CN113697830A - Device and process for producing high-purity nano lithium carbonate - Google Patents
Device and process for producing high-purity nano lithium carbonate Download PDFInfo
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- CN113697830A CN113697830A CN202111134084.4A CN202111134084A CN113697830A CN 113697830 A CN113697830 A CN 113697830A CN 202111134084 A CN202111134084 A CN 202111134084A CN 113697830 A CN113697830 A CN 113697830A
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- 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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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 device and a process for producing high-purity nano lithium carbonate, wherein the device comprises a synthesis reaction module, a filtering and washing module, a separation module, a distilled water recycling module and a drying module; the synthesis reaction module and the filtering and washing module are connected to form a circulation loop, the filtering and washing module is sequentially connected with the separation module and the synthesis reaction module to form a circulation loop, the separation module is connected with the distilled water recycling module, the distilled water recycling module is connected with the filtering and washing module, and the filtering and washing module is connected with the drying module; the synthesis reaction module is used for reacting and synthesizing the nano lithium carbonate, the filtering and washing module is used for carrying out solid-liquid separation and filter cake washing on the synthesized nano lithium carbonate slurry, and the separation module is used for separating and processing the filtrate and recovering the elution agent for producing the nano lithium carbonate. According to the invention, the materials are recycled through the cyclic connection of the modules, the produced by-products can be effectively recovered, the implementation cost is low, and the obtained nano lithium carbonate has high purity and small particle size.
Description
Technical Field
The invention belongs to the technical field of production processes of nano lithium carbonate, and particularly relates to a device and a process for producing high-purity nano lithium carbonate.
Background
Lithium carbonate is used in a wide range of industrial applications, and is often used as a raw material for producing other lithium salts (lithium chloride, lithium bromide, lithium molybdate, lithium hydroxide, lithium oxide, etc.), and more importantly, lithium carbonate is one of the main raw materials for preparing lithium iron phosphate, which is a positive electrode material of lithium batteries.
The conventional lithium carbonate preparation process mainly comprises an aqueous solution method, a gas-liquid phase contact method and the like, the operation process is complicated, the automation degree of production equipment is low, the energy consumption is high, secondary pollution to the environment is often caused, and the particle size of a synthesized lithium carbonate finished product is large and cannot be directly used as a raw material for synthesizing lithium iron phosphate.
Disclosure of Invention
In order to solve the problems, the invention mainly aims to provide a device for producing high-concentration nano lithium carbonate and a process thereof.
In order to achieve the purpose, the following technical scheme is provided:
a device for producing high-purity nano lithium carbonate comprises a synthesis reaction module, a filtering and washing module, a separation module, a distilled water recycling module and a drying module; the synthesis reaction module and the filtering and washing module are connected to form a circulation loop, the filtering and washing module is sequentially connected with the separation module and the synthesis reaction module to form a circulation loop, the separation module is connected with the distilled water recycling module, the distilled water recycling module is connected with the filtering and washing module, and the filtering and washing module is connected with the drying module;
the synthesis reaction module is used for reacting and synthesizing the nano lithium carbonate, the filtering and washing module is used for carrying out solid-liquid separation and filter cake washing on the synthesized nano lithium carbonate slurry, and the separation module is used for separating and processing the filtrate and recovering the elution agent for producing the nano lithium carbonate.
Further, the synthesis reaction module comprises a lithium salt quantitative feeding device, an impurity removing device, a residue filtering device, a carbonate quantitative feeding device, a lithium solution synthesizing device, a lithium solution transferring pump, a nanometer lithium carbonate synthesizing device and a lithium carbonate transferring pump; lithium salt dosing device is connected with the edulcoration equipment, and the edulcoration equipment passes through the pump to be connected with residue filtration equipment, and residue filtration equipment is connected with lithium solution synthesis equipment, and carbonate dosing device is connected with lithium solution synthesis equipment, and lithium solution synthesis equipment passes through lithium solution and changes the material pump to be connected with nanometer lithium carbonate synthesis equipment, and nanometer lithium carbonate synthesis equipment passes through lithium carbonate and changes the material pump and filter the washing module and be connected.
Furthermore, the filtering and washing module comprises a lithium carbonate washing and filtering device, a filtrate tank, a plurality of water washing tanks and a plurality of corresponding water washing recycling pumps, the lithium carbonate transferring pump is connected with the lithium carbonate washing and filtering device, the lithium carbonate washing and filtering device is used for separating filter cakes and filtrate and washing the filter cakes with synthesized nano lithium carbonate slurry, the front end of the lithium carbonate washing and filtering device is connected with the filtrate tank, the rear end of the lithium carbonate washing and filtering device is connected with the plurality of water washing tanks, the outlet of the filtrate tank is connected with the separating module, a washing water tank for collecting washing water after the filter cake is primarily washed is connected with impurity removal equipment through a washing water recycling pump to form a circulation loop, and the washing water tank for collecting the washing water after the later washing of the filter cake is connected with the lithium carbonate washing and filtering equipment by connecting the respective washing water recycling pumps to form a circulating washing system, and a discharge hole of the lithium carbonate washing and filtering equipment is connected with the drying module.
Furthermore, the separation module comprises a drying agent quantitative feeding device, a drying reaction device, a first filtering device, a crystallization evaporation feeding tank, a crystallization evaporation heater, an evaporator, a dissolving agent recycling tank and a second filtering device, wherein the drying agent quantitative feeding device is connected with the drying reaction device, the drying reaction device is connected with the first filtering device through a pump, the first filtering device is connected with the crystallization evaporation feeding tank, a bottom pipeline of the crystallization evaporation heater is divided into two pipelines, one pipeline is connected with the crystallization evaporation feeding tank through the pump, the other pipeline is connected with a bottom outlet of the evaporator through a circulating pump, a top outlet of the crystallization evaporation heater is connected with the evaporator through a pipeline to form a circulation loop, and the top of the evaporator is connected with the distilled water recycling module through a pipeline; and a pipeline which is connected with the bottom outlet of the evaporator and the circulating pump is divided into a pipeline which is sequentially connected with the second filtering equipment and the elution agent recycling tank, and the elution agent recycling tank is connected with the nano-scale lithium carbonate synthesizing equipment through the elution agent recycling pump.
Further, distilled water retrieval and utilization module include steam condenser, distilled water retrieval and utilization jar and distilled water retrieval and utilization pump, the top of evaporimeter is passed through the pipeline and is connected with steam condenser, steam condenser's export connects gradually distilled water retrieval and utilization jar and distilled water retrieval and utilization pump, distilled water retrieval and utilization pump is connected with lithium carbonate washing filtration equipment.
Further, the drying module comprises a dryer quantitative feeding device, a flash dryer, a bag-type dust collector and an induced draft fan, a discharge port of the lithium carbonate washing and filtering equipment is connected with the dryer quantitative feeding device, the dryer quantitative feeding device is connected with the flash dryer, and an outlet of the flash dryer is sequentially connected with the bag-type dust collector and the induced draft fan.
Furthermore, flow controllers are arranged on a connecting pipeline of the washing water recycling pump and the impurity removing equipment, a connecting pipeline of the dissolving agent recycling pump and the nano-scale lithium carbonate synthesizing equipment, a connecting pipeline of the filtrate tank and the drying reaction equipment, and a connecting pipeline of the crystallization evaporation feeding tank and the crystallization evaporation heater.
A process for producing high-purity nano lithium carbonate comprises the following steps:
1) a reaction process: firstly, adding water into impurity removal equipment through a flow controller, starting stirring, adding lithium salt into the impurity removal equipment through a lithium salt quantitative feeding device, then adding liquid alkali into the impurity removal equipment through the flow controller, carrying out impurity removal reaction, filtering and deslagging an obtained solution through residue filtering equipment, and then feeding the obtained solution into lithium solution synthesis equipment; adding carbonate into lithium solution synthesis equipment through a carbonate quantitative feeding device, carrying out lithium solution synthesis reaction at 20 ℃, pumping the reacted lithium solution into nano lithium carbonate synthesis equipment through a lithium solution transfer pump, simultaneously adding a elution agent, carrying out elution reaction at 20 ℃, and feeding the reacted lithium carbonate slurry into a washing process through a lithium carbonate transfer pump;
2) a filtering and washing procedure: the nanometer lithium carbonate slurry enters lithium carbonate washing and filtering equipment for filtering, filtrate and a lithium carbonate filter cake are filtered out, the filtrate enters a filtrate tank, the filter cake is washed by water for multiple times to obtain a lithium carbonate wet material, and the lithium carbonate wet material enters a drying procedure;
3) and (3) separating by-products: adding the filtrate in the filtrate tank into a drying reaction device through a flow controller, simultaneously adding a drying agent through a drying agent quantitative feeding device, carrying out drying reaction at room temperature, adding the solution into a first filtering device for solid-liquid separation after the drying agent is completely added, filtering to obtain calcium sulfate, placing the separated liquid into a crystallization evaporation feeding tank for temporary storage, heating the separated liquid in a crystallization evaporation heater, heating the heated separated liquid in an evaporator for evaporation, circularly evaporating the heated separated liquid through a circulating pump, filtering the evaporated and crystallized slurry through a second filtering device, and separating out sodium hydroxide and a solventing-out agent;
4) recycling of distilled water and a leaching agent: condensing steam at the top of the evaporator through a steam condenser, temporarily storing the steam in a distilled water recycling tank, and feeding the distilled water into lithium carbonate washing and filtering equipment through a distilled water recycling pump for washing; the elution agent temporarily stored in the elution agent recycling tank enters the nano-scale lithium carbonate synthesis equipment through an elution agent recycling pump for recycling;
5) a drying procedure: and (3) adding the filter cake washed in the step 2) into a flash evaporation dryer through a dryer dosing device for drying, and removing dust through a bag-type dust remover.
Further, the elution agent in the step 1) is at least one of dihydric alcohol, trihydric alcohol or sulfoxide; the dihydric alcohol comprises at least one of ethylene glycol and propylene glycol, the trihydric alcohol comprises at least one of glycerol and butanetriol, and the sulfoxide comprises at least one of dimethyl sulfoxide and diethyl sulfoxide.
Further, the lithium salt is lithium sulfate, the carbonate is sodium carbonate, the caustic soda is 34% of industrial common caustic soda liquid, the drying agent is calcium oxide, the concentration of the lithium sulfate is 0.1-1 mol/L, the concentration of the sodium carbonate is 0.1-1 mol/L, the feeding molar ratio of the calcium oxide to the lithium sulfate to the sodium carbonate is 1:1, and the feeding volume ratio of the elution agent to the water is 0.1-5: 1.
The invention has the beneficial effects that: according to the invention, the materials are recycled through the cyclic connection of the modules, the produced by-products can be effectively recovered, no secondary pollution is caused, the whole process is green and efficient, the implementation cost is low, and the prepared nano lithium carbonate has high purity and small particle size.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a schematic flow chart of the apparatus of the present invention;
in the figure: 1. a lithium salt quantitative feeding device; 2. impurity removal equipment; 3. a residue filtration device; 4. a carbonate dosing device; 5. a lithium solution synthesis device; 6. a lithium solution transfer pump; 7. nanometer lithium carbonate synthesis equipment; 8. a lithium carbonate transfer pump; 9. washing and filtering equipment by lithium carbonate; 10. a filtrate tank; 11. a water washing tank; 12. a washing water recycling pump; 13. a desiccant dosing device; 14. drying the reaction equipment; 15. a first filtering device; 16. a crystallization evaporation feed tank; 17. a crystallization evaporation heater; 18. an evaporator; 19. a leaching agent recycling tank; 20. a second filtering device; 21. a steam condenser; 22. a distilled water recycling tank; 23. a distilled water recycling pump; 24. a leaching agent recycling pump; 25. a dryer dosing device; 26. a flash dryer; 27. a bag-type dust collector; 28. an induced draft fan; 29. a flow controller.
Detailed Description
The invention will be further described with reference to the drawings and examples in the following description, but the scope of the invention is not limited thereto.
As shown in fig. 1, a process for producing high-purity nano lithium carbonate includes the following steps: sequentially adding lithium salt and water into an impurity removal device 2, then adding liquid alkali for impurity removal reaction, filtering through a residue filtering device 3 to obtain a first by-product, adding the solution obtained by the reaction into a lithium solution synthesis device 5, then adding carbonate for lithium solution synthesis reaction, feeding the lithium solution obtained by the reaction into a nano lithium carbonate synthesis device 7, simultaneously adding a elution agent for reaction, filtering the nano lithium carbonate generated by the reaction through a lithium carbonate washing and filtering device 9, filtering to obtain a filter cake and filtrate, washing the filter cake, recycling the washing water in the washing process, wherein one part of the recycling water is used as the water in the lithium solution synthesis device 5, and the other part of the recycling water is used as washing water; drying the washed filter cake by drying equipment to obtain a nano lithium carbonate product; and (3) carrying out reaction separation on the filtrate through a drying reaction device 14 and a first filtering device 15 to obtain a secondary product II, carrying out evaporation and condensation on the slurry to obtain pure water, recycling the pure water for washing, carrying out solid-liquid separation on the slurry through a second filtering device 20 to obtain a secondary product III and a elutriating agent, and recycling the elutriating agent.
As shown in fig. 2, an apparatus for producing high-purity nano lithium carbonate includes an impurity removing device 2, a residue filtering device 3, a lithium solution synthesizing device 5, a nano-scale lithium carbonate synthesizing device 7, a lithium carbonate washing filtering device 9, a drying reaction device 14, a first filtering device 15, a crystallization evaporation heater 17, an evaporator 18, a second filtering device 20, a steam condenser 21 and a flash dryer 26; the lithium salt quantitative feeding device 1 is connected with the impurity removing device 2, the impurity removing device 2 is connected with the residue filtering device 3 through a pump, the residue filtering device 3 is connected with the lithium solution synthesizing device 5, the carbonate quantitative feeding device 4 is arranged on the lithium solution synthesizing device 5, the lithium solution synthesizing device 5 is connected with the nanometer lithium carbonate synthesizing device 7 through a lithium solution transferring pump 6, the nanometer lithium carbonate synthesizing device 7 is connected with the lithium carbonate washing filtering device 9 through a lithium carbonate transferring pump 8, the lithium carbonate washing filtering device 9 is used for separating filter cakes and filtrate of synthesized nanometer lithium carbonate slurry and washing the filter cakes, a filtrate tank 10 is arranged at the front end of the lithium carbonate washing filtering device 9, the rear end of the lithium carbonate washing filtering device is connected with a plurality of washing tanks 11, the outlet of the filtrate tank 10 is connected with the drying reaction device 14, the washing tank 11 for collecting washing water after primary washing is connected with the impurity removing device 2 through a washing water recycling pump 12 to form a circulation loop, a washing water tank 11 for collecting washing water after the later washing of the filter cake is connected with a lithium carbonate washing and filtering device 9 through respective washing water recycling pumps 12 to form a circulating washing system, a discharge port of the lithium carbonate washing and filtering device 9 is connected with a flash evaporation dryer 26 through a dryer quantitative feeding device 25, and an outlet of the flash evaporation dryer 26 is sequentially connected with a bag-type dust collector 27 and an induced draft fan 28; a drying agent quantitative feeding device 13 is arranged on the drying reaction equipment 14, the drying reaction equipment 14 is connected with a first filtering device 15 through a pump, the first filtering device 15 is connected with a crystallization evaporation feeding tank 16, a bottom pipeline of a crystallization evaporation heater 17 is divided into two pipelines, one pipeline is connected with the crystallization evaporation feeding tank 16 through the pump, the other pipeline is connected with an outlet at the bottom of an evaporator 18 through a circulating pump, an outlet at the top of the crystallization evaporation heater 17 is connected with the evaporator 18 through a pipeline to form a circulating loop, the top of the evaporator 18 is connected with a steam condenser 21 through a pipeline, an outlet of the steam condenser 21 is sequentially connected with a distilled water recycling tank 22 and a distilled water recycling pump 23, the distilled water recycling pump 23 is connected with a lithium carbonate washing filtering device 9, a pipeline which is connected with the circulating pump and is divided from the outlet at the bottom of the evaporator 18 and is sequentially connected with a second filtering device 20 and a solvent-out agent tank 19, the eluent recycling tank 19 is connected with the nano-scale lithium carbonate synthesis equipment 7 through an eluent recycling pump 24.
A flow controller 29 is arranged on a connecting pipeline between the washing water recycling pump 12 and the impurity removing device 2, a connecting pipeline between the dissolving agent recycling pump 24 and the nano lithium carbonate synthesizing device 7, a connecting pipeline between the filtrate tank 10 and the drying reaction device 14, and a connecting pipeline between the crystallization evaporation feeding tank 16 and the crystallization evaporation heater 17.
Example 1
1) A reaction process: firstly, 8000L of water is added into impurity removing equipment 2 through a flow controller 29, then lithium sulfate is added into the impurity removing equipment 2 through a lithium salt quantitative feeding device 1, then 34 percent of liquid alkali is added, the final concentration is 0.02 mol/L to carry out impurity removal reaction, the reactant is filtered by residue filtering equipment 3, the filtered solution enters lithium solution synthesis equipment 5, sodium carbonate is added into a lithium solution synthesis device 5 through a carbonate quantitative feeding device 4, stirring is started, the concentration of the sodium carbonate is 1 mol/L, the concentration of the lithium sulfate is 1 mol/L, performing lithium solution synthesis reaction at the normal temperature of 20 ℃, pumping the lithium solution into nano-scale lithium carbonate synthesis equipment 7 through a lithium solution transfer pump 6, simultaneously adding 800L of a solvent-out agent dimethyl sulfoxide (DMSO), carrying out elution reaction at normal temperature, and after the reaction is finished, enabling the nano lithium carbonate slurry to enter a filtering and washing process through a lithium carbonate transfer pump 8;
2) a filtering and washing procedure: the nanometer lithium carbonate slurry enters a lithium carbonate washing and filtering device 9 for filtering, filtrate and a lithium carbonate filter cake are filtered out, the filtrate enters a filtrate tank 10, the filter cake is washed by water for five times to obtain a lithium carbonate wet material, and the lithium carbonate wet material enters a drying procedure;
3) and (3) separating by-products: adding the filtrate in the filtrate tank 10 into a drying reaction device 14 through a flow controller 29, simultaneously adding a calcium oxide desiccant through a desiccant quantitative feeding device 13, wherein the final concentration of calcium oxide is 1 mol/L, performing drying reaction at room temperature, adding the solution into a first filtering device 15 for solid-liquid separation after the desiccant is completely added, filtering to obtain calcium sulfate, temporarily storing the separated liquid in a crystallization evaporation feeding tank 16, heating the separated liquid in a crystallization evaporation heater 17 at a heating temperature of 130 ℃, then evaporating the separated liquid in an evaporator 18, circularly evaporating the separated liquid through a circulating pump, filtering the slurry subjected to evaporation crystallization through a second filtering device 20, and separating out sodium hydroxide and a dissolving agent;
4) recycling of distilled water and a leaching agent: steam at the top of the evaporator 18 is condensed by a steam condenser 21 and temporarily stored by a distilled water recycling tank 22, and the distilled water enters the lithium carbonate washing and filtering device 9 through a distilled water recycling pump 23 for water washing; the elution agent temporarily stored in the elution agent recycling tank 19 enters the nano-scale lithium carbonate synthesis equipment 7 through an elution agent recycling pump 24 for recycling;
5) a drying procedure: the filter cake washed in the step 2) is added into a flash dryer 26 through a dryer dosing device 25, dried at the temperature of 180-220 ℃, and dedusted through a bag-type deduster 27.
The particle size of the nano lithium carbonate prepared by the experiment is 80 nm, and the purity is 99.5-99.7%.
Example 2
1) A reaction process: firstly, 5000L of water is added into impurity removing equipment 2 through a flow controller 29, then lithium sulfate is added into the impurity removing equipment 2 through a lithium salt quantitative feeding device 1, then 34 percent of liquid alkali is added, the final concentration is 0.002 mol/L for impurity removing reaction, the reactant is filtered by a residue filtering device 3, the filtered solution enters a lithium solution synthesizing device 5, sodium carbonate is added into a lithium solution synthesis device 5 through a carbonate quantitative feeding device 4, stirring is started, the concentration of the sodium carbonate is 0.1 mol/L, the concentration of the lithium sulfate is 0.1 mol/L, performing lithium solution synthesis reaction at the normal temperature of 20 ℃, pumping the lithium solution into nano-scale lithium carbonate synthesis equipment 7 through a lithium solution transfer pump 6, simultaneously adding 25000L of solvent-out agent ethylene glycol, carrying out elution reaction at normal temperature, and after the reaction is finished, enabling the nano lithium carbonate slurry to enter a filtering and washing process through a lithium carbonate transfer pump 8;
2) a filtering and washing procedure: the nanometer lithium carbonate slurry enters a lithium carbonate washing and filtering device 9 for filtering, filtrate and a lithium carbonate filter cake are filtered out, the filtrate enters a filtrate tank 10, the filter cake is washed by water for five times to obtain a lithium carbonate wet material, and the lithium carbonate wet material enters a drying procedure;
3) and (3) separating by-products: adding the filtrate in the filtrate tank 10 into a drying reaction device 14 through a flow controller 29, simultaneously adding a calcium oxide desiccant through a desiccant quantitative feeding device 13, wherein the final concentration of calcium oxide is 0.1 mol/L, performing drying reaction at room temperature, adding the solution into a first filtering device 15 for solid-liquid separation after the desiccant is completely added, filtering to obtain calcium sulfate, temporarily storing the separated liquid in a crystallization evaporation feeding tank 16, heating the separated liquid in a crystallization evaporation heater 17 at a heating temperature of 130 ℃, then evaporating the heated liquid in an evaporator 18, circularly evaporating the heated liquid by a circulating pump, and filtering the slurry subjected to evaporation crystallization by a second filtering device 20 to separate sodium hydroxide and a dissolving agent;
4) recycling of distilled water and a leaching agent: steam at the top of the evaporator 18 is condensed by a steam condenser 21 and temporarily stored by a distilled water recycling tank 22, and the distilled water enters the lithium carbonate washing and filtering device 9 through a distilled water recycling pump 23 for water washing; the elution agent temporarily stored in the elution agent recycling tank 19 enters the nano-scale lithium carbonate synthesis equipment 7 through an elution agent recycling pump 24 for recycling;
5) a drying procedure: the filter cake washed in the step 2) is added into a flash dryer 26 through a dryer dosing device 25, then is dried at the temperature of 180-220 ℃, and finally is dedusted through a bag-type deduster 27.
The particle size of the nano lithium carbonate prepared by the experiment is 150 nm, and the purity can reach 99.9%.
Example 3
1) A reaction process: firstly, 10000L of water is added into impurity removing equipment 2 through a flow controller 29, then lithium sulfate is added into the impurity removing equipment 2 through a lithium salt quantitative feeding device 1, then 34 percent of liquid alkali is added, the final concentration is 0.008 mol/L for impurity removal reaction, the reactant is filtered by a residue filtering device 3, the filtered solution enters a lithium solution synthesizing device 5, sodium carbonate is added into a lithium solution synthesis device 5 through a carbonate quantitative feeding device 4, stirring is started, the concentration of the sodium carbonate is 0.4 mol/L, the concentration of the lithium sulfate is 0.4 mol/L, performing lithium solution synthesis reaction at the normal temperature of 20 ℃, pumping the lithium solution into nano-scale lithium carbonate synthesis equipment 7 through a lithium solution transfer pump 6, simultaneously adding 10000L of solvent-out agent glycerol, carrying out elution reaction at normal temperature, and after the reaction is finished, enabling the nano lithium carbonate slurry to enter a filtering and washing process through a lithium carbonate transfer pump 8;
2) a filtering and washing procedure: the nanometer lithium carbonate slurry enters a lithium carbonate washing and filtering device 9 for filtering, filtrate and a lithium carbonate filter cake are filtered out, the filtrate enters a filtrate tank 10, the filter cake is washed by water for five times to obtain a lithium carbonate wet material, and the lithium carbonate wet material enters a drying procedure;
3) and (3) separating by-products: adding the filtrate in the filtrate tank 10 into a drying reaction device 14 through a flow controller 29, simultaneously adding a calcium oxide desiccant through a desiccant quantitative feeding device 13, wherein the final concentration of calcium oxide is 0.4 mol/L, performing drying reaction at room temperature, adding the solution into a first filtering device 15 for solid-liquid separation after the desiccant is completely added, filtering to obtain calcium sulfate, temporarily storing the separated liquid in a crystallization evaporation feeding tank 16, heating the separated liquid in a crystallization evaporation heater 17 at a heating temperature of 130 ℃, then evaporating the heated liquid in an evaporator 18, circularly evaporating the heated liquid by a circulating pump, and filtering the slurry subjected to evaporation crystallization by a second filtering device 20 to separate sodium hydroxide and a dissolving agent;
4) recycling of distilled water and a leaching agent: steam at the top of the evaporator 18 is condensed by a steam condenser 21 and temporarily stored by a distilled water recycling tank 22, and the distilled water enters the lithium carbonate washing and filtering device 9 through a distilled water recycling pump 23 for water washing; the elution agent temporarily stored in the elution agent recycling tank 19 enters the nano-scale lithium carbonate synthesis equipment 7 through an elution agent recycling pump 24 for recycling;
5) a drying procedure: the filter cake washed in the step 2) is added into a flash dryer 26 through a dryer dosing device 25, then is dried at the temperature of 180-220 ℃, and finally is dedusted through a bag-type deduster 27.
The particle size of the nano lithium carbonate prepared by the experiment is 100 nm, and the purity is 99.8%.
Claims (10)
1. The device for producing the high-purity nano lithium carbonate is characterized by comprising a synthesis reaction module, a filtering and washing module, a separation module, a distilled water recycling module and a drying module; the synthesis reaction module and the filtering and washing module are connected to form a circulation loop, the filtering and washing module is sequentially connected with the separation module and the synthesis reaction module to form a circulation loop, the separation module is connected with the distilled water recycling module, the distilled water recycling module is connected with the filtering and washing module, and the filtering and washing module is connected with the drying module;
the synthesis reaction module is used for reacting and synthesizing the nano lithium carbonate, the filtering and washing module is used for carrying out solid-liquid separation and filter cake washing on the synthesized nano lithium carbonate slurry, and the separation module is used for separating and processing the filtrate and recovering the elution agent for producing the nano lithium carbonate.
2. The apparatus for producing high-purity nano lithium carbonate according to claim 1, wherein the synthesis reaction module comprises a lithium salt dosing device (1), an impurity removing device (2), a residue filtering device (3), a carbonate dosing device (4), a lithium solution synthesizing device (5), a lithium solution transferring pump (6), a nano lithium carbonate synthesizing device (7) and a lithium carbonate transferring pump (8); lithium salt dosing device (1) is connected with edulcoration equipment (2), edulcoration equipment (2) are connected with residue filtration equipment (3) through the pump, residue filtration equipment (3) are connected with lithium solution synthesis equipment (5), carbonate dosing device (4) are connected with lithium solution synthesis equipment (5), lithium solution synthesis equipment (5) are passed through lithium solution and are expected pump (6) and be connected with nanometer lithium carbonate synthesis equipment (7), nanometer lithium carbonate synthesis equipment (7) are passed through lithium carbonate and are expected pump (8) and are filtered the washing module and be connected.
3. The apparatus for producing high-purity nano lithium carbonate according to claim 2, wherein the filtering and washing module comprises a lithium carbonate washing and filtering device (9), a filtrate tank (10), a plurality of washing water tanks (11) and a plurality of corresponding washing water recycling pumps (12), the lithium carbonate transferring pump (8) is connected with the lithium carbonate washing and filtering device (9), the lithium carbonate washing and filtering device (9) is used for separating filter cakes and filtrate of the synthesized nano lithium carbonate slurry and washing the filter cakes, the front end of the lithium carbonate washing and filtering device (9) is connected with the filtrate tank (10), the rear end of the lithium carbonate washing and filtering device is connected with the plurality of washing water tanks (11), the outlet of the filtrate tank (10) is connected with the separation module, the washing water tank (11) used for collecting washing water after primary washing and recycling of the filter cakes is connected with the impurity removing device (2) through the washing water pump (12) to form a circulation loop, and the washing water tank (11) for collecting the washing water after the filter cake post-washing is connected with the lithium carbonate washing and filtering equipment (9) through connecting the respective washing water recycling pump (12) to form a circulating washing system, and a discharge hole of the lithium carbonate washing and filtering equipment (9) is connected with the drying module.
4. The apparatus for producing high-purity nano lithium carbonate according to claim 3, wherein the separation module comprises a desiccant dosing device (13), a drying reaction device (14), a first filtering device (15), a crystallization evaporation feeding tank (16), a crystallization evaporation heater (17), an evaporator (18), a elutriation agent recycling tank (19) and a second filtering device (20), the desiccant dosing device (13) is connected with the drying reaction device (14), the drying reaction device (14) is connected with the first filtering device (15) through a pump, the first filtering device (15) is connected with the crystallization evaporation feeding tank (16), a bottom pipeline of the crystallization evaporation heater (17) is divided into two pipelines, one pipeline is connected with the crystallization evaporation feeding tank (16) through the pump, the other pipeline is connected with a bottom outlet of the evaporator (18) through a circulating pump, the top outlet of the crystallization evaporation heater (17) is connected with the evaporator (18) through a pipeline to form a circulation loop, and the top of the evaporator (18) is connected with the distilled water recycling module through a pipeline; a pipeline which is connected with the bottom outlet of the evaporator (18) and the circulating pump is divided into a pipeline which is sequentially connected with a second filtering device (20) and a dissolving agent recycling tank (19), and the dissolving agent recycling tank (19) is connected with the nano-scale lithium carbonate synthesizing device (7) through a dissolving agent recycling pump (24).
5. The apparatus for producing high-purity nano lithium carbonate according to claim 4, wherein the distilled water recycling module comprises a steam condenser (21), a distilled water recycling tank (22) and a distilled water recycling pump (23), the top of the evaporator (18) is connected with the steam condenser (21) through a pipeline, the outlet of the steam condenser (21) is sequentially connected with the distilled water recycling tank (22) and the distilled water recycling pump (23), and the distilled water recycling pump (23) is connected with the lithium carbonate washing and filtering device (9).
6. The apparatus for producing high-purity nano lithium carbonate according to claim 5, wherein the drying module comprises a dryer dosing device (25), a flash dryer (26), a bag-type dust remover (27) and an induced draft fan (28), the discharge port of the lithium carbonate washing and filtering device (9) is connected with the dryer dosing device (25), the dryer dosing device (25) is connected with the flash dryer (26), and the outlet of the flash dryer (26) is sequentially connected with the bag-type dust remover (27) and the induced draft fan (28).
7. The apparatus for producing high-purity nano lithium carbonate according to claim 5, wherein a flow controller (29) is arranged on a connecting pipeline between the washing water recycling pump (12) and the impurity removing device (2), a connecting pipeline between the eluent recycling pump (24) and the nano lithium carbonate synthesizing device (7), a connecting pipeline between the filtrate tank (10) and the drying reaction device (14), and a connecting pipeline between the crystallization evaporation feed tank (16) and the crystallization evaporation heater (17).
8. The process for producing high-purity nano lithium carbonate according to claim 6, which comprises the steps of:
1) a reaction process: firstly, adding water into impurity removal equipment (2) through a flow controller (29), starting stirring, adding lithium salt into the impurity removal equipment (2) through a lithium salt quantitative feeding device (1), then adding liquid alkali into the impurity removal equipment (2) through the flow controller (29), carrying out impurity removal reaction, filtering and deslagging an obtained solution through residue filtering equipment (3), and then feeding the obtained solution into lithium solution synthesis equipment (5); adding carbonate into lithium solution synthesis equipment (5) through a carbonate quantitative feeding device (4), carrying out lithium solution synthesis reaction at 20 ℃, pumping the reacted lithium solution into nano lithium carbonate synthesis equipment (7) through a lithium solution transfer pump (6), simultaneously adding a elution agent through a flow controller (29), carrying out elution reaction at 20 ℃, and feeding the reacted lithium carbonate slurry into a washing process through a lithium carbonate transfer pump (8);
2) a filtering and washing procedure: the nano lithium carbonate slurry enters lithium carbonate washing and filtering equipment (9) for filtering, filtrate and a lithium carbonate filter cake are filtered, the filtrate enters a filtrate tank (10), the filter cake is washed for multiple times to obtain a lithium carbonate wet material, and the lithium carbonate wet material enters a drying process;
3) and (3) separating by-products: adding filtrate in a filtrate tank (10) into a drying reaction device (14) through a flow controller (29), simultaneously adding a drying agent through a drying agent quantitative feeding device (13), carrying out drying reaction at room temperature, adding the solution into a first filtering device (15) for solid-liquid separation after the drying agent is completely added, filtering to obtain calcium sulfate, temporarily storing the separated liquid in a crystallization evaporation feeding tank (16), heating the separated liquid in a crystallization evaporation heater (17), heating the heated separated liquid in an evaporator (18) for evaporation, circularly evaporating by a circulating pump, filtering the evaporated and crystallized slurry through a second filtering device (20), and separating sodium hydroxide and a dissolving agent;
4) recycling of distilled water and a leaching agent: steam at the top of the evaporator (18) is condensed by a steam condenser (21) and temporarily stored by a distilled water recycling tank (22), and the distilled water enters lithium carbonate washing and filtering equipment (9) through a distilled water recycling pump (23) for washing; the elution agent temporarily stored in the elution agent recycling tank (19) enters the nano-scale lithium carbonate synthesis equipment (7) through an elution agent recycling pump (24) for recycling;
5) a drying procedure: and (3) adding the filter cake washed in the step 2) into a flash evaporation dryer (26) through a dryer dosing device (25) for drying, and removing dust through a bag-type dust remover (27).
9. The process for producing high-purity nano lithium carbonate according to claim 8, wherein the elution solvent in step 1) is at least one of diol, triol or sulfoxide; the dihydric alcohol comprises at least one of ethylene glycol and propylene glycol, the trihydric alcohol comprises at least one of glycerol and butanetriol, and the sulfoxide comprises at least one of dimethyl sulfoxide and diethyl sulfoxide.
10. The process for producing high-purity nano lithium carbonate according to claim 8, wherein the lithium salt is lithium sulfate, the carbonate is sodium carbonate, the caustic soda is 34% of industrial common caustic soda, the drying agent is calcium oxide, the concentration of lithium sulfate is 0.1-1 mol/L, the concentration of sodium carbonate is 0.1-1 mol/L, the feeding molar ratio of calcium oxide to lithium sulfate to sodium carbonate is 1:1, and the feeding volume ratio of the leaching agent to water is 0.1-5: 1.
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