CN113636578A - Process for preparing lithium carbonate from lepidolite to improve quality - Google Patents
Process for preparing lithium carbonate from lepidolite to improve quality Download PDFInfo
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- CN113636578A CN113636578A CN202111059520.6A CN202111059520A CN113636578A CN 113636578 A CN113636578 A CN 113636578A CN 202111059520 A CN202111059520 A CN 202111059520A CN 113636578 A CN113636578 A CN 113636578A
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- lithium
- lithium carbonate
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- sulfate
- lepidolite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a process for preparing lithium carbonate from lepidolite to improve quality, which relates to the field of lithium carbonate preparation, and comprises the following steps of mixing, roasting, leaching, neutralizing to remove impurities, evaporating and concentrating, precipitating lithium, drying and crushing, wherein the preparation process comprises the following steps: the method comprises the following steps: mixing, namely adding lepidolite into the mixer to mix with the sulfate auxiliary material, and performing step two: roasting, namely conveying the mixture into a rotary kiln through a belt for high-temperature roasting; step three: and (4) leaching, namely adding water into the roasted material obtained in the step two, performing ball milling, and leaching lithium into a mother solution. According to the invention, the feeding speed of the lithium sulfate mixed solution is controlled during the reaction period, the feeding mode of spiral spraying is adopted, the materials are uniformly sprayed on the liquid surface, the crystal form nucleation effect of the lithium carbonate is ensured, meanwhile, the purity of the lithium carbonate generated by the reaction is improved, the impurity content of potassium, sodium and sulfate radicals in the lithium carbonate product is reduced, and the quality of the lithium carbonate is improved by changing the reaction time, the stirring speed and the like of the lithium sulfate mother solution and the saturated lithium carbonate solution.
Description
Technical Field
The invention relates to the field of lithium carbonate preparation, in particular to a process for preparing lithium carbonate from lepidolite to improve quality.
Background
Lepidolite is also called lepidolite and often contains rubidium, cesium and the like and is of a monoclinic system; the lithium-rich mineral is a mineral raw material for extracting lithium, is usually a scaly aggregate, is light purple, is sometimes yellow green and has glass luster, is mainly found in pegmatite, is also found in astragalite and high-temperature hydrothermal veins; lithium carbonate is an inorganic compound, is dissolved in dilute acid, is slightly soluble in water, and has higher solubility in cold water than in hot water; insoluble in alcohol and acetone, and can be used for preparing ceramics, medicines, catalysts, etc.; common lithium ion battery raw materials; because the main raw material for producing the lithium carbonate is salt lake brine (the ore method has low global capacity due to high cost), enterprises for producing the lithium carbonate on a large scale must have the exploitation right of salt lake resources with rich lithium resource reserves, so that the industry has higher resource barrier; on the other hand, most of the resources of the salt lake in the world are high-magnesium low-lithium types, and the technical difficulty of the process for purifying and separating lithium carbonate from high-magnesium low-lithium old brine is high, so that the technologies are only mastered in a few foreign companies before, and the lithium carbonate industry has a technical barrier; thus, a global oligopolistic pattern of the lithium carbonate industry is created.
In the existing process for preparing lithium carbonate from lepidolite, the temperature, the stirring speed and the stirring mode of the mother liquor in the lithium precipitation process, the feeding mode and the like are optimized and improved in the preparation process of lithium carbonate, so that the impurities of potassium, sodium and sulfate radicals in lithium carbonate products are obviously reduced, and the higher-level standard is reached.
In the traditional lithium precipitation process, potassium, sodium, sulfate radicals and other impurities are easily coated by a lithium carbonate product generated by a lithium precipitation reaction, so that the lithium carbonate product has low main purity and high impurity content, and the quality is influenced.
Disclosure of Invention
The invention aims to: in order to solve the problems of low purity and high impurity content of lithium carbonate prepared by the conventional process, the process for preparing the lithium carbonate from the lepidolite is provided for improving the quality.
In order to achieve the purpose, the invention provides the following technical scheme: a process for preparing lithium carbonate from lepidolite to improve quality comprises the following steps of mixing, roasting, leaching, neutralizing and impurity removing, evaporating and concentrating, lithium precipitating, drying and crushing, and the preparation process comprises the following steps:
the method comprises the following steps: mixing material
Adding lepidolite and sulfate auxiliary materials into a mixer for mixing;
step two: roasting
Inputting the mixed materials into a rotary kiln through a belt for high-temperature roasting, wherein the roasting temperature is controlled to be 800-900 ℃;
step three: leaching
Adding water into the roasted material obtained in the second step according to a certain proportion, ball-milling the mixture by a ball mill, heating the ball-milled slurry to 60-70 ℃ in a leaching kettle, performing leaching reaction, and performing solid-liquid separation on the reacted material by a belt filter;
step four: neutralizing and removing impurities
Adding the leaching mother liquor obtained in the third step into an impurity removal kettle, adding lime milk into the impurity removal kettle, adjusting the pH value to 11.5-12, and performing solid-liquid separation through a plate-and-frame filter press after the reaction is completed;
step five: concentrating by evaporation
Adding the mother liquor obtained in the fourth step after filter pressing into an MVR evaporator, evaporating and concentrating to improve the concentration of lithium oxide in the mother liquor, wherein the concentrated mother liquor is mainly a mixed solution of lithium sulfate, sodium sulfate and potassium sulfate;
step six: precipitating lithium
Adding the mixed solution obtained in the fifth step into a reaction kettle, adding a 10% excessive sodium carbonate saturated solution into the reaction kettle, starting a stirrer, heating to 85 ℃, and starting to add the lithium sulfate mixed solution with the temperature of more than 85 ℃; meanwhile, the feeding speed of the lithium sulfate mixed solution is controlled during the reaction period, and the feeding adopts a spiral spraying feeding mode, so that the materials can be uniformly sprayed on the liquid surface, lithium carbonate generated by the reaction is rapidly crystallized and nucleated, and smaller crystal-form particles are formed; after the feeding is finished, carrying out heat preservation reaction for 30min, after the reaction is finished, feeding the material into a siphon centrifuge for solid-liquid separation to obtain crude lithium carbonate, and washing and centrifugally separating the crude lithium carbonate twice to obtain secondary washed lithium carbonate;
step seven: drying and crushing
And adding the secondary washing lithium carbonate into a disc dryer for drying, conveying the dried lithium carbonate into an airflow crusher for crushing through vacuum feeding equipment, and packaging the crushed lithium carbonate to obtain a high-purity lithium carbonate finished product.
Further, in the sixth step, the reaction kettle comprises an upper end enclosure, a lower end enclosure, a cylinder, a feed liquid inlet, a coupler, a speed reducer, a motor, a stirrer and a discharge hole.
Through adopting above-mentioned technical scheme, the material can be imported inside adding to the barrel through the feed liquid, and the material can be discharged through the discharge gate simultaneously.
Furthermore, the lithium sulfate liquid inlets are uniformly distributed on the upper end enclosure kettle cover, and the feeding pipes are respectively provided with a spiral nozzle.
By adopting the technical scheme, the feeding of the lithium sulfate mixed mother liquor is ensured to be sprayed to the reaction liquid level in a vaporific manner.
Furthermore, the stirrer adopts an improved multi-curved-surface variable-section three-blade propeller stirrer, the whole propeller type is streamline, the curved surface of the propeller blade faces downwards, so that a high-efficiency downward suction effect is generated by minimum thrust, the smooth motion of a medium is finally obtained, the boundary separation of consumed energy is prevented, the root of the stirring blade can exceed the lower plane of the hub, the disturbance degree of the shaft end of the stirrer is reduced by utilizing the resistance effect of the stirring blade, the critical rotating speed of the stirrer is improved, and the stirring blade comprises a main stirring blade and an auxiliary stirring blade.
By adopting the technical scheme, the lithium sulfate mixed mother liquor and the sodium carbonate mother liquor can be mixed more fully, and the reaction effect is better.
Furthermore, a right-angle flow baffle is arranged in the cylinder body.
Through adopting above-mentioned technical scheme, when sinking lithium reaction, can effectively prevent that stirring in-process material from becoming the vortex form, stirring effect is better, improves the effect of sinking lithium reaction.
Further, during the lithium precipitation reaction, the temperature of the lithium sulfate mixed mother liquor during feeding is controlled between 80 and 90 ℃,
by adopting the technical scheme, the reaction rate between materials is improved, and the lithium sulfate can quickly react with a saturated sodium carbonate solution to form microcrystalline lithium carbonate which is not easy to coat impurity ions such as potassium, sodium and the like.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the feeding speed of the lithium sulfate mixed solution is controlled during the reaction period, the feeding mode of spiral spraying is adopted, the materials are uniformly sprayed on the liquid surface, the crystal form nucleation effect of the lithium carbonate is ensured, and meanwhile, the purity of the lithium carbonate generated by the reaction is improved, the impurity content of potassium, sodium and sulfate radicals in the lithium carbonate product is reduced, and the quality of the lithium carbonate is improved by changing the reaction time, the stirring speed, the stirring mode and the like of the lithium sulfate mother solution and the saturated lithium carbonate solution.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a process for preparing lithium carbonate from lepidolite to improve quality comprises the following steps of mixing, roasting, leaching, neutralizing and impurity removing, evaporating and concentrating, lithium precipitating, drying and crushing, and the preparation process comprises the following steps:
the method comprises the following steps: mixing material
Adding lepidolite and sulfate auxiliary materials into a mixer for mixing;
step two: roasting
Inputting the mixed materials into a rotary kiln through a belt for high-temperature roasting, wherein the roasting temperature is controlled to be 800-900 ℃;
step three: leaching
Adding water into the roasted material obtained in the second step according to a certain proportion, ball-milling the mixture by a ball mill, heating the ball-milled slurry to 60-70 ℃ in a leaching kettle, performing leaching reaction, and performing solid-liquid separation on the reacted material by a belt filter;
step four: neutralizing and removing impurities
Adding the leaching mother liquor obtained in the third step into an impurity removal kettle, adding lime milk into the impurity removal kettle, adjusting the pH value to 11.5-12, and performing solid-liquid separation through a plate-and-frame filter press after the reaction is completed;
step five: concentrating by evaporation
Adding the mother liquor obtained in the fourth step after filter pressing into an MVR evaporator, evaporating and concentrating to improve the concentration of lithium oxide in the mother liquor, wherein the concentrated mother liquor is mainly a mixed solution of lithium sulfate, sodium sulfate and potassium sulfate;
step six: precipitating lithium
Adding the mixed solution obtained in the fifth step into a reaction kettle, adding a 10% excessive sodium carbonate saturated solution into the reaction kettle, starting a stirrer, heating to 85 ℃, and starting to add the lithium sulfate mixed solution with the temperature of more than 85 ℃; meanwhile, the feeding speed of the lithium sulfate mixed solution is controlled during the reaction period, and the feeding adopts a spiral spraying feeding mode, so that the materials can be uniformly sprayed on the liquid surface, lithium carbonate generated by the reaction is rapidly crystallized and nucleated, and smaller crystal-form particles are formed; after the feeding is finished, carrying out heat preservation reaction for 30min, after the reaction is finished, feeding the material into a siphon centrifuge for solid-liquid separation to obtain crude lithium carbonate, and washing and centrifugally separating the crude lithium carbonate twice to obtain secondary washed lithium carbonate;
step seven: drying and crushing
And adding the secondary washing lithium carbonate into a disc dryer for drying, conveying the dried lithium carbonate into an airflow crusher for crushing through vacuum feeding equipment, and packaging the crushed lithium carbonate to obtain a high-purity lithium carbonate finished product.
Further, in the sixth step, the reaction kettle comprises an upper end enclosure, a lower end enclosure, a cylinder, a feed liquid inlet, a coupler, a speed reducer, a motor, a stirrer and a discharge hole.
Through adopting above-mentioned technical scheme, the material can be imported inside adding to the barrel through the feed liquid, and the material can be discharged through the discharge gate simultaneously.
Furthermore, the lithium sulfate liquid inlets are uniformly distributed on the upper end enclosure kettle cover, and the feeding pipes are respectively provided with a spiral nozzle.
By adopting the technical scheme, the feeding of the lithium sulfate mixed mother liquor is ensured to be sprayed to the reaction liquid level in a vaporific manner.
Furthermore, the stirrer adopts an improved multi-curved-surface variable-section three-blade propeller stirrer, the whole propeller type is streamline, the curved surface of the propeller blade faces downwards, so that a high-efficiency downward suction effect is generated by minimum thrust, the smooth motion of a medium is finally obtained, the boundary separation of consumed energy is prevented, the root of the stirring blade can exceed the lower plane of the hub, the disturbance degree of the shaft end of the stirrer is reduced by utilizing the resistance effect of the stirring blade, the critical rotating speed of the stirrer is improved, and the stirring blade comprises a main stirring blade and an auxiliary stirring blade.
By adopting the technical scheme, the lithium sulfate mixed mother liquor and the sodium carbonate mother liquor can be mixed more fully, and the reaction effect is better.
Furthermore, a right-angle flow baffle is arranged in the cylinder body.
Through adopting above-mentioned technical scheme, when sinking lithium reaction, can effectively prevent that stirring in-process material from becoming the vortex form, stirring effect is better, improves the effect of sinking lithium reaction.
Further, during the lithium precipitation reaction, the temperature of the lithium sulfate mixed mother liquor during feeding is controlled between 80 and 90 ℃,
by adopting the technical scheme, the reaction rate between materials is improved, and the lithium sulfate can quickly react with a saturated sodium carbonate solution to form microcrystalline lithium carbonate which is not easy to coat impurity ions such as potassium, sodium and the like.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. A process for preparing lithium carbonate from lepidolite to improve quality is characterized by comprising the following steps: the preparation method comprises the following steps of mixing, roasting, leaching, neutralizing and impurity removing, evaporating and concentrating, precipitating lithium, drying and crushing, and the preparation process comprises the following steps:
the method comprises the following steps: mixing material
Adding lepidolite and sulfate auxiliary materials into a mixer for mixing;
step two: roasting
Inputting the mixed materials into a rotary kiln through a belt for high-temperature roasting, wherein the roasting temperature is controlled to be 800-900 ℃;
step three: leaching
Adding water into the roasted material obtained in the second step according to a certain proportion, ball-milling the mixture by a ball mill, heating the ball-milled slurry to 60-70 ℃ in a leaching kettle, performing leaching reaction, and performing solid-liquid separation on the reacted material by a belt filter;
step four: neutralizing and removing impurities
Adding the leaching mother liquor obtained in the third step into an impurity removal kettle, adding lime milk into the impurity removal kettle, adjusting the pH value to 11.5-12, and performing solid-liquid separation through a plate-and-frame filter press after the reaction is completed;
step five: concentrating by evaporation
Adding the mother liquor obtained in the fourth step after filter pressing into an MVR evaporator, evaporating and concentrating to improve the concentration of lithium oxide in the mother liquor, wherein the concentrated mother liquor is mainly a mixed solution of lithium sulfate, sodium sulfate and potassium sulfate;
step six: precipitating lithium
Adding the mixed solution obtained in the fifth step into a reaction kettle, adding a 10% excessive sodium carbonate saturated solution into the reaction kettle, starting a stirrer, heating to 85 ℃, and starting to add the lithium sulfate mixed solution with the temperature of more than 85 ℃; meanwhile, the feeding speed of the lithium sulfate mixed solution is controlled during the reaction period, and the feeding adopts a spiral spraying feeding mode, so that the materials can be uniformly sprayed on the liquid surface, lithium carbonate generated by the reaction is rapidly crystallized and nucleated, and smaller crystal-form particles are formed; after the feeding is finished, carrying out heat preservation reaction for 30min, after the reaction is finished, feeding the material into a siphon centrifuge for solid-liquid separation to obtain crude lithium carbonate, and washing and centrifugally separating the crude lithium carbonate twice to obtain secondary washed lithium carbonate;
step seven: drying and crushing
And adding the secondary washing lithium carbonate into a disc dryer for drying, conveying the dried lithium carbonate into an airflow crusher for crushing through vacuum feeding equipment, and packaging the crushed lithium carbonate to obtain a high-purity lithium carbonate finished product.
2. The process of claim 1 for improving the quality of lithium carbonate prepared from lepidolite, wherein the process comprises the following steps: in the sixth step, the reaction kettle comprises an upper seal head, a lower seal head, a cylinder, a feed liquid inlet, a coupling, a speed reducer, a motor, a stirrer and a discharge hole.
3. The process of claim 2 for improving the quality of lithium carbonate prepared from lepidolite, wherein the process comprises the following steps: the lithium sulfate liquid inlet is uniformly distributed on the upper end enclosure kettle cover, the feed pipe is respectively provided with a spiral nozzle, and the feeding of the lithium sulfate mother liquid is ensured to be sprayed to the liquid level in a vaporific manner.
4. The process of claim 2 for improving the quality of lithium carbonate prepared from lepidolite, wherein the process comprises the following steps: the stirrer adopts an improved multi-curved-surface variable-section three-blade propeller stirrer, the whole propeller type is streamline, the curved surface of the propeller blade faces downwards, so that a high-efficiency downward suction effect is generated by minimum thrust, the smooth motion of a medium is finally obtained, the boundary separation of consumed energy is prevented, the root of the stirring blade can exceed the lower plane of the hub, the disturbance degree of the shaft end of the stirrer is reduced by utilizing the resistance effect of the stirring blade, the critical rotating speed of the stirrer is improved, and the stirring blade comprises a main stirring blade and an auxiliary stirring blade.
5. The process of claim 2 for improving the quality of lithium carbonate prepared from lepidolite, wherein the process comprises the following steps: the right-angle flow baffle is arranged in the cylinder body, so that materials can be effectively prevented from being whirlpool in the stirring process during the lithium precipitation reaction, and the effect of the lithium precipitation reaction is improved.
6. The process of claim 1 for improving the quality of lithium carbonate prepared from lepidolite, wherein the process comprises the following steps: during the lithium deposition reaction, the temperature of the lithium sulfate mixed mother liquor during feeding is controlled to be 80-90 ℃, and lithium sulfate can rapidly react with a saturated sodium carbonate solution to form microcrystal lithium carbonate which is not easy to coat impurity ions such as potassium, sodium and the like.
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