CN115198110A - Method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate - Google Patents
Method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate Download PDFInfo
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- CN115198110A CN115198110A CN202210793349.XA CN202210793349A CN115198110A CN 115198110 A CN115198110 A CN 115198110A CN 202210793349 A CN202210793349 A CN 202210793349A CN 115198110 A CN115198110 A CN 115198110A
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 153
- 229910052701 rubidium Inorganic materials 0.000 title claims abstract description 95
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910052792 caesium Inorganic materials 0.000 title claims abstract description 93
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000012141 concentrate Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000002386 leaching Methods 0.000 claims abstract description 57
- 239000000654 additive Substances 0.000 claims abstract description 39
- 230000000996 additive effect Effects 0.000 claims abstract description 29
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 230000004927 fusion Effects 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000004576 sand Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 66
- 239000000292 calcium oxide Substances 0.000 claims description 28
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 4
- 229910052629 lepidolite Inorganic materials 0.000 description 18
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 12
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 8
- 229910052642 spodumene Inorganic materials 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000002195 synergetic effect Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 229910018516 Al—O Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 2
- QSNQXZYQEIKDPU-UHFFFAOYSA-N [Li].[Fe] Chemical compound [Li].[Fe] QSNQXZYQEIKDPU-UHFFFAOYSA-N 0.000 description 2
- BHKCBKMUUHAIAX-UHFFFAOYSA-N [Rb].[Cs].[Li] Chemical compound [Rb].[Cs].[Li] BHKCBKMUUHAIAX-UHFFFAOYSA-N 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- JJFHSTASBVENMB-UHFFFAOYSA-N [Li].[Cs] Chemical compound [Li].[Cs] JJFHSTASBVENMB-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KOPBYBDAPCDYFK-UHFFFAOYSA-N caesium oxide Chemical compound [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- 229910001942 caesium oxide Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- DJMZKFUAQIEDKC-UHFFFAOYSA-N lithium rubidium Chemical compound [Li].[Rb] DJMZKFUAQIEDKC-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 229910001952 rubidium oxide Inorganic materials 0.000 description 1
- CWBWCLMMHLCMAM-UHFFFAOYSA-M rubidium(1+);hydroxide Chemical compound [OH-].[Rb+].[Rb+] CWBWCLMMHLCMAM-UHFFFAOYSA-M 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
-
- 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
-
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for extracting lithium, cesium and rubidium from pegmatite lithium concentrate, which comprises the following steps: step 1: uniformly mixing the mixed roasting additive and pegmatite lithium concentrate to obtain a mixed material; step 2: carrying out alkali fusion roasting on the mixed material to obtain roasted sand containing lithium, rubidium and cesium; and step 3: grinding the roasted product containing lithium, rubidium and cesium, and adding a leaching agent to leach after grinding to obtain a solution containing lithium, rubidium and cesium; and 4, step 4: extracting lithium, rubidium and cesium from the solution containing lithium, rubidium and cesium. According to the invention, the mixed roasting additive is added into the pegmatite lithium concentrate raw material, so that low-temperature alkali fusion roasting can be realized. In addition, the method provided by the invention can be used for large-scale industrial production, is energy-saving and environment-friendly, has low cost and has wide popularization prospect.
Description
Technical Field
The invention relates to the field of ore extraction, in particular to a method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate.
Background
At present, the lithium product is in the lithium battery industry, and accounts for about 71 percent of the total consumption. With the rapid development of the new energy battery industry in recent years, the supply of the raw materials of the lithium battery is short. Imbalances in supply and demand for lithium products have led to a rise in the price of lithium carbonate and lithium hydroxide over the last 2020. Rubidium and cesium have excellent photoelectric properties and unique chemical properties, so that metals and compounds of the rubidium and cesium are more and more widely applied to the high-new and emerging technical fields of national economy, national defense and military industry and the like. The lithia ore resources which are large in reserves in nature and convenient to develop, such as spodumene, lepidolite and lepidolite, belong to pegmatite type minerals. Mica lithium ore also contains rare metal elements such as rubidium and cesium, and is an important resource for extracting rubidium and cesium. The lithium grade of the lepidolite lithium is about 1.30 percent, and the lepidolite lithium contains a small amount of rubidium and cesium; the lithium-containing grade of the lepidolite is 1.36-3.6%, the content of rubidium is about 1%, and the lepidolite is an important resource for extracting lithium, rubidium and cesium and is one of the currently mainly exploited lithium and rubidium ore resources. The lithium grade of spodumene is 3.7%, and the spodumene is the lithium ore resource with the largest exploitation amount at present. The comprehensive development and utilization of lithium, rubidium and cesium resources in the pegmatite type minerals have extremely high economic and strategic values.
The main methods applied in the lithium extraction process industry of pegmatite lithium ore at present are respectively as follows: sulfate roasting, sulfuric acid aging, chloride roasting, etc. The roasting temperature of the sulfate roasting method is 850 ℃, the process flow is short but the cost is high, and the method is mainly used for lepidolite Dan Dili; the heating temperature of the sulfuric acid curing method is about 200 ℃, but concentrated sulfuric acid and hydrogen fluoride can volatilize in the heating process, so that severe corrosion can be caused to equipment, and the subsequent purification process is also complex; the roasting temperature of the chlorination roasting method is 850 ℃, the problem of equipment corrosion also exists, and the application is less at present. In addition, although the leaching rates of lithium by a sulfuric acid curing method and a sulfate roasting method can reach more than 95%, the leaching rates of rubidium and cesium are only 20-30%, and the comprehensive utilization rate of mica lithium ores is low; although the leaching rates of lithium, rubidium and cesium in the lepidolite concentrate by the chlorination roasting method are high and can reach 97%, the equipment is corroded by chloride ions rich in the mother liquor due to the fact that chloride salt is used as a roasting additive; the alkali roasting method needs high-pressure boiling, is not suitable for large-scale production, and can only be used for experimental research.
Therefore, the problems of high roasting temperature, high energy consumption, equipment corrosion, incapability of large-scale popularization and the like exist in the conventional process. Therefore, in the technical field of roasting and extracting lithium, rubidium and cesium from lithium ore, a method for extracting lithium, rubidium and cesium, which is efficient, energy-saving and capable of being popularized on a large scale, is urgently needed.
Disclosure of Invention
In order to solve the problems, the invention provides a method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate, which comprises the following steps:
step 1: uniformly mixing the mixed roasting additive and pegmatite lithium concentrate to obtain a mixed material;
step 2: carrying out alkali fusion roasting on the mixed material to obtain roasted sand containing lithium, rubidium and cesium;
and step 3: grinding the roasted product containing lithium, rubidium and cesium, and adding a leaching agent to leach after grinding to obtain a solution containing lithium, rubidium and cesium;
and 4, step 4: extracting lithium, rubidium and cesium from the solution containing lithium, rubidium and cesium.
Preferably, the mixed roasting additives are calcium oxide and sodium hydroxide.
Preferably, the mass ratio of sodium hydroxide to calcium oxide in the mixed roasting additive is 1-2.
Preferably, the mass ratio of the pegmatite lithium concentrate to the mixed roasting additive is 1.0-2.5.
Preferably, the roasting temperature of the alkali fusion roasting is 500-700 ℃.
Preferably, the heat preservation time of the alkali fusion roasting is 60-240 min.
Preferably, the leaching agent is water.
Preferably, in step 3, a liquid-solid ratio between the leaching agent and the roasted product containing lithium, rubidium and cesium is 2 to 4:1.
Preferably, the temperature of the leaching is 60-90 ℃.
Preferably, the leaching time is 60-90 min.
Compared with the prior art, the invention has the following advantages:
the invention discloses a method for extracting lithium, cesium and rubidium from pegmatite lithium concentrate, which comprises the following steps: step 1: uniformly mixing the mixed roasting additive with the pegmatite lithium concentrate to obtain a mixed material; step 2: carrying out alkali fusion roasting on the mixed material to obtain roasted sand containing lithium, rubidium and cesium; and step 3: grinding the roasted product containing lithium, rubidium and cesium, and adding a leaching agent to leach after grinding to obtain a solution containing lithium, rubidium and cesium; and 4, step 4: extracting lithium, rubidium and cesium from the solution containing lithium, rubidium and cesium. According to the invention, the mixed roasting additive is added into the pegmatite lithium concentrate raw material, so that low-temperature alkali fusion roasting can be realized. In addition, the method provided by the invention can be used for large-scale industrial production, is energy-saving and environment-friendly, has low cost and has wide popularization prospect.
According to the invention, the mixed roasting additive is added into the pegmatite lithium concentrate raw material, and the synergistic effect of the mixed roasting additives is utilized to destroy the structure of the lithium concentrate at a lower roasting temperature, so that the lithium concentrate is effectively decomposed, and valuable metals such as rubidium and cesium are efficiently extracted from the pegmatite lithium concentrate at a low temperature. The method provided by the invention realizes low-temperature alkali fusion roasting, and has the advantages of low energy consumption, energy conservation, environmental protection, low cost, high benefit (high leaching rate) and the like. In addition, the reaction condition in the method provided by the invention is mild (under normal pressure), so that the method provided by the invention can be used for large-scale industrial production and has wide popularization prospect.
Drawings
Fig. 1 is a flowchart of a method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate according to an embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the specific examples, which should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. The present invention employs, unless otherwise indicated, examples of reagents, methods and apparatus conventional in the art.
The invention provides a method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate, which comprises the following steps:
s101, uniformly mixing the mixed roasting additive with pegmatite lithium concentrate to obtain a mixed material;
s102, carrying out alkali fusion roasting on the mixed material to obtain roasted sand containing lithium, rubidium and cesium;
s103, grinding the roasted product containing lithium, rubidium and cesium, and adding a leaching agent to leach after grinding to obtain a solution containing lithium, rubidium and cesium;
and S104, extracting lithium, rubidium and cesium from the solution containing lithium, rubidium and cesium.
According to the embodiment of the invention, the calcine containing lithium, rubidium and cesium can be obtained at a lower roasting temperature, so that valuable metals such as lithium, rubidium and cesium can be further easily extracted from the calcine.
According to the invention, the mixed roasting additive is added into the pegmatite lithium concentrate raw material, and the synergistic effect of the mixed roasting additives is utilized to destroy the structure of the lithium concentrate at a lower roasting temperature, so that the lithium concentrate is effectively decomposed, and valuable metals such as rubidium and cesium are efficiently extracted from the pegmatite lithium concentrate at a low temperature. The method provided by the invention realizes low-temperature alkali fusion roasting, and has the advantages of low energy consumption, energy conservation, environmental protection, low cost, high benefit (high leaching rate) and the like. In addition, the reaction condition in the method provided by the invention is mild (under normal pressure), so that the method provided by the invention can be used for large-scale industrial production and has wide popularization prospect.
Preferably, the mixed roasting additives are calcium oxide and sodium hydroxide.
In the embodiment of the invention, the mixture of calcium oxide and sodium hydroxide is used as a roasting additive, and the synergistic effect of the calcium oxide and the sodium hydroxide is utilized to reduce the roasting temperature from the previous 850 ℃ to the current 700 ℃. Specifically, the synergistic effect is as follows: (1) After the roasting temperature is gradually increased, the molten NaOH provides a molten environment for the reaction of CaO, and the reaction of the lithium concentrate soaked in the molten NaOH and the CaO is more complete, so that the ion diffusion is facilitated; (2) NaOH and CaO respectively react with different structures in the lithium concentrate, so that the lithium concentrate is decomposed more thoroughly, and the subsequent leaching of lithium, rubidium and cesium is facilitated. The invention takes the mixture of the two roasting additives as the roasting additive, so that the lithium concentrate can be effectively decomposed during roasting.
Preferably, the mass ratio of sodium hydroxide to calcium oxide in the mixed roasting additive is 1-2.
Preferably, the mass ratio of the pegmatite lithium concentrate to the mixed roasting additive is 1.0-2.5.
Preferably, the roasting temperature of the alkali fusion roasting is 500-700 ℃.
In the embodiment of the invention, after the roasting temperature is gradually increased, naOH is converted from a solid state into a molten state (a nearly liquid fluid), and the molten NaOH and Al-O in lithium concentrate]The structure reacts to generate NaAlO 2 And H 2 O, thereby destroying Al-O in the lithium concentrate]Structure; caO and [ Si-O ] in lithium concentrate]The structure reacts to generate Na 4 SiO 4 、Ca 2 SiO 4 And H 2 O, further destroying [ Si-O ] in the lithium concentrate]And (5) structure. In addition, the earlier molten state NaOH provides conditions (melting environment) for the later reaction (structure damage) of CaO, and the lithium concentrate and the CaO are soaked in the molten state NaOH, so that ion diffusion is facilitated, and the reaction is more complete.
According to the invention, the synergistic effect (the two points) of NaOH and CaO is utilized, so that the structure in the lithium concentrate is more seriously damaged, and the lithium concentrate is completely decomposed, so that the subsequent leaching of lithium, cesium and rubidium is not influenced.
Preferably, the heat preservation time of the alkali fusion roasting is 60-240 min.
Preferably, the leaching agent is water.
In the embodiment of the invention, the leaching agent is selected from water for the following two reasons: (1) According to the properties of the materials to be leached in the invention, the leaching effect of water is the best; (2) convenient, inexpensive and nontoxic.
Preferably, in step 3, a liquid-solid ratio between the leaching agent and the roasted product containing lithium, rubidium and cesium is 2 to 4:1.
Preferably, the temperature of the leaching is 60-90 ℃.
Preferably, the leaching time is 60-90 min.
In the embodiment of the present invention, lithium in the calcine after calcination exists in the form of lithium hydroxide, and more rubidium and cesium in the calcine exist in the form of oxides. Grinding the calcine, adding a certain amount of leaching agent for cyclic leaching, and leaching the primary leaching solution, namely the leaching solution containing lithium, rubidium and cesium, as the leaching agent of a new batch of calcine in a co-cyclic manner for three times. Through a circulating water leaching process, lithium, rubidium and cesium in lithium hydroxide, rubidium oxide and cesium oxide are selectively leached into a solution, a leachate rich in lithium, rubidium and cesium is obtained, and impurities such as silicon and aluminum are left in leached residues. Among them, lithium hydroxide is hygroscopic, and thus, it is more advantageous for the subsequent water immersion after being dissolved in water.
In the embodiment of the invention, the alkali fusion roasting is adopted to effectively decompose the lithium concentrate, so that lithium, rubidium and cesium are well dissolved out during water leaching so as to be extracted. In the process of alkali fusion roasting, the lithium concentrate is effectively and completely decomposed by utilizing the synergistic effect of NaOH and CaO, so that the leaching rate of lithium can reach 91.7%, the leaching rate of rubidium can reach 98.8% and the leaching rate of cesium can reach 98.2% by combining with a circulating water leaching process.
In order to make the present invention more comprehensible to those skilled in the art, the method provided by the present invention is explained by selecting refractory metal raw materials with different shapes and carrying out experiments, thereby obtaining a plurality of specific examples.
In examples 1 to 7, lepidolite concentrate was used as the pegmatite lithium concentrate.
Example 1
Uniformly mixing the lepidolite concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; grinding the roasted product containing lithium, rubidium and cesium, adding water (serving as a leaching agent) with the solid-to-liquid ratio of 1:2, leaching at the leaching temperature of 90 ℃ for 60min to obtain a solution rich in lithium, rubidium and cesium, wherein the leaching rates of lithium, rubidium and cesium are 87.9%,98.8% and 84.4% respectively; finally, lithium, rubidium and cesium can be easily extracted from the solution containing lithium, rubidium and cesium.
Example 2
Uniformly mixing the lepidolite iron ore concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; grinding the roasted product containing lithium, rubidium and cesium, adding water (serving as a leaching agent) with the solid-to-liquid ratio of 1:2, leaching at the leaching temperature of 90 ℃ for 60min to obtain a solution rich in lithium, rubidium and cesium, wherein the leaching rates of lithium, rubidium and cesium are 77.5%, 97.9% and 63.8% respectively; finally, lithium, rubidium and cesium can be easily extracted from the solution containing lithium, rubidium and cesium.
Example 3
Uniformly mixing the lepidolite concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; grinding the roasted product containing lithium, rubidium and cesium, adding water (serving as a leaching agent) with the solid-to-liquid ratio of 1:2, leaching at the leaching temperature of 90 ℃ for 60min to obtain a solution rich in lithium, rubidium and cesium, wherein the leaching rates of lithium, rubidium and cesium are 76.9%, 98.7% and 65.2% respectively; finally, lithium, rubidium and cesium can be easily extracted from the solution containing lithium, rubidium and cesium.
Example 4
Uniformly mixing the lepidolite concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; finally, lithium, rubidium and cesium can be easily extracted from the solution containing lithium, rubidium and cesium.
Example 5
Uniformly mixing a lithium iron mica concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; lithium, rubidium and cesium are finally easily extracted from the solution containing lithium, rubidium and cesium.
Example 6
Uniformly mixing the lepidolite concentrate, naOH and CaO (serving as mixed roasting additives) according to the mass ratio of 1; finally, lithium, rubidium and cesium can be easily extracted from the solution containing lithium, rubidium and cesium.
Example 7
Uniformly mixing the lithium iron mica concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; lithium, rubidium and cesium are finally easily extracted from the solution containing lithium, rubidium and cesium.
In examples 8 to 10, lepidolite concentrate was used as pegmatite lithium concentrate.
Example 8
Uniformly mixing lepidolite concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; finally, lithium, rubidium and cesium can be easily extracted from the solution containing lithium, rubidium and cesium.
Example 9
Uniformly mixing lepidolite concentrate with mixed additives NaOH and CaO (serving as mixed roasting additives) according to the mass ratio of 1; finally, lithium, rubidium and cesium can be easily extracted from the solution containing lithium, rubidium and cesium.
Example 10
Uniformly mixing lepidolite concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; finally, lithium, rubidium and cesium can be easily extracted from the solution containing lithium, rubidium and cesium.
In examples 11-13, the pegmatite lithium concentrate was spodumene concentrate, and since the spodumene concentrate contained no rubidium and no cesium, only lithium was leached in examples 11-13.
Example 11
Uniformly mixing spodumene concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; lithium is eventually easily extracted from the solution containing lithium.
Example 12
Uniformly mixing spodumene concentrate, mixed additives of NaOH and CaO (serving as mixed roasting additives) according to the mass ratio of 1; lithium is finally easily extracted from the solution containing lithium rubidium cesium.
Example 13
Uniformly mixing spodumene concentrate, naOH and CaO (serving as a mixed roasting additive) according to the mass ratio of 1; grinding the calcine containing lithium, rubidium and cesium, adding water (serving as a leaching agent) with the solid-to-liquid ratio of 1:4, and leaching under the conditions that the leaching temperature is 90 ℃ and the leaching time is 60min to obtain a lithium-rich solution, wherein the leaching rate of lithium is 86.5%; lithium is finally easily extracted from the solution containing lithium rubidium cesium.
The leaching rates of cesium lithium and rubidium lithium from pegmatite lithium concentrates obtained in the above examples after low-temperature roasting are shown in table 1 below.
TABLE 1 comparison of the experimental conditions and leaching rates of lithium, cesium and rubidium in each example
For simplicity of explanation, the method embodiments are described as a series of acts or combinations, but those skilled in the art will appreciate that the present invention is not limited by the order of acts, as some steps may occur in other orders or concurrently in accordance with the invention. Further, those skilled in the art will appreciate that the embodiments described in the specification are preferred embodiments and that the acts and elements referred to are not necessarily required to practice the invention.
The method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate provided by the invention is described in detail above, and the principle and the embodiment of the invention are explained in the text by applying specific examples, and the description of the above examples is only used for helping understanding the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. A method for extracting lithium, rubidium and cesium from pegmatite lithium concentrate is characterized by comprising the following steps:
step 1: uniformly mixing the mixed roasting additive with the pegmatite lithium concentrate to obtain a mixed material;
step 2: carrying out alkali fusion roasting on the mixed material to obtain roasted sand containing lithium, rubidium and cesium;
and step 3: grinding the roasted product containing lithium, rubidium and cesium, and adding a leaching agent to leach after grinding to obtain a solution containing lithium, rubidium and cesium;
and 4, step 4: extracting lithium, rubidium and cesium from the solution containing lithium, rubidium and cesium.
2. The method of claim 1, wherein the mixed roasting additive is calcium oxide and sodium hydroxide.
3. The method according to claim 2, wherein the mass ratio of sodium hydroxide to calcium oxide in the mixed roasting additive is 1-2.
4. The method according to claim 1, wherein the mass ratio of pegmatite lithium concentrate to the mixed roasting additive is 1.0-2.5.
5. The method as claimed in claim 1, wherein the roasting temperature of the alkali fusion roasting is 500-700 ℃.
6. The method of claim 1, wherein the holding time of the alkali fusion roasting is 60-240 min.
7. The method of claim 1, wherein the leaching agent is water.
8. The method according to claim 1, wherein in step 3, a liquid-solid ratio of the leaching agent to the calcine containing lithium, rubidium and cesium is 2 to 4:1.
9. The method according to claim 1, characterized in that the temperature of the leaching is 60-90 ℃.
10. The method according to claim 1, characterized in that the leaching time is 60-90 min.
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