CN113636578B - Technology for improving quality of lithium carbonate prepared from lepidolite - Google Patents
Technology for improving quality of lithium carbonate prepared from lepidolite Download PDFInfo
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- CN113636578B CN113636578B CN202111059520.6A CN202111059520A CN113636578B CN 113636578 B CN113636578 B CN 113636578B CN 202111059520 A CN202111059520 A CN 202111059520A CN 113636578 B CN113636578 B CN 113636578B
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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 by lepidolite to improve quality, which relates to the field of lithium carbonate preparation and comprises the following steps of mixing, roasting, leaching, neutralizing, removing impurities, evaporating, concentrating, precipitating lithium, drying and crushing: step one: mixing, namely adding lepidolite into a mixer to be mixed with sulfate auxiliary materials, and step two: roasting, namely inputting the mixture into a rotary kiln through a belt to perform high-temperature roasting; step three: leaching, namely adding water into the roasting material obtained in the second step to carry out ball milling, and leaching lithium into mother liquor. According to the invention, the feeding speed of the lithium sulfate mixed solution is controlled during the reaction, a spiral spraying feeding mode is adopted, the material is uniformly sprayed on the liquid level, the crystal form nucleation effect of lithium carbonate is ensured, meanwhile, the purity of lithium carbonate generated by the reaction is improved by changing the reaction time, stirring speed and the like of the lithium sulfate mother solution and the saturated lithium carbonate solution, the impurity content of potassium, sodium and sulfate radical in the lithium carbonate product is reduced, and the quality of lithium carbonate is improved.
Description
Technical Field
The invention relates to the field of lithium carbonate preparation, in particular to a process for improving the quality of lithium carbonate prepared from lepidolite.
Background
Lepidolite, also known as "lepidolite", often contains rubidium, cesium, etc., monoclinic systems; the aggregate is usually in a fine scale shape, is light purple, is sometimes yellowish green and has glass luster, is mainly found in peganite, is also found in cloud rock and high-temperature hydrothermal pulse, and is a mineral raw material for extracting lithium; lithium carbonate is an inorganic compound, is dissolved in dilute acid and slightly dissolved in water, and has higher solubility in cold water than in hot water; is insoluble in alcohol and acetone, and can be used for preparing ceramics, medicines, catalysts, etc.; commonly used lithium ion battery raw materials; because the main raw material for producing lithium carbonate is salt lake brine (the ore method has low global productivity due to high cost), enterprises for producing lithium carbonate in large scale must have the salt lake resource exploitation rights with rich lithium resource reserves, which makes the industry have high resource barriers; on the other hand, as most of the resources of the global salt lake are high-magnesium low-lithium, and the technical difficulty of the process for purifying and separating lithium carbonate from high-magnesium low-lithium old brine is great, the technologies are only mastered in a few foreign companies before, so that the lithium carbonate industry has technical barriers; thus, a global oligopolistic pattern of the lithium carbonate industry is created.
In the existing process for preparing lithium carbonate by lepidolite, the temperature, stirring speed and mode, feeding mode and the like of mother liquor in a lithium precipitation process are optimized and improved in the preparation process of lithium carbonate, so that potassium, sodium and sulfate impurities of a lithium carbonate product are obviously reduced, and the higher-level standard is achieved.
In the traditional lithium precipitation process, the lithium carbonate product generated by the lithium precipitation reaction is easy to coat impurities such as potassium, sodium, sulfate radical and the like, so that the main purity of the lithium carbonate product is lower, the impurity content is higher, and the quality is influenced.
Disclosure of Invention
The invention aims at: in order to solve the problems of lower purity and higher impurity in the existing process for preparing lithium carbonate, the process for preparing lithium carbonate by lepidolite is provided for improving the quality.
In order to achieve the above purpose, the present invention provides the following technical solutions: the process for preparing the lithium carbonate by using the lepidolite for improving the quality comprises the following steps of mixing, baking, leaching, neutralizing, removing impurities, evaporating, concentrating, precipitating lithium, drying and crushing, wherein the preparation process comprises the following steps:
step one: mixing material
Adding lepidolite and sulfate auxiliary materials into a mixer for mixing;
step two: roasting
Feeding the mixed materials into a rotary kiln through a belt to perform high-temperature roasting, wherein the roasting temperature is controlled to be 800-900 ℃;
step three: leaching
Adding water into the roasting material obtained in the second step according to a certain proportion, ball-milling the roasting material by a ball mill, heating the ball-milled slurry to 60-70 ℃ in a leaching kettle, carrying out leaching reaction, and carrying out solid-liquid separation on the reacted material by a belt filter;
step four: neutralization impurity removal
Adding the leaching mother liquor obtained in the step three into a impurity removing kettle, adding lime milk into the impurity removing kettle, adjusting the PH to 11.5-12, and carrying out solid-liquid separation through a plate-and-frame filter press after the reaction is completed;
step five: evaporating and concentrating
Adding the mother liquor obtained in the step four after plate and frame 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: lithium precipitation
Adding the mixed solution obtained in the step five into a reaction kettle, adding 10% excessive saturated sodium carbonate solution into the reaction kettle, starting a stirrer at the same time, 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, and the feeding adopts a feeding mode of spiral spraying, so that materials can be uniformly sprayed on the liquid level, 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, enabling the materials to enter a siphon centrifuge for solid-liquid separation to obtain crude lithium carbonate, and carrying out twice washing and centrifugal separation on the crude lithium carbonate to obtain twice washed lithium carbonate;
step seven: drying and crushing
And adding the secondary washed lithium carbonate into a disc dryer for drying, conveying the secondary washed lithium carbonate into an air flow pulverizer for pulverization through vacuum feeding equipment after drying, and packaging after pulverization to obtain a high-purity lithium carbonate finished product.
In the sixth step, the reaction kettle comprises an upper sealing head, a lower sealing head, a cylinder body, a feed liquid inlet, a coupler, a speed reducer, a motor, a stirrer and a discharge port.
Through adopting above-mentioned technical scheme, the material can be through the feed liquid import to add to the barrel inside, and the material can be discharged through the discharge gate simultaneously.
Furthermore, the lithium sulfate feed liquid inlets are uniformly distributed on the kettle cover of the upper sealing head, and the feeding pipes are respectively provided with spiral nozzles.
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 mist state.
Further, the improved multi-curved-surface variable-section three-blade propeller stirrer is adopted, the whole propeller is streamline, the curved surface of the propeller blade is downward, so that efficient downward suction effect is generated by minimum thrust, smooth movement of a medium is finally obtained, boundary separation of energy loss is prevented, the root of the stirring blade exceeds the lower plane of the hub, the disturbance degree of the shaft end of the stirrer is reduced and the critical rotating speed of the stirrer is improved by utilizing the resistance effect of the stirring blade, 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 fully mixed, and the reaction effect is better.
Further, a right-angle flow baffle plate is arranged in the cylinder body.
Through adopting above-mentioned technical scheme, when heavy lithium reaction, can prevent effectively that stirring in-process material from becoming the vortex form, stirring effect is better, improves the effect of heavy lithium reaction.
Further, during the lithium precipitation reaction, the temperature of the lithium sulfate mixed mother liquor is controlled to be 80-90 degrees during feeding,
by adopting the technical scheme, the reaction rate between materials is improved, lithium sulfate can be rapidly reacted with saturated sodium carbonate solution to form microcrystalline lithium carbonate, and impurity ions such as potassium, sodium and the like are not easy to coat.
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, a spiral spraying feeding mode is adopted, the material is uniformly sprayed on the liquid level, the crystal form nucleation effect of lithium carbonate is ensured, meanwhile, the purity of lithium carbonate generated by the reaction is improved by changing the reaction time, stirring speed, stirring mode and the like of the lithium sulfate mother solution and the saturated lithium carbonate solution, the impurity content of potassium, sodium and sulfate radicals in the lithium carbonate product is reduced, and the quality of lithium carbonate is improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one:
the process for preparing the lithium carbonate by using the lepidolite for improving the quality comprises the following steps of mixing, baking, leaching, neutralizing, removing impurities, evaporating, concentrating, precipitating lithium, drying and crushing, wherein the preparation process comprises the following steps:
step one: mixing material
Adding lepidolite and sulfate auxiliary materials into a mixer for mixing;
step two: roasting
Feeding the mixed materials into a rotary kiln through a belt to perform high-temperature roasting, wherein the roasting temperature is controlled to be 800-900 ℃;
step three: leaching
Adding water into the roasting material obtained in the second step according to a certain proportion, ball-milling the roasting material by a ball mill, heating the ball-milled slurry to 60-70 ℃ in a leaching kettle, carrying out leaching reaction, and carrying out solid-liquid separation on the reacted material by a belt filter;
step four: neutralization impurity removal
Adding the leaching mother liquor obtained in the step three into a impurity removing kettle, adding lime milk into the impurity removing kettle, adjusting the PH to 11.5-12, and carrying out solid-liquid separation through a plate-and-frame filter press after the reaction is completed;
step five: evaporating and concentrating
Adding the mother liquor obtained in the step four after plate and frame 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: lithium precipitation
Adding the mixed solution obtained in the step five into a reaction kettle, adding 10% excessive saturated sodium carbonate solution into the reaction kettle, starting a stirrer at the same time, 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, and the feeding adopts a feeding mode of spiral spraying, so that materials can be uniformly sprayed on the liquid level, 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, enabling the materials to enter a siphon centrifuge for solid-liquid separation to obtain crude lithium carbonate, and carrying out twice washing and centrifugal separation on the crude lithium carbonate to obtain twice washed lithium carbonate;
step seven: drying and crushing
And adding the secondary washed lithium carbonate into a disc dryer for drying, conveying the secondary washed lithium carbonate into an air flow pulverizer for pulverization through vacuum feeding equipment after drying, and packaging after pulverization to obtain a high-purity lithium carbonate finished product.
In the sixth step, the reaction kettle comprises an upper sealing head, a lower sealing head, a cylinder body, a feed liquid inlet, a coupler, a speed reducer, a motor, a stirrer and a discharge port.
Through adopting above-mentioned technical scheme, the material can be through the feed liquid import to add to the barrel inside, and the material can be discharged through the discharge gate simultaneously.
Furthermore, the lithium sulfate feed liquid inlets are uniformly distributed on the kettle cover of the upper sealing head, and the feeding pipes are respectively provided with spiral nozzles.
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 mist state.
Further, the improved multi-curved-surface variable-section three-blade propeller stirrer is adopted, the whole propeller is streamline, the curved surface of the propeller blade is downward, so that efficient downward suction effect is generated by minimum thrust, smooth movement of a medium is finally obtained, boundary separation of energy loss is prevented, the root of the stirring blade exceeds the lower plane of the hub, the disturbance degree of the shaft end of the stirrer is reduced and the critical rotating speed of the stirrer is improved by utilizing the resistance effect of the stirring blade, 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 fully mixed, and the reaction effect is better.
Further, a right-angle flow baffle plate is arranged in the cylinder body.
Through adopting above-mentioned technical scheme, when heavy lithium reaction, can prevent effectively that stirring in-process material from becoming the vortex form, stirring effect is better, improves the effect of heavy lithium reaction.
Further, during the lithium precipitation reaction, the temperature of the lithium sulfate mixed mother liquor is controlled to be 80-90 degrees during feeding,
by adopting the technical scheme, the reaction rate between materials is improved, lithium sulfate can be rapidly reacted with saturated sodium carbonate solution to form microcrystalline lithium carbonate, and impurity ions such as potassium, sodium and the like are not easy to coat.
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 characteristics 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 (4)
1. A process for preparing lithium carbonate from lepidolite to improve quality is characterized by comprising the following steps: comprises the steps of mixing materials, baking, leaching, neutralizing, removing impurities, evaporating, concentrating, precipitating lithium, drying and crushing, and the preparation process comprises the following steps:
step one: mixing material
Adding lepidolite and sulfate auxiliary materials into a mixer for mixing;
step two: roasting
Feeding the mixed materials into a rotary kiln through a belt to perform high-temperature roasting, wherein the roasting temperature is controlled to be 800-900 ℃;
step three: leaching
Adding water into the roasting material obtained in the second step according to a certain proportion, ball-milling the roasting material by a ball mill, heating the ball-milled slurry to 60-70 ℃ in a leaching kettle, carrying out leaching reaction, and carrying out solid-liquid separation on the reacted material by a belt filter;
step four: neutralization impurity removal
Adding the leaching mother liquor obtained in the step three into a impurity removing kettle, adding lime milk into the impurity removing kettle, adjusting the PH to 11.5-12, and carrying out solid-liquid separation through a plate-and-frame filter press after the reaction is completed;
step five: evaporating and concentrating
Adding the mother liquor obtained in the step four after plate and frame 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: lithium precipitation
Adding the mixed solution obtained in the fifth step into a reaction kettle, heating, and starting to add the lithium sulfate mixed solution with the temperature of more than 85 ℃; simultaneously, a spiral nozzle is arranged on a feed pipe to ensure that lithium sulfate mother liquor is fed and sprayed to a liquid level in a mist mode, the feeding speed of lithium sulfate mixed solution is controlled during the reaction, materials can be uniformly sprayed to the liquid level by adopting a spiral spraying feeding mode, so that lithium carbonate generated by the reaction is rapidly crystallized and nucleated to form smaller crystal particles, the crystal nucleation effect of the lithium carbonate is ensured, a right-angle baffle plate is arranged in the reaction kettle, after the feeding is finished, the reaction is kept for 30min, after the reaction is finished, the materials enter a siphon centrifuge to carry out solid-liquid separation to obtain crude lithium carbonate, the crude lithium carbonate is subjected to twice washing and centrifugal separation to obtain secondary washed lithium carbonate, the reaction kettle comprises an upper end socket, a lower end socket, a cylinder body, a feed liquid inlet, a coupler, a speed reducer, a motor, a stirrer, a feed pipe and a discharge port, and an excessive 10% sodium carbonate saturated solution is added into the reaction kettle, simultaneously, the stirrer is started, the stirring kettle is heated to 85 ℃, the lithium sulfate mixed solution is started to be added, the stirring kettle adopts an improved multi-curved variable-section three-blade stirrer, the whole blade is streamline, a blade is a minimum curved surface is used for carrying out solid-liquid separation, and a smooth blade is effectively pumped to move to a main blade, and a stirring blade is provided with a stirring blade, and a stirring medium is provided with a smooth stirring blade, and a stirring blade is finally provided with a stirring blade and a stirring blade is used for stirring blade;
step seven: drying and crushing
And adding the secondary washed lithium carbonate into a disc dryer for drying, conveying the secondary washed lithium carbonate into an air flow pulverizer for pulverization through vacuum feeding equipment after drying, and packaging after pulverization to obtain a high-purity lithium carbonate finished product.
2. The process for preparing lithium carbonate from lepidolite according to claim 1, wherein the process comprises the following steps: in the sixth step, the feed liquid inlet is a lithium sulfate feed liquid inlet, and the lithium sulfate feed liquid inlet is uniformly distributed on the upper end socket kettle cover.
3. The process for preparing lithium carbonate from lepidolite according to claim 1, wherein the process comprises the following steps: in the sixth step, the setting of the stirrer prevents the boundary separation of the energy loss, and the root of the stirring blade exceeds the lower plane of the hub, so that the resistance effect of the stirring blade is utilized to reduce the disturbance of the shaft end of the stirrer and improve the critical rotation speed of the stirrer, thereby playing a role in preventing resonance.
4. The process for preparing lithium carbonate from lepidolite according to claim 1, wherein the process comprises the following steps: when lithium precipitation reaction is carried out, the temperature of the lithium sulfate mixed mother liquor is controlled to be 80-90 ℃, and the lithium sulfate can rapidly react with saturated sodium carbonate solution to form microcrystalline lithium carbonate, so that potassium and sodium impurity ions are not easy to coat.
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| CN109250733B (en) * | 2013-10-23 | 2021-07-16 | 内玛斯卡锂公司 | Method for preparing lithium carbonate |
| CN107416869A (en) * | 2017-05-17 | 2017-12-01 | 江西创迪科技有限公司 | A kind of production line that lithium carbonate is extracted from lepidolite ore |
| CN107162024A (en) * | 2017-07-15 | 2017-09-15 | 汕头市泛世矿产资源股份有限公司 | The technique that a kind of acidization extracts lithium carbonate from amblygonite |
| CN107902679A (en) * | 2017-11-14 | 2018-04-13 | 大余县旭日矿业科技有限公司 | A kind of industrial method for producing battery-level lithium carbonate |
| CN108640131A (en) * | 2018-04-28 | 2018-10-12 | 四川思达能环保科技有限公司 | Lithium ore prepares the method and system of lithium carbonate |
| CN110817906A (en) * | 2018-08-09 | 2020-02-21 | 戴艾霖 | Technology for greatly reducing sulfate radical content in lithium carbonate of each level in spodumene sulfuric acid process |
| CN110040750B (en) * | 2019-04-26 | 2021-10-22 | 核工业北京化工冶金研究院 | Method for treating lithium carbonate precipitation mother liquor |
| CN110342551B (en) * | 2019-08-27 | 2022-02-18 | 江西金德锂新能源科技有限公司 | Lithium carbonate production system using lepidolite as raw material |
| RU2749598C1 (en) * | 2020-11-30 | 2021-06-15 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method for processing mica concentrate |
| CN113104867A (en) * | 2021-04-07 | 2021-07-13 | 江西南氏锂电新材料有限公司 | Method for preparing lithium carbonate by acidifying and roasting lepidolite through composite sulfate |
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