CN114032388B - Process for extracting metal salt from lepidolite raw material - Google Patents
Process for extracting metal salt from lepidolite raw material Download PDFInfo
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- CN114032388B CN114032388B CN202111094471.XA CN202111094471A CN114032388B CN 114032388 B CN114032388 B CN 114032388B CN 202111094471 A CN202111094471 A CN 202111094471A CN 114032388 B CN114032388 B CN 114032388B
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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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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
- C22B21/00—Obtaining aluminium
- C22B21/0015—Obtaining aluminium by wet processes
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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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- 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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Abstract
The application belongs to the technical field of lepidolite extraction, and particularly relates to a process for extracting metal salt from lepidolite raw materials. The application provides a process for extracting metal salt from lepidolite raw materials, which is characterized by comprising the following steps of: step 1, mixing lepidolite and concentrated sulfuric acid in a closed stirring type reaction kettle, and slowly adding water while stirring to react to obtain a pasty reactant; wherein the mass ratio of lepidolite to concentrated sulfuric acid to water is 1:1: (0.2 to 0.5); and 2, after the paste reactant is reacted, adding water into the closed stirring type reaction kettle to obtain a solid-liquid mixture, and carrying out solid-liquid separation on the solid-liquid mixture to obtain a liquid containing metal salt. The application provides a process for extracting metal salt from lepidolite raw materials, which can effectively solve the technical problems of high energy consumption and high acid consumption in the existing lepidolite extraction scheme.
Description
Technical Field
The application belongs to the technical field of lepidolite extraction, and particularly relates to a process for extracting metal salt from lepidolite raw materials.
Background
Lepidolite is an important mineral resource that contains abundant rare metal materials, lithium, sodium, potassium, rubidium, cesium, aluminum, and the like. The development of lepidolite ore resources has very important reality and profound significance. Therefore, development and application of lepidolite are a hot subject at present. In the process of developing and applying lithium and salts thereof, since the lepidolite raw material contains rich other metal elements, only the metal lithium and salts thereof are extracted, and the other metals are not developed and applied, so that precious mineral resources are wasted greatly, and certain pollution is caused to the environment, therefore, in the process of extracting the lithium and salts thereof in the lepidolite raw material, the extraction of lithium, sodium, potassium, rubidium, cesium, aluminum and the like is also necessary; for example, when lithium carbonate is extracted, the production cost of lithium carbonate can be greatly reduced by simultaneously extracting other metal lithium, sodium, potassium, rubidium, cesium, aluminum salt and the like.
The prior method for treating lepidolite ore mainly comprises a limestone roasting method, a sulfuric acid method, a sulfate method and an autoclaving method. The limestone roasting method is to mix and grind lepidolite ore and limestone according to a ratio of 1:3, and roast the lepidolite ore and the limestone at 875-911 ℃. Quenching the roasting material with water, grinding and leaching; the lithium decomposition rate was about 81%. The method has the advantages of wide raw material sources and low cost. However, the method has the defects of large material flow, low equipment efficiency, high energy consumption, low metal recovery rate and the like. The sulfuric acid process is to bake lepidolite ore at 900 deg.c, to eliminate fluorine, and to bake with 98% concentrated sulfuric acid at 300 deg.c for 2 hr, and the leaching rate of lithium may be over 90%. However, the lepidolite treated by the sulfuric acid method can react iron, manganese, calcium, magnesium and aluminum in the lepidolite with sulfuric acid to generate corresponding sulfate, especially aluminum, and the content of the sulfate in minerals is up to more than 20%, so that a large amount of sulfuric acid is consumed; moreover, these metals enter the leachate, which increases the purification amount of the solution, which is an environmental problem insurmountable by the sulfuric acid process. The sulfate process is superior to limestone process in that lepidolite and potassium sulfate are mixed, roasted and leached to result in high production cost. An emerging method for treating lepidolite ore by autoclaving. The autoclaving method is to bake lepidolite for defluorination and then leach the lepidolite with sodium carbonate, lime and the like, but the defluorination is not in place during defluorination and roasting, and the mechanical activation is insufficient, the autoclaving temperature is high, and high-pressure equipment is needed, so that the application of the method is greatly limited. Thus, until now, the industrial production has not been achieved yet.
Disclosure of Invention
In view of the above, the application provides a process for extracting metal salt from lepidolite raw materials, which can effectively solve the technical problems of high energy consumption and high acid consumption in the existing lepidolite extraction scheme.
The application provides a process for extracting metal salt from lepidolite raw materials, which comprises the following steps:
step 1, in a closed stirring type reaction kettle, mixing lepidolite and concentrated sulfuric acid under a closed condition, and then slowly adding water while stirring for reaction to obtain a pasty reactant; wherein the mass ratio of lepidolite to concentrated sulfuric acid to water is 1: (0.8-1): (0.2-0.35);
and 2, after the paste reactant is reacted, adding water into the closed stirring type reaction kettle to obtain a solid-liquid mixture, and carrying out solid-liquid separation on the solid-liquid mixture to obtain a liquid containing metal salt.
Specifically, the airtight stirring type reaction kettle used in the application is airtight and heat-preserving, and can stir paste.
Specifically, in a closed pressure reaction kettle, the pressure in the reaction kettle is increased to 0.4-0.5 MPa, the self-reaction temperature is up to 140-150 ℃, and the process of the application utilizes the pressure and heat generated by the self-heating principle of concentrated sulfuric acid and water in the closed stirring reaction kettle to extract alkali metals (including salts of lithium, sodium, potassium, rubidium and cesium) and salts of aluminum, and the like.
In another embodiment, in step 1, the temperature of the paste reactant is 140-150 ℃ after adding water.
In another embodiment, in step 1, after adding water, the pressure in the closed stirring type reaction kettle is 0.4-0.5 MPa.
In another embodiment, in the step 1, the lepidolite is lepidolite obtained after ball milling, and the mesh number of the lepidolite is 80-500 mesh.
In another embodiment, in step 1, the concentration of the concentrated sulfuric acid is 98% or more. Specifically, the concentration of the concentrated sulfuric acid is more than or equal to 98 percent, so that the concentrated sulfuric acid is mixed with water to generate enough heat and pressure for reaction.
In another embodiment, in step 1, the reaction time after adding water is 1 to 1.5 hours, specifically, the reaction time after adding water is 1 hour.
In another embodiment, in step 2, the temperature of the water is 25 ℃ or higher, specifically, the temperature of the water is 80 ℃.
In another embodiment, in step 2, the amount of water added is 2-3 times that of the paste reactant, and the amount of water added is 3 times that of the paste reactant.
In another embodiment, in step 2, the metal salt is one or more of lithium salt, sodium salt, potassium salt, rubidium salt, cesium salt, and aluminum salt.
In another embodiment, step 2 is followed by step 3, where step 3 is to perform impurity removal, concentration and separation treatment on the liquid containing the metal salt.
Specifically, the impurity removal, the concentration and the separation treatment are conventional treatment means.
In the conventional lepidolite acid leaching reaction, the sulfuric acid content is required to be excessive by 20% -50%, so that the reaction is ensured to be sufficient, and meanwhile, external heating is required, and the temperature during acid leaching is maintained. In the acidification roasting process, an external heat source is also required to be introduced so as to enable lepidolite to fully react with sulfuric acid. Obviously, the existing processes for extracting metal salts from lepidolite raw materials all require a large amount of sulfuric acid or severe conditions (high-temperature equipment is required to be provided), so that the energy consumption and acid consumption of the existing processes are very large.
Therefore, all the current processes for producing lithium salt or alkali metal by using lepidolite as a raw material need to adopt an external heating mode or a mode of adding a large amount of sulfuric acid for extraction, but the process is developed by utilizing the characteristic that lepidolite contains fluorine and can fully react in an acidic and pressurized environment. Meanwhile, when the acid method process is adopted, excessive acid (1.2-2 times of the acid required by the metal amount in lepidolite) is consumed to complete the reaction, and the process does not need excessive acid and only needs about 0.8-1 (0.8-1 times of the acid required by the metal amount in lepidolite) to complete the reaction. The process reduces energy consumption and acid consumption, realizes carbon emission reduction, and improves the extraction rate of valuable metals.
Detailed Description
The application provides a process for extracting metal salt from lepidolite raw materials, which is used for solving the technical defects of high energy consumption and high acid consumption in the lepidolite extraction scheme in the prior art.
The following description of the technical solutions in the embodiments of the present application will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Wherein, the raw materials or reagents used in the following examples are all commercially available or self-made.
The airtight stirring type reaction kettle used in the following examples can stir and mix pasty materials.
The lepidolite used in the examples below was ball-milled lepidolite having a mesh size of 300 mesh.
Example 1
The embodiment of the application provides a process for extracting metal salt from lepidolite raw materials, which comprises the following steps:
after 1000g of lepidolite (lithium oxide content is 3.0%) and 800g of sulfuric acid (> 98%) are uniformly mixed, the mixture is transferred into a 5L sealed stirring type reaction kettle, stirring is started under sealed conditions, then 300g of water is slowly added through a pressurizing pump, the materials in the reaction kettle start to be heated, meanwhile, the pressure is increased, a pasty reactant is obtained after the water is added, the temperature of the materials in the reaction kettle is increased to about 140 ℃, the pressure is increased to about 0.4MPa, after one hour of reaction in the reaction kettle, the reaction is completed, 3000g of cold water is continuously added into the reaction kettle, and the generated solid-liquid mixture is subjected to solid-liquid separation, so that the liquid containing metal salt is obtained.
The metal leaching rate of the above-mentioned metal salt-containing liquid was measured and found to be 95.8%.
Example 2
The embodiment of the application provides a process for extracting metal salt from lepidolite raw materials, which comprises the following steps:
after 1000g of lepidolite (lithium oxide content is 3.5%) and 900g of sulfuric acid (> 98%) are uniformly mixed, the mixture is transferred into a 5L sealed stirring type reaction kettle, stirring is started under sealed conditions, then 300g of water is slowly added through a pressurizing pump, the materials in the reaction kettle start to be heated, meanwhile, the pressure is increased, a pasty reactant is obtained after the water is added, the temperature of the materials in the reaction kettle is increased to about 145 ℃, the pressure is increased to about 0.45MPa, after one hour of reaction in the reaction kettle, the reaction is completed, 3000g of cold water is continuously added into the reaction kettle, and the generated solid-liquid mixture is subjected to solid-liquid separation, so that the liquid containing metal salt is obtained.
The metal leaching rate of the above-mentioned metal salt-containing liquid was measured and found to be 97.3%.
Example 3
The embodiment of the application provides a process for extracting metal salt from lepidolite raw materials, which comprises the following steps:
after 1000g lepidolite (lithium oxide content 4.0) and 1000g sulfuric acid (> 98%) are uniformly mixed, the mixture is transferred into a 5L closed stirring type reaction kettle, stirring is started under closed conditions, then 300g of water is slowly added through a pressurizing pump, the materials in the reaction kettle start to be heated, meanwhile, the pressure is increased, a pasty reactant is obtained after the water is added, the temperature of the materials is increased to about 150 ℃, the pressure is increased to about 0.5MPa, after one hour of reaction in the reaction kettle, the reaction is completed, 3000g of cold water is continuously added into the reaction kettle, and the generated solid-liquid mixture is subjected to solid-liquid separation, so that the liquid containing metal salt is obtained.
The metal leaching rate of the above-mentioned metal salt-containing liquid was measured and found to be 97.6%.
Comparative example 1
The comparative examples of the present application provide a control process comprising:
referring to the process flow of example 1, the difference is that in the comparative example, a non-closed non-stirring reaction kettle is adopted, the rest steps are identical to those of example 1, and after materials are added, the materials can be gradually solidified in the stirring process due to the fact that the corresponding pressure cannot be reached, so that stirring cannot be continued, and the experiment cannot be continued.
Comparative example 2
The comparative examples of the present application provide a control process comprising:
the procedure of example 1 was referred to, except that the comparative example was conducted using an excessive amount of sulfuric acid, namely, lepidolite was mixed with sulfuric acid at a sulfuric acid concentration of 50% and a mass ratio of lepidolite to sulfuric acid of 1:1.2, and after the addition of the materials, lepidolite and sulfuric acid could not form a paste, and the remaining steps were the same as those of example 1 to obtain a liquid containing a metal salt.
The metal leaching rate of the above-mentioned metal salt-containing liquid was measured and found to be 23%.
Comparative example 3
The comparative examples of the present application provide a control process comprising:
the procedure of example 1 was referred to, except that the comparative example was conducted using an excessive amount of sulfuric acid, namely, lepidolite was mixed with sulfuric acid at a sulfuric acid concentration of 50% and a mass ratio of lepidolite to sulfuric acid of 1:1.5, and after the addition of the materials, lepidolite and sulfuric acid could not form a paste, and the remaining steps were the same as those of example 1 to obtain a liquid containing a metal salt.
The metal leaching rate of the above-mentioned metal salt-containing liquid was measured and found to be 27%.
In summary, the application discloses a process for extracting metal salt from lepidolite raw materials, which is carried out in a sealed, heat-insulating and pasty material stirring reaction kettle, and can be realized only by fully reacting concentrated sulfuric acid with a small amount of water under the sealing condition and stirring in the reaction kettle. According to the process provided by the embodiment of the application, only the addition amount of concentrated sulfuric acid and water is controlled, and under the airtight heat preservation condition, the metal salt of lepidolite can be efficiently extracted without heating and pressurizing, and the leaching rate of the metal salt reaches more than 95%; if the amount of sulfuric acid and water is excessive, the amount of heat and pressure required for the reaction of sulfuric acid and water cannot be increased, and the metal salt of lepidolite cannot be extracted efficiently.
The foregoing is merely a preferred embodiment of the present application and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present application, which are intended to be comprehended within the scope of the present application.
Claims (8)
1. A process for extracting a metal salt from a lepidolite feedstock, comprising:
step 1, in a closed stirring type reaction kettle, mixing lepidolite and concentrated sulfuric acid under a closed condition, and then slowly adding water while stirring for reaction to obtain a pasty reactant; wherein the mass ratio of lepidolite to concentrated sulfuric acid to water is 1: (0.8-1): (0.2-0.35), wherein the concentration of the concentrated sulfuric acid is more than or equal to 98%, and the reaction time after adding water is 1-1.5 h;
and 2, after the paste reactant is reacted, adding water into the closed stirring type reaction kettle to obtain a solid-liquid mixture, and carrying out solid-liquid separation on the solid-liquid mixture to obtain a liquid containing metal salt.
2. The process according to claim 1, wherein in step 1, the temperature of the paste-like reactant is 140 to 150 ℃ after adding water.
3. The process according to claim 1, wherein in step 1, after adding water, the pressure in the closed stirred tank reactor is 0.4 to 0.5MPa.
4. The process according to claim 1, wherein in step 1, the lepidolite is obtained after ball milling, and the lepidolite has a mesh size of 80-500 mesh.
5. The process according to claim 1, wherein in step 2, the temperature of the water is 25 ℃ or higher.
6. The process according to claim 1, wherein in step 2, the water is added in an amount of 2 to 3 times the paste reactant.
7. The process of claim 1, wherein in step 2, the metal salt is one or more of a lithium salt, a sodium salt, a potassium salt, a rubidium salt, a cesium salt, and an aluminum salt.
8. The process according to any one of claims 1 to 7, further comprising a step 3 after the step 2, wherein the step 3 is to perform impurity removal, concentration and separation treatment on the liquid containing the metal salt.
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| CN202111094471.XA CN114032388B (en) | 2021-09-17 | 2021-09-17 | Process for extracting metal salt from lepidolite raw material |
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Citations (8)
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|---|---|---|---|---|
| US3189407A (en) * | 1960-02-11 | 1965-06-15 | Saint Gobain | Method of recovering lithium from lepidolite |
| CN101186968A (en) * | 2006-11-24 | 2008-05-28 | 江西赣锋锂业有限公司 | Method for producing refined lithium sulfate solution used in lepidolite lithium-extracting technique by sulfuric acid process |
| CN106064824A (en) * | 2016-05-26 | 2016-11-02 | 四川思达能环保科技有限公司 | A kind of production technology of sulfuric acid process lithium salts |
| CN107267754A (en) * | 2017-06-01 | 2017-10-20 | 江西南氏锂电新材料有限公司 | A kind of method that utilization sulfuric acid extracts alkali metal salt with lepidolite low-temperature solid phase reaction |
| CN107475537A (en) * | 2017-07-17 | 2017-12-15 | 江西南氏锂电新材料有限公司 | Lithium, rubidium, the method for cesium salt are extracted from lepidolite raw material |
| CN109055737A (en) * | 2018-09-03 | 2018-12-21 | 核工业北京化工冶金研究院 | A kind of method of sulfuric acid leaching lepidolite ore |
| WO2019210351A1 (en) * | 2018-04-30 | 2019-11-07 | Silica Technology Pty Ltd | Improved mica processing |
| AU2019310188A1 (en) * | 2018-07-24 | 2021-03-18 | Australian Nuclear Science And Technology Organisation | Caustic conversion process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10894997B2 (en) * | 2016-02-18 | 2021-01-19 | Li-Technology Pty Ltd. | Lithium recovery from phosphate minerals |
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2021
- 2021-09-17 CN CN202111094471.XA patent/CN114032388B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3189407A (en) * | 1960-02-11 | 1965-06-15 | Saint Gobain | Method of recovering lithium from lepidolite |
| CN101186968A (en) * | 2006-11-24 | 2008-05-28 | 江西赣锋锂业有限公司 | Method for producing refined lithium sulfate solution used in lepidolite lithium-extracting technique by sulfuric acid process |
| CN106064824A (en) * | 2016-05-26 | 2016-11-02 | 四川思达能环保科技有限公司 | A kind of production technology of sulfuric acid process lithium salts |
| CN107267754A (en) * | 2017-06-01 | 2017-10-20 | 江西南氏锂电新材料有限公司 | A kind of method that utilization sulfuric acid extracts alkali metal salt with lepidolite low-temperature solid phase reaction |
| CN107475537A (en) * | 2017-07-17 | 2017-12-15 | 江西南氏锂电新材料有限公司 | Lithium, rubidium, the method for cesium salt are extracted from lepidolite raw material |
| WO2019210351A1 (en) * | 2018-04-30 | 2019-11-07 | Silica Technology Pty Ltd | Improved mica processing |
| AU2019310188A1 (en) * | 2018-07-24 | 2021-03-18 | Australian Nuclear Science And Technology Organisation | Caustic conversion process |
| CN109055737A (en) * | 2018-09-03 | 2018-12-21 | 核工业北京化工冶金研究院 | A kind of method of sulfuric acid leaching lepidolite ore |
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