CN110904343A - Method for extracting lithium by drying lepidolite by utilizing waste heat - Google Patents
Method for extracting lithium by drying lepidolite by utilizing waste heat Download PDFInfo
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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
- C22B1/06—Sulfating 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
- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention provides a method for drying lepidolite by using waste heat to extract lithium salt, which takes the lepidolite as a raw material and adopts a rotary kiln to roast the lepidolite, and comprises the processes of crushing the raw material, drying by using the waste heat, roasting in the rotary kiln, leaching, filtering, concentrating, precipitating lithium and the like, wherein the waste heat of the rotary kiln is fully utilized, and the dried lepidolite is mixed with salt and other auxiliary materials to ensure that the dried lepidolite has the water content of 4-5 percent, is favorable for being uniformly mixed with acid and is not easy to raise dust; the waste heat of the rotary kiln is fully utilized without baking the lepidolite by using extra fuel, so that the energy consumption can be saved by 20-30%; the recovery rate of rubidium and cesium can reach 5-6 times of that of the prior art; thereby improving the comprehensive development and utilization rate of the lepidolite.
Description
The technical field is as follows:
the invention relates to a method for extracting lithium from lepidolite, in particular to a method for extracting lithium salt by drying lepidolite by utilizing waste heat.
Background art:
lepidolite is an important mineral resource and contains abundant rare metal materials, lithium, sodium, potassium, rubidium, cesium, aluminum and the like. With the increasing shortage of world energy, the development and utilization of new energy are common problems in the world, and the new energy of the lithium battery is more and more regarded by various countries as one of important industries for the development of the new energy; lithium and salts thereof such as lithium carbonate and lithium sulfate are basic raw material products of the lithium new energy industry, and since lepidolite contains lithium metal which is a basic material of the lithium new energy industry, the development and application of lepidolite become a popular problem at present. In the process of developing and applying lithium and salts thereof, because the lepidolite raw material contains abundant other metal elements, only the metal lithium and the salts thereof are extracted, and the other metals are not developed and applied, precious mineral resources are greatly wasted, certain pollution is caused to the environment, and the production cost of the lithium salt is greatly reduced.
Meanwhile, in the existing calcination process of the lepidolite, a kiln production mode is generally used, mainly a vertical coal kiln and the like are used for calcination, the layered structure of the lepidolite is opened at the temperature of 800-950 ℃ during the calcination of the lepidolite, and the bulkiness of the lepidolite material is increased. When the existing calcining device and method are used at the temperature, the time of at least about 60 minutes is needed, so that firstly, the high-temperature heating is maintained for too long time, and the energy consumption is too large; and secondly, as the lepidolite ore raw material is dissolved and calcined at high temperature for a long time, the loss rate of the rare metal material in the lepidolite ore raw material is improved, and the recovery utilization rate of the rare metal, particularly lithium, is reduced.
Therefore, people begin to use a rotary kiln type calcination lithium salt preparation mode and a rotary kiln calcination lepidolite lithium extraction process, and in the rotary kiln calcination lithium extraction process commonly adopted in the lithium salt preparation of lithium ores at present, especially a lepidolite lithium extraction process with the lepidolite as a raw material is adopted. The method has the following defects that firstly, the energy consumption is high, a separate drying treatment system for the lepidolite is required, and meanwhile, the recovery rate of rubidium and cesium in the lepidolite is low and is less than 10 percent. Secondly, because the residual heat of the rotary kiln is not enough to dry all the required lepidolite, the lepidolite is often dried by additional supplementary fuel, the moisture of the general dried lepidolite is less than 1 percent, and the lepidolite is easy to raise dust in the transportation process, so that the environment is polluted; on the other hand, the single calcination mode and the stirring and mixing method for the extract have great influence on the lithium extraction yield of the lepidolite preparation. Therefore, how to provide a comprehensive roasting method adopting a rotary kiln, and waste heat generated in the roasting process of the rotary kiln is utilized to dry and treat the lepidolite, so that the yield of lithium extracted from the lepidolite can be greatly improved, the energy consumption is greatly reduced, and the extraction rates of rubidium and cesium are improved.
The invention content is as follows:
the invention provides a method for drying lepidolite by using waste heat to extract lithium salt, which takes the lepidolite as a raw material and adopts a rotary kiln to roast the lepidolite, and comprises the processes of crushing the raw material, drying by using the waste heat, roasting in the rotary kiln, leaching, filtering, concentrating, precipitating lithium and the like, wherein the waste heat of the rotary kiln is fully utilized, and the dried lepidolite is mixed with salt and other auxiliary materials to ensure that the dried lepidolite has the water content of 4-5 percent, is favorable for being uniformly mixed with acid and is not easy to raise dust; the waste heat of the rotary kiln is fully utilized without baking the lepidolite by using extra fuel, so that the energy consumption can be saved by 20-30%; the recovery rate of rubidium and cesium can reach 5-6 times of that of the prior art. Thereby improving the comprehensive development and utilization rate of the lepidolite.
The invention provides a method for extracting lithium salt by drying lepidolite by utilizing waste heat, which takes the lepidolite as a raw material and adopts a rotary kiln roasting method; which comprises the following steps of the method,
1) crushing the raw materials, namely putting the lithia ore raw materials into a crushing device for crushing to obtain lepidolite raw material powder;
2) drying by using waste heat, namely drying the lepidolite raw material powder into lepidolite semi-wet powder by using the waste heat generated by the rotary kiln;
3) preparing a mixed roasting material, fully mixing the lepidolite semi-wet powder, salt and auxiliary materials to form a mixture, controlling the corresponding moisture content of the mixture, adding concentrated sulfuric acid, and uniformly stirring and mixing to obtain the mixed roasting material;
4) feeding the materials into a rotary kiln furnace for roasting, and mechanically conveying the mixed roasted material to an inner cavity of the rotary kiln furnace for roasting to prepare a roasted material;
5) mechanical ball milling activation, namely placing the roasting material obtained in the step 4) in a ball milling device, and performing mechanical wet ball milling activation treatment to obtain a ball milling activation material;
6) leaching lithium, namely putting the ball-milling activated material obtained in the step 5) into a leaching tank, adding water, fully stirring and mixing, and performing leaching treatment to dissolve lithium in the ball-milling activated material into an aqueous solution in an ion form to obtain a leaching solution of a mixture of a lithium sulfate solution and slag;
7) filtering and deslagging, namely filtering the leachate obtained in the step 6) by using a belt filter to obtain a lithium sulfate solution and leaching slag;
8) concentrating, separating and extracting, namely purifying and impurity-removing the lithium sulfate solution obtained in the step 7), then precipitating lithium by using a sodium carbonate solution to obtain lithium carbonate and lithium precipitation mother liquor, and concentrating, separating and extracting rubidium and cesium salt products from the lithium precipitation mother liquor by using an extraction tank.
The invention relates to a method for extracting lithium salt by drying lepidolite by utilizing waste heat, which comprises the step 1) of controlling the moisture content in the lepidolite raw material powder to be 16-20 wt%.
The method for extracting lithium salt by drying lepidolite by using waste heat is characterized in that the moisture content of half-wet lepidolite powder is controlled to be 6-8 wt%; the water content of the mixture formed by fully mixing the half-wet lepidolite powder, the salt and the auxiliary materials is 4-5 wt%.
The invention relates to a method for extracting lithium salt by drying lepidolite by utilizing waste heat, which comprises the step 3) of controlling the adding amount of concentrated sulfuric acid to be 1-2 wt% of the mass of a mixture.
The invention relates to a method for drying lepidolite to extract lithium salt by utilizing waste heat, wherein in the step 4), mechanical conveying is carried out by using a screw feeder through a conveying pipeline, and an air cannon is arranged in the conveying pipeline.
The invention relates to a method for extracting lithium salt by drying lepidolite by utilizing waste heat, wherein the salt is potassium sulfate or sodium sulfate; the auxiliary materials are sodium humate and calcium hydroxide.
The main process flow of the invention comprises the following steps: lepidolite raw material crushing → waste heat drying → batching → mixer → mixing → rotary kiln roasting → clinker → ball milling → leaching tank water leaching → solid-liquid separation → slag discharge → separation to obtain lithium solution → filtration, waste removal → lithium precipitation to prepare lithium salt product.
The method has the beneficial effects that the method for drying the lepidolite to extract the lithium salt by utilizing the waste heat disclosed by the invention is based on the steps that the lepidolite with the moisture content of 16-20% is dried by utilizing the tail gas obtained after roasting in the rotary kiln to obtain semi-wet lepidolite powder with the moisture content of 6-10%, then the semi-wet lepidolite powder is mixed with salt and other auxiliary materials, then 1-2% of concentrated sulfuric acid is added, and the mixture is uniformly mixed and enters the rotary kiln to be roasted; the method of the invention cancels a lepidolite independent drying system, can save the energy consumption by 20 to 30 percent, has the recovery rate of rubidium more than 5 times of the prior art, has the recovery rate of cesium more than 6 times of the prior art, and can only achieve 0.2 to 0.4g/l of the recovery of cesium and rubidium in the process of roasting lithium salt, cesium and rubidium by using a rotary kiln without using the raw materials of the method of the invention; the method of the invention can only recover 1-1.2g/l of cesium and rubidium by drying waste heat and roasting concentrated sulfuric acid.
When the lepidolite is roasted by the conventional rotary kiln, the waste heat of the rotary kiln is not enough to dry the required lepidolite, so that the lepidolite is often dried by additionally supplementing fuel until the moisture of the dried mica is less than 1%, and the lepidolite raw material powder is very easy to fly dust in the transportation process. The method firstly utilizes the residual heat of the rotary kiln to dry the lepidolite raw material powder until the moisture content is 6-8%. And the applicant verifies through actual production that the waste heat of the rotary kiln is enough to dry the required lithium mica until the moisture content is 6-8%. Thus, the residual heat of the rotary kiln can be fully utilized without additionally supplementing fuel required for completely drying the lepidolite, and the lepidolite raw material powder with the moisture content of 6-8 percent is mixed with salt and other auxiliary materials to obtain the lepidolite powder with the moisture content of 4-5 percent. On one hand, the dust-proof agent is favorable for being uniformly mixed with acid and is not easy to raise dust. The moisture content of the mixture formed by fully mixing the lepidolite semi-wet powder, the salt and the auxiliary materials is 4-5 wt%, dust is not easy to fly in the transportation process, but due to the caking property of the mixture, the invention ensures smooth transportation by using a mandatory transportation device of the screw feeder and adding an air cannon in the conveying pipe. The invention fully utilizes the waste heat of the rotary kiln without using extra fuel to bake the lepidolite, and can save 20 to 30 percent of energy consumption. The recovery rate of rubidium and cesium is high: because the sulfuric acid is added to facilitate the leaching of rubidium and cesium, the recovery rate of rubidium can reach 5 times of the original process, and the recovery rate of cesium can reach 6 times of the original process.
On the other hand, the invention improves the extraction utilization rate of the rare metal raw material in the lepidolite raw material, reduces the energy consumption and shortens the reaction time; the ball milling of the lepidolite raw material is very convenient for the subsequent extraction and filtration of the lepidolite. Therefore, when the method is used for roasting the lepidolite raw material, the extraction rate of lithium and other rare metal elements in the lepidolite raw material is greatly improved, and the lithium extraction rate is more than 97 percent through detection.
The specific implementation mode is as follows:
the following will further describe the specific technical scheme of the present invention in detail with reference to the examples, wherein the components are referred to by mass parts or mass ratios, and the concentrations are mass concentrations.
Example 1:
the invention discloses a method for extracting lithium salt by drying lepidolite by utilizing waste heat, which is a method for roasting lepidolite by using a rotary kiln, wherein the lepidolite is produced by using some tantalum-niobium lithium ore which is suitable for spring, the raw material used in the embodiment is a lepidolite raw material, the main chemical components of the lepidolite comprise the following components (wt%), and the balance is fluorine, and the following table 1:
| Li2O | K2O | Na2O | AL2O3 | SiO2 | Fe2O3 | Rb2O | Cs2O |
| 3.24 | 12.76 | 0.61 | 24.01 | 52.78 | 0.51 | 1.66 | 0.40 |
the invention discloses a method for extracting lithium salt by drying lepidolite by utilizing waste heat, which takes the lepidolite as a raw material and adopts a rotary kiln roasting method; which comprises the following steps of the method,
1) crushing the raw materials, namely putting the lithia ore raw materials into a crushing device for crushing to obtain lepidolite raw material powder;
2) drying by using waste heat, namely drying the lepidolite raw material powder with the moisture content of 16-20 wt% by using the waste heat generated by the rotary kiln to obtain lepidolite semi-wet powder with the moisture content of 6-8 wt%;
3) preparing a mixed roasting material, fully mixing the lepidolite semi-wet powder with the water content of 6-8wt%, salt and auxiliary materials,
forming a mixture with the water content of 4-5 wt%, controlling the corresponding water content of the mixture, adding concentrated sulfuric acid with the mass of 1-2 wt% of the mass of the mixture, wherein the concentrated sulfuric acid is a sulfuric acid solution with the mass concentration of more than 96% and generally less than 98%, and stirring and mixing uniformly to obtain a mixed roasting material; the salt is potassium sulfate or sodium sulfate; the auxiliary materials are sodium humate and calcium hydroxide, and the mass ratio of the sodium humate to the calcium hydroxide can be controlled to be 0.5-1: 1; the auxiliary material can also be the mixture of calcium chloride, sodium hydroxide and calcium oxide;
4) feeding the mixture into a rotary kiln furnace for roasting, and mechanically conveying the mixed roasted material, namely conveying the mixed roasted material by a screw feeder through a conveying pipeline, wherein an air cannon is arranged in the conveying pipeline to an inner cavity of the rotary kiln furnace for roasting to prepare the roasted material;
5) mechanical ball milling activation, namely placing the roasting material obtained in the step 4) in a ball milling device, and performing mechanical wet ball milling activation treatment to obtain a ball milling activation material;
6) leaching lithium, namely putting the ball-milling activated material obtained in the step 5) into a leaching tank, adding water, fully stirring and mixing, and performing leaching treatment to dissolve lithium in the ball-milling activated material into an aqueous solution in an ion form to obtain a leaching solution of a mixture of a lithium sulfate solution and slag;
7) filtering and deslagging, namely filtering the leachate obtained in the step 6) by using a belt filter to obtain a lithium sulfate solution and leaching slag;
8) concentrating, separating and extracting, namely purifying and impurity-removing the lithium sulfate solution obtained in the step 7), then precipitating lithium by using a sodium carbonate solution to obtain lithium carbonate and lithium precipitation mother liquor, and concentrating, separating and extracting rubidium and cesium salt products from the lithium precipitation mother liquor by using an extraction tank. Preparing lithium carbonate by using salt; adding sulfate to prepare a lithium sulfate extracting product; the extraction rate of each rare metal is shown in table 2.
Through detection and calculation, the extraction and leaching rates of lithium, rubidium and cesium in the lepidolite raw material are greatly improved after the lepidolite raw material is dried by waste heat and calcined in a rotary kiln, and the leaching rates of various rare elements in the method are shown in table 2.
TABLE 2
Description of the drawings: table 2 shows the comparison between the method for extracting lithium salt by drying lepidolite using waste heat according to the present invention and the method for extracting lithium from lepidolite material using a rotary kiln as in the prior art, and the extraction and leaching rates of each rare metal element.
In table 2, 1, the leaching rate of lithium and various rare elements in the lepidolite raw material is extracted by the method for extracting lithium salt by drying lepidolite by using waste heat according to the invention;
reference 2 is a comparison example, which is the extraction leaching rate of extracting lithium and various rare elements in the lepidolite raw material by adopting the roasting extraction technology of the existing rotary kiln.
The energy consumption for extracting the lithium salt in the lepidolite by using the method is low: the waste heat of the rotary kiln is fully utilized without baking the lepidolite by using extra fuel, so that the energy consumption can be saved by 20-30%; the recovery rate of rubidium and cesium is high: because the sulfuric acid is added to facilitate the leaching of rubidium and cesium, the recovery rate of rubidium can reach 5 times of the original process, and the recovery rate of cesium can reach 6 times of the original process.
Technical features not described in the present invention may be implemented by or using the prior art, and are not described herein again. It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above embodiments, and those skilled in the art may make modifications, alterations, additions or substitutions within the spirit and scope of the present invention.
Claims (6)
1. A method for extracting lithium salt by drying lepidolite by utilizing waste heat takes the lepidolite as a raw material and adopts a rotary kiln roasting method; the method is characterized by comprising the following method steps,
1) crushing the raw materials, namely putting the lithia ore raw materials into a crushing device for crushing to obtain lepidolite raw material powder;
2) drying by using waste heat, namely drying the lepidolite raw material powder into lepidolite semi-wet powder by using the waste heat generated by the rotary kiln;
3) preparing a mixed roasting material, fully mixing the lepidolite semi-wet powder, salt and auxiliary materials to form a mixture, controlling the corresponding moisture content of the mixture, adding concentrated sulfuric acid, and uniformly stirring and mixing to obtain the mixed roasting material;
4) feeding the materials into a rotary kiln furnace for roasting, and mechanically conveying the mixed roasted material to an inner cavity of the rotary kiln furnace for roasting to prepare a roasted material;
5) mechanical ball milling activation, namely placing the roasting material obtained in the step 4) in a ball milling device, and performing mechanical wet ball milling activation treatment to obtain a ball milling activation material;
6) leaching lithium, namely putting the ball-milling activated material obtained in the step 5) into a leaching tank, adding water, fully stirring and mixing, and performing leaching treatment to dissolve lithium in the ball-milling activated material into an aqueous solution in an ion form to obtain a leaching solution of a mixture of a lithium sulfate solution and slag;
7) filtering and deslagging, namely filtering the leachate obtained in the step 6) by using a belt filter to obtain a lithium sulfate solution and leaching slag;
8) concentrating, separating and extracting, namely purifying and impurity-removing the lithium sulfate solution obtained in the step 7), then precipitating lithium by using a sodium carbonate solution to obtain lithium carbonate and lithium precipitation mother liquor, and concentrating, separating and extracting rubidium and cesium salt products from the lithium precipitation mother liquor by using an extraction tank.
2. The method for extracting lithium salt from lepidolite by drying with residual heat according to claim 1, wherein the moisture content in the lepidolite raw material powder in step 1) is controlled to 16-20 wt%.
3. The method for extracting lithium salt from lepidolite by drying with waste heat as claimed in claim 1, wherein the moisture content of the half wet powder of lepidolite is controlled to 6-8 wt%; the water content of the mixture formed by fully mixing the half-wet lepidolite powder, the salt and the auxiliary materials is 4-5 wt%.
4. The method for extracting lithium salt by drying lepidolite through waste heat according to claim 1, wherein the adding amount of concentrated sulfuric acid in the step 3) is controlled to be 1-2 wt% of the mass of the mixture.
5. The method for extracting lithium salt by drying lepidolite through waste heat according to claim 1, wherein the mechanical conveying in the step 4) is carried out by using a screw feeder through a conveying pipeline, and an air cannon is arranged in the conveying pipeline.
6. The method for extracting lithium salt by drying lepidolite through waste heat according to claim 1, wherein the salt is potassium sulfate or sodium sulfate; the auxiliary materials are sodium humate and calcium hydroxide.
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