulfur high-alkali lepidolite concentrate smelting slag |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365180A (en) * | 2016-08-29 | 2017-02-01 | 西南化工研究设计院有限公司 | Technology for extracting high-purity lithium chloride from lithium ore |
| CN108118143A (en) * | 2017-12-27 | 2018-06-05 | 中南大学 | Two sections of chloridising roastings-alkaline leaching method puies forward the method that lithium prepares lithium carbonate from lepidolite |
| JP2020066795A (en) * | 2018-10-26 | 2020-04-30 | 住友金属鉱山株式会社 | Method for leaching lithium and method for recovering lithium |
| CN112357936A (en) * | 2020-11-12 | 2021-02-12 | 萍乡市拓源实业有限公司 | Roasting process of non-mainstream lithium ore |
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- 2022-06-27 CN CN202210740704.7A patent/CN114990357A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365180A (en) * | 2016-08-29 | 2017-02-01 | 西南化工研究设计院有限公司 | Technology for extracting high-purity lithium chloride from lithium ore |
| CN108118143A (en) * | 2017-12-27 | 2018-06-05 | 中南大学 | Two sections of chloridising roastings-alkaline leaching method puies forward the method that lithium prepares lithium carbonate from lepidolite |
| JP2020066795A (en) * | 2018-10-26 | 2020-04-30 | 住友金属鉱山株式会社 | Method for leaching lithium and method for recovering lithium |
| CN112357936A (en) * | 2020-11-12 | 2021-02-12 | 萍乡市拓源实业有限公司 | Roasting process of non-mainstream lithium ore |
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