CN113174480A - Method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals - Google Patents
Method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals Download PDFInfo
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- CN113174480A CN113174480A CN202110359501.9A CN202110359501A CN113174480A CN 113174480 A CN113174480 A CN 113174480A CN 202110359501 A CN202110359501 A CN 202110359501A CN 113174480 A CN113174480 A CN 113174480A
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
- C22B3/14—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals, and belongs to the technical field of metallurgy. The method comprises the steps of firstly, uniformly mixing finely ground silicate mineral powder containing lithium, rubidium and cesium with calcium chloride and a chlorine fixing agent according to a certain proportion, then roasting the mixed material at high temperature, finally leaching the obtained roasted product, obtaining lithium salt from a leaching solution through a chemical precipitation method, and obtaining rubidium salt and cesium salt from the solution after lithium precipitation through an extraction/back extraction method. The method has the advantages of strong adaptability to raw materials, short flow, few working procedures and high extraction rate of rubidium and cesium, the utilization rate of calcium chloride is increased by adding the chlorine fixing agent, compared with the traditional chlorination roasting method, the use of chloride is greatly reduced, no chlorine tail gas is generated in the roasting process after the chlorine fixing agent is added, the problem that flue gas contains chlorine in the traditional chlorination roasting is solved, and green and clean production is realized.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals.
Background
Lithium, rubidium and cesium are all silvery white and soft alkali metals, and the application is very wide. Lithium is a metal element having the smallest atomic diameter and the lowest density, and is widely used in the fields of batteries, heat-resistant glass, lubricants, refrigerants, nuclear industry, and the like. Rubidium and cesium have excellent photoelectric effect performance, and are widely used in the fields of photomultiplier tubes, atomic clocks, photocells, infrared technology, nuclear medicine and the like. For a long time, rubidium has been mostly extracted from lepidolite, and a considerable part of rubidium is also obtained from pollucite, and besides, is rarely obtained from other minerals. China has abundant lepidolite reserves, and researchers carry out a great deal of related research to effectively develop and utilize lepidolite ores, so that a lot of precious experiences are obtained.
Currently, the development of lepidolite mainly includes the following methods:
(1) the sulfuric acid method is that sulfuric acid is used to make lepidolite undergo the process of long-time moderate-temperature curing decomposition, and then leached so as to obtain the solution containing lithium, rubidium and cesium.
Zhang Xiufeng et al (sulfuric acid aging research of lepidolite concentrate, 04 in 2018, mineral protection and utilization) have leaching rates of lithium, rubidium and cesium respectively reaching 97.6%, 96.7% and 97.4% under the conditions of acid-mineral ratio of 1:1, sulfuric acid mass concentration of 80%, aging time of 4h and aging temperature of 150 ℃. The method has the advantages of simple process flow, high leaching rate, low raw material cost, no need of high temperature and low energy consumption, but because aluminum is almost completely leached in the leaching process, a large amount of lithium is lost in the subsequent impurity removal process.
(2) The sulfate roasting method is that lepidolite is mixed with sulfate such as sodium sulfate, potassium sulfate and the like, then the mixture is roasted at high temperature, and then leached to obtain solution containing lithium, rubidium and cesium.
Pigment group xuan (high-efficiency extraction research of valuable metals in lepidolite, 2012, database of doctor thesis in chinese) in lepidolite: sodium sulfate: potassium sulfate: the mass ratio of calcium oxide is 1:0.5:0.1:0.1, the leaching rates of lithium, rubidium and cesium respectively reach 91.6%, 29.3% and 23.2% under the conditions that the roasting temperature is 900 ℃ and the roasting time is 30 min. The method is characterized in that the aluminum in the minerals cannot be leached, so that the loss of lithium is reduced; however, the method has the defects of large reagent consumption and low rubidium and cesium leaching rate.
(3) The chloridizing roasting method is that the lepidolite is mixed with calcium chloride and sodium chloride and then roasted at high temperature, and then leached to obtain the solution containing lithium, rubidium and cesium.
Pigment group xuan (high-efficiency extraction research of valuable metals in lepidolite, 2012, database of doctor thesis in chinese) in lepidolite: calcium chloride: the mass ratio of sodium chloride is 1:0.6:0.4, the leaching rates of lithium, rubidium and cesium respectively reach 92.9%, 94.1% and 93.1% under the conditions that the roasting temperature is 880 ℃ and the time is 30 min. The method has the advantages that the comprehensive utilization rate is good, the recovery rates of lithium, rubidium and cesium are high, and fluorine in the raw ore is fixed in slag in the form of calcium fluoride; however, the use of a large amount of chloride causes a large amount of chlorine gas and hydrogen chloride gas in the roasting process, so that the equipment is seriously corroded, and the environmental pollution is very easily caused.
Therefore, the development of a method for efficiently, cleanly and economically extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals has important significance for promoting the development of lithium, rubidium and cesium non-ferrous metal industries in China.
Disclosure of Invention
Aiming at the defects and shortcomings of the extraction process of lithium, rubidium and cesium in the prior art, the invention provides a method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals. The process method disclosed by the invention is efficient and environment-friendly, has high extraction rate of lithium, rubidium and cesium, and provides important reference significance for development and utilization of lithium, rubidium and cesium-containing minerals in China.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals comprises the following steps:
(1) finely grinding lithium-containing, rubidium-containing and cesium-containing silicate minerals to obtain mineral powder;
(2) uniformly mixing the mineral powder with calcium chloride and a chlorine fixing agent according to a certain proportion to obtain a mixed material; the chlorine fixing agent comprises one or more of calcium oxide, calcium hydroxide, calcium carbonate, magnesium oxide, magnesium hydroxide and magnesium carbonate;
(3) roasting the mixed material at high temperature to obtain roasted sand;
(4) adding a leaching agent into the calcine to carry out leaching reaction, and carrying out solid-liquid separation after the leaching reaction is finished to obtain a leaching solution containing lithium, rubidium and cesium;
(5) and adding a lithium precipitator into the leachate to precipitate lithium in the solution, and extracting the solution after lithium precipitation by an extraction-back extraction method to obtain rubidium salt and cesium salt.
Further, the lithium, rubidium and cesium silicate minerals in the step (1) comprise one or more of lepidolite, spodumene, pollucite, rubidium mica, plagioclase feldspar, muscovite and biotite.
Further, the particle size of the ore powder in the step (1) is smaller than 100 meshes (<0.15 mm).
Further, the calcium chloride in the step (2) comprises one or more of anhydrous calcium chloride, calcium chloride dihydrate and calcium chloride hexahydrate.
Further, in the step (2), the mass ratio of the calcium chloride to the mineral powder is 0.1:1-0.5:1, and the mass ratio of the chlorine fixing agent to the mineral powder is 0.1:1-0.5: 1.
Further, the temperature of the high-temperature roasting in the step (3) is 600-.
Further, the leaching agent in the step (4) comprises water or alkali liquor, the alkali liquor comprises one or more of ammonia water, hydroxide aqueous solution and carbonate aqueous solution, and the alkali concentration is 10-100 g/L.
Further, the liquid-solid ratio of the leaching reaction in the step (4) is 1.5:1-10:1, the leaching temperature is 20-100 ℃, and the leaching time is 0.5-3 h.
Further, the lithium precipitator in the step (5) comprises one or more of sodium carbonate, carbon dioxide, phosphoric acid and sodium phosphate, and the lithium precipitation reaction temperature is 50-100 ℃ and the time is 0.5-3 h.
Further, the extractant used in the extraction-stripping method in the step (5) is 4-tert-butyl-2- (. alpha. -methylbenzyl) phenol (t-BAMBP), and the stripping agent is one of sulfuric acid, hydrochloric acid, nitric acid, oxalic acid and carbon dioxide.
The beneficial effects of the above technical scheme are as follows:
the method has the advantages of strong adaptability to raw materials, short flow, few working procedures and high extraction rate of rubidium and cesium, the utilization rate of calcium chloride is increased by adding the chlorine fixing agent, compared with the traditional chlorination roasting method, the use of chloride is greatly reduced, no chlorine tail gas is generated in the roasting process after the chlorine fixing agent is added through the detection of moist starch-potassium iodide test paper and the analysis of the roasted tail gas absorption liquid, the total chlorine content in the absorption liquid is reduced by about 99.8 percent, the generation of hydrogen chloride tail gas in the roasting process is greatly reduced, the problem that the flue gas contains chlorine in the traditional chlorination roasting process is solved, and green clean production is realized.
Drawings
FIG. 1 is a process flow diagram of the method for extracting lithium, rubidium and cesium according to the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention discloses a method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals, and a process flow chart is shown in figure 1. The method specifically comprises the steps of grinding, high-temperature roasting, leaching, lithium precipitation, extraction/back extraction and the like, and is described below by combining specific embodiments.
Example 1
The lepidolite mineral is finely ground to be below 100 meshes through a sampling machine, 100g of mineral powder is weighed and evenly mixed with calcium chloride and a chlorine fixing agent, wherein the adding amount of the calcium chloride is 20g, the adding amount of the calcium oxide is 20g, and the reaction is carried out for 1h at the temperature of 900 ℃. The flue gas in the roasting process is tested by starch-potassium iodide test paper, and no chlorine gas is generated; after absorption by two-stage alkali liquor, the content of chloride ions in the absorption liquid is extremely low, and the chloride ions are generated by decomposing the added amount of 0.1 percent of calcium chloride. Leaching the roasted product after high-temperature roasting for 1 hour at room temperature by using 200mL of water, and then obtaining leachate containing lithium, rubidium and cesium through solid-liquid separation. The leaching rates of lithium, rubidium and cesium in the leaching process respectively reach 85.8%, 95.4% and 97.3%. And adjusting the alkalinity of the lithium-containing solution, and then adding sodium carbonate to perform a precipitation reaction to obtain lithium carbonate. And extracting/back-extracting the solution after lithium precipitation by using an extracting agent (t-BAMBP) and hydrochloric acid to obtain rubidium chloride and cesium chloride.
The components of the leaching solution are as follows:
example 2
The lepidolite mineral is finely ground to be below 100 meshes through a sampling machine, 100g of mineral powder is uniformly mixed with calcium chloride and a chlorine fixing agent, wherein the addition amount of calcium chloride dihydrate is 30g, the addition amount of calcium carbonate is 40g, and the reaction is carried out for 0.5h at the temperature of 800 ℃. The flue gas in the roasting process is tested by starch-potassium iodide test paper, and no chlorine gas is generated; after absorption by two-stage alkali liquor, the content of chloride ions in the absorption liquid is extremely low, and the chloride ions are generated by decomposing the added amount of calcium chloride dihydrate of 0.12 percent. The roasted product after high-temperature roasting is leached for 2 hours at 60 ℃ by 300mL of a 40g/L sodium hydroxide solution, and then a leachate containing lithium, rubidium and cesium is obtained by solid-liquid separation. The leaching rates of lithium, rubidium and cesium in the leaching process reach 87.8%, 96.1% and 95.4% respectively. And adjusting the alkalinity of the lithium-containing solution, and then adding sodium phosphate to perform precipitation reaction to obtain lithium phosphate. And extracting/back-extracting the solution after lithium precipitation by using an extracting agent (t-BAMBP) and sulfuric acid to obtain rubidium sulfate and cesium sulfate.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium-containing silicate minerals is characterized by comprising the following steps:
(1) finely grinding lithium-containing, rubidium-containing and cesium-containing silicate minerals to obtain mineral powder;
(2) uniformly mixing the mineral powder with calcium chloride and a chlorine fixing agent according to a certain proportion to obtain a mixed material; the chlorine fixing agent comprises one or more of calcium oxide, calcium hydroxide, calcium carbonate, magnesium oxide, magnesium hydroxide and magnesium carbonate;
(3) roasting the mixed material at high temperature to obtain roasted sand;
(4) adding a leaching agent into the calcine to carry out leaching reaction, and carrying out solid-liquid separation after the leaching reaction is finished to obtain a leaching solution containing lithium, rubidium and cesium;
(5) and adding a lithium precipitator into the leachate to precipitate lithium in the solution, and extracting the solution after lithium precipitation by an extraction-back extraction method to obtain rubidium salt and cesium salt.
2. The method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium silicate-containing minerals according to claim 1, wherein the lithium, rubidium and cesium silicate-containing minerals in the step (1) comprise one or more of lepidolite, spodumene, pollucite, rubidium mica, plagioclase, muscovite and biotite.
3. The method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium silicate minerals according to claim 1, wherein the particle size of the ore powder in step (1) is smaller than 100 meshes.
4. The method of claim 1, wherein the calcium chloride in step (2) comprises one or more of anhydrous calcium chloride, calcium chloride dihydrate and calcium chloride hexahydrate.
5. The method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium silicate minerals according to claim 1, wherein the mass ratio of the calcium chloride to the mineral powder in step (2) is 0.1:1-0.5:1, and the mass ratio of the chlorine fixing agent to the mineral powder is 0.1:1-0.5: 1.
6. The method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium silicate-containing minerals as claimed in claim 1, wherein the temperature of the high-temperature roasting in step (3) is 600-1000 ℃ and the time is 10-60 min.
7. The method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium silicate minerals according to claim 1, wherein the leaching agent in the step (4) comprises water or alkali liquor, wherein the alkali liquor comprises one or more of ammonia water, hydroxide aqueous solution and carbonate aqueous solution, and the alkali concentration is 10-100 g/L.
8. The method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium silicate minerals according to claim 1, wherein the liquid-solid ratio of leaching reaction in the step (4) is 1.5:1-10:1, the leaching temperature is 20-100 ℃, and the leaching time is 0.5-3 h.
9. The method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium silicate-containing minerals according to claim 1, wherein the lithium precipitating agent in the step (5) comprises one or more of sodium carbonate, carbon dioxide, phosphoric acid and sodium phosphate, and the lithium precipitating reaction is carried out at a temperature of 50-100 ℃ for 0.5-3 h.
10. The method for extracting lithium, rubidium and cesium from lithium, rubidium and cesium silicate minerals as claimed in claim 1, wherein the extractant used in the extraction-stripping process in step (5) is 4-tert-butyl-2- (alpha-methylbenzyl) phenol, and the stripping agent is one of sulfuric acid, hydrochloric acid, nitric acid, oxalic acid and carbon dioxide.
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Cited By (7)
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| CN114105171A (en) * | 2021-11-04 | 2022-03-01 | 四川顺应动力电池材料有限公司 | Method for recycling and comprehensively utilizing lepidolite and lithium hydroxide prepared by method |
| CN114318008A (en) * | 2021-12-27 | 2022-04-12 | 四川顺应锂材料科技有限公司 | Method for extracting lithium by secondary reverse leaching of spodumene with nitric acid |
| CN115198110A (en) * | 2022-07-07 | 2022-10-18 | 有研资源环境技术研究院(北京)有限公司 | Method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate |
| CN115466854A (en) * | 2022-10-13 | 2022-12-13 | 江西闪凝科技有限公司 | Comprehensive extraction method for lithium ore |
| CN115491520A (en) * | 2022-02-09 | 2022-12-20 | 江西东鹏新材料有限责任公司 | Separation and extraction process for dilute alkali metal |
| CN115522070A (en) * | 2022-09-26 | 2022-12-27 | 北京科技大学 | Method for selectively extracting lithium from lithium aluminosilicate minerals |
| WO2024074162A1 (en) * | 2022-10-04 | 2024-04-11 | Geomet S.R.O. | Method and system for treatment of lithiferous ore |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114105171A (en) * | 2021-11-04 | 2022-03-01 | 四川顺应动力电池材料有限公司 | Method for recycling and comprehensively utilizing lepidolite and lithium hydroxide prepared by method |
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| CN115198110A (en) * | 2022-07-07 | 2022-10-18 | 有研资源环境技术研究院(北京)有限公司 | Method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate |
| CN115522070A (en) * | 2022-09-26 | 2022-12-27 | 北京科技大学 | Method for selectively extracting lithium from lithium aluminosilicate minerals |
| WO2024074162A1 (en) * | 2022-10-04 | 2024-04-11 | Geomet S.R.O. | Method and system for treatment of lithiferous ore |
| CN115466854A (en) * | 2022-10-13 | 2022-12-13 | 江西闪凝科技有限公司 | Comprehensive extraction method for lithium ore |
| CN115466854B (en) * | 2022-10-13 | 2024-01-16 | 江西闪凝科技有限公司 | Comprehensive extraction method of lithium ore |
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