CN102408120A - Method for preparing high-purity ultrafine lithium-carbonate micro powder - Google Patents
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- CN102408120A CN102408120A CN2010102876962A CN201010287696A CN102408120A CN 102408120 A CN102408120 A CN 102408120A CN 2010102876962 A CN2010102876962 A CN 2010102876962A CN 201010287696 A CN201010287696 A CN 201010287696A CN 102408120 A CN102408120 A CN 102408120A
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Abstract
The invention relates to a method for preparing high-purity ultrafine lithium-carbonate micro powder, which is characterized in that primary lithium carbonate (purity: less than 95%) and CO2 gas are taken as raw materials, and through adopting a new efficient carbonization device, the insoluble lithium carbonate is converted into large-solubility lithium bicarbonate; and after a lithium bicarbonate solution is purified, in a spray drying device, the decomposition of the lithium bicarbonate solution and the crystallization and drying of the lithium carbonate are completed in one step, and then an ultrafine lithium-carbonate micro powder product is directly obtained. The method disclosed by the invention has the advantages that the method is simple in process, excellent in product, stable in quality, high in recovery rate and convenient for industrialization; the prepared ultrafine lithium-carbonate micro powder has a porous hollow sphere structure (D0.5 can be less than 5 microns) formed by carrying out self-assembling on lithium-carbonate crystalline granules (about 200 nm); the BET specific surface area of the ultrafine lithium-carbonate micro powder can reach 7 m<2>/g, which is far higher than that of a product prepared by using the existing method, therefore, the method has a strong application value in the industries such as lithium ion batteries and the like.
Description
[technical field]
The present invention relates to the Quilonum Retard technical field, specifically, is a kind of method for preparing the pure Lithium Carbonate ultra-fine micropowder.
[background technology]
As basic lithium salts, Quilonum Retard all has a wide range of applications in industries such as glass, pottery, aluminium metallurgy, information, nuclear industry, medicine.It also is a main raw material of making metallic lithium and isotropic substance thereof, various meticulous lithium salts (lithium molybdate, Lithium Hydroxide MonoHydrate, lithiumbromide etc.).Highly purified Quilonum Retard (greater than 99.9%) is the requisite of lithium ion battery, magneticsubstance, electronic material and opticinstrument; After getting into 21 century; Along with the high speed development of new forms of energy industry and information industry, growing to the demand of pure Lithium Carbonate both at home and abroad.Therefore, highly purified Quilonum Retard just more and more receives publicity, and powerful growth momentum is arranged.
Some high-tech applications are except Quilonum Retard purity there being strict requirement, to Quilonum Retard particulate granularity and the also very high requirement of pattern.Such as, in recent years, along with highlighting day by day of energy problem, the development of lithium ion battery, especially power-type lithium ion battery is in the ascendant.Quilonum Retard is the main raw material of anode material for lithium-ion batteries (lithium manganate, cobalt acid lithium, iron lithium phosphate etc.); Quilonum Retard joins in the battery as the additive of electrolytic solution, can improve the film forming properties of battery, thereby improves the cycle performance and the low temperature performance of battery.Battery carbon acid lithium will satisfy the requirement of two aspects at least: at first Quilonum Retard will have very high purity, and secondly the granularity of Quilonum Retard is as much as possible little.
The preparation method of pure Lithium Carbonate mainly comprises Zint1-Harder-Dauth method, recrystallization method, the causticization precipitator method, carbonization decomposition method or the like.Wherein, the carbonization decomposition method is expected most, and this method raw material is relatively inexpensive to be easy to get, and technology is simple, process environmental protection, the Li that makes
2CO
3Particle diameter is big, and the recovery is high, has higher operation possibility.It mainly comprises carbonization process and thermal decomposition process, and its principle can be expressed as:
Li
2CO
3+CO
2+H
2O→2LiHCO
3
2LiHCO
3→Li
2CO
3↓+CO
2↑+H
2O
Its main technique flow process is following.Elementary Li
2CO
3(purity is less than 95%) is mixed into aqueous solution slip with deionized water, under condition of stirring, to wherein leading to the high-purity CO of people
2Gas.Control suitable temperature of reaction, stirring velocity and CO
2Feeding speed, control the suitable reaction times, change the Quilonum Retard of indissoluble into solubleness bigger lithium bicarbonate.Filter slip then to remove insoluble impurity.The impurity that is dissolved in the filtrating can be removed through methods such as IX and extractions.Lithia water after in another reactor drum, adding thermal purification, constant temperature stir removes CO
2Gas, lithium bicarbonate will decompose deposition and generate Li
2CO
3Through cooling, filter out deposition again, oven dry obtains highly purified Li under suitable temperature then
2CO
3Product.
Current, all there are certain defective in the carbonization technique of carbonization decomposition method and thermal decomposition process, need further to improve.As far as carbonization process, at present main application machine steel basin carries out carbonization, in order to enhance productivity, just increases working pressure.Adopt higher pressure exerting device to carry out carbonization, increased facility investment and process cost, be not easy to production control and continuous operation.Theoretical according to gas liquid reaction; Partial pressure and liquid-gas interface are the important factors that influences body series gas liquid reaction speed; Thereby can increase liquid-gas interface through the form of improving gas-liquid reactor (carbonizer), to reach the higher carbonization efficient of acquisition under the moderate pressure condition.As far as thermal decomposition process, pyrolysis carries out in the heated and stirred still, Li
2CO
3Particle is assembled seriously each other, and granularity is bigger, is not easy to direct application, must be through pulverizing the demand to lithium carbonate product such as the industry that could satisfy lithium ion battery.In the pyrolysis process, Li
2CO
3The crystal wall sticking phenomenon is very serious, and the generation of brilliant dirt has reduced heat transfer efficiency and production efficiency, has increased energy consumption and cleaning maintenance cost.
Obtain the method for fine granularity Quilonum Retard in the prior art, mainly comprise mechanical crushing method, solid phase method, mixed phase method, liquid phase method (precipitator method) and vapor phase process.But prior art still mainly relies on disintegrating apparatus to realize to the control of Quilonum Retard the finished product granularity.
CN 1267636A discloses a kind of preparation method of sulfuric acid process to produce battery-level lithium carbonate.Its production technique is that make the transition roasting, acidizing fired, leaching, purifying treatment, concentration, sinker processing, cleaning, drying treatment, pulverizing, packaged for processing of lithium concentrate formed.This method is raw material with the lithium concentrate, but then may not be suitable for the lithium resource that exists with the salt lake brine form.Although the purity of the Quilonum Retard that is obtained by this method can satisfy the requirement of battery, obviously this method is very loaded down with trivial details, production technique is too complicated, and because the restriction of disintegrating apparatus grindability, the granularity of the Quilonum Retard primary particle that obtains is a micron order.
CN 101209846A discloses a kind of preparation method of nano-scale lithium carbonate for battery, and this method is included in the aqueous solution, with Lithium Hydroxide MonoHydrate or water-soluble lithium salts and carbonic acid gas or water soluble carbonate contact reacts.Contact reacts is carried out in the presence of dispersion agent, and said dispersion agent is water soluble anionic surfactant and/or the organic amine that has carboxylic acid ester groups and/or sulfonate group.This method can access the granularity of thinner Quilonum Retard, but this method is higher to the purity requirement of feed hydrogen Lithium Oxide 98min or water-soluble lithium salts; Operational cycle very long (the gas liquid reaction time in the specific embodiment that CN101209846A provides generally reaches 20-40 hour, and digestion time reaches 24 hours, reaches 48 hours time of drying); In the gas-liquid reaction process, Quilonum Retard is assembled the obstruction vent line easily; And the gained lithium carbonate product still need pass through subsequent disposal such as filtration, washing, drying.
So research purpose of the present invention is sought a kind of advantages of simplicity and high efficiency process method for to be the basis with carbonization decomposition method principle, preparation pure Lithium Carbonate ultra-fine micropowder is to satisfy the demand of industry such as lithium ion battery to high-end lithium carbonate product.
[summary of the invention]
The objective of the invention is to overcome the deficiency of prior art, a kind of method for preparing the pure Lithium Carbonate ultra-fine micropowder is provided.
The objective of the invention is to realize through following technical scheme:
A kind of method for preparing the pure Lithium Carbonate ultra-fine micropowder is characterized in that, concrete steps are: with first level lithium carbonate and CO
2Gas is raw material, adopts new and effective carbonizing apparatus, replaces traditional mechanical agitating tank to carry out carbonization, changes the Quilonum Retard of indissoluble into solubleness bigger lithium bicarbonate; Remove insoluble impurities through filtering slip, remove the foreign ion that is dissolved in the filtrating through IX; The decomposition drying process of the lithia water after the purification, in spray drying device, a step accomplishes, and directly obtains Quilonum Retard ultra-fine micropowder product; Do not need further processing treatment.Rather than as traditional technology, thermal degradation lithia water in stirring tank obtains the Quilonum Retard post precipitation again through subsequent operationss such as filtration, washing, drying, pulverizing.
The preparation method of pure Lithium Carbonate ultra-fine micropowder provided by the invention is a raw material with first level lithium carbonate; If just the level lithium carbonate crystal size is bigger, in order to obtain higher carbonization efficient, can the Quilonum Retard raw material be carried out pulverization process, breaking method can be ball mill pulverizing, comminution by gas stream and sonicated or the like.
In carbonizing apparatus, elementary lithium carbonate aqueous solution slip and CO
2Gas carries out carburizing reagent and generates lithium bicarbonate; CO
2Gas and Li
2CO
3Carburizing reagent in the aqueous solution is the gas-liquid-solid phase reaction process that a mass transfer process and chemical reaction process carry out simultaneously, and the essence of reaction is still the ionic reaction in the aqueous solution, and critical step is exactly CO
2The dissolving of gas and Li
2CO
3Mass transfer process; The factor that influences carburizing reagent is a lot, like Li
2CO
3The temperature of the massfraction of slurries (solid-to-liquid ratio of reaction), reaction, the speed, the CO that have or not stirring and stir
2Dividing potential drop, reaction times etc.
The present invention selects for use new and effective carbonizing apparatus to strengthen carburizing reagent, improves carburizing reagent speed and CO
2Utilization ratio; Comprise falling-film tower (wet-wall tower), spray tower, bubble tower and rotating disk (rotation film) reactor drum; Working pressure is 0～1.0Mpa, and service temperature is 5～65 ℃; [Li+] concentration should be more than 0.5mol/L during the carbonization terminal point.Because the liquid-gas interface of the carbonizing apparatus that falling-film tower (wet-wall tower) etc. are new and effective is more much higher than mechanical agitating tank, so under the same operation condition, its carbonization efficiency far is higher than mechanical agitating tank.
Slip after the carbonization is filtered, remove insoluble impurities, like molysite, silico-aluminate or the like; With filtrating successively through anion and cation exchange resin with foreign ions such as the calcium of removing solubility wherein, magnesium.
Lithia water after purifying is transported in the spray drying device, sprays and decompose drying, service temperature is 60～600 ℃; Spray drying device of the present invention does not have special demands to spray pattern, and no matter form such as air-flowing type, centrifugal still ultrasonic type as long as spray droplet is enough little, all can obtain satisfactory product.
The prepared Quilonum Retard micro mist of the present invention has porous hollow spherical structure (D
0.5Can be as small as below 5 microns), its secondary structure is about 200 nano-calcium carbonate crystalline lithium particles; The BET specific surface area of this Quilonum Retard micro mist can reach 7m
2More than/the g, (the highest BET specific surface area of having reported is 2.79m to be higher than the specific surface area that has the prepared product of method far away
2/ g), have very strong using value.
Compared with prior art, positively effect of the present invention is:
Method provided by the present invention, technology is simple, product fine, steady quality, the recovery is high, is convenient to industriallization.
[description of drawings]
Fig. 1 normal pressure descending film absorbs the carbonization Experimental equipment;
Fig. 2 ion exchange unit figure;
Fig. 3 sprays and decomposes drying installation figure;
Fig. 4 sprays and decomposes drying prods XRD spectra and the comparison of standard spectrogram;
Fig. 5 a, the drying prods pattern is decomposed in the 5b spraying;
Fig. 6 sprays and decomposes the drying prods size-grade distribution;
Mark in the accompanying drawing is respectively: 1, CO
2Steel cylinder, 2, film-falling absorption tower, 3, recycle pump, 4, mechanical stirring, 5, steel basin, 6, thermostatic bath, 7, anion-exchange column, 8, cationic exchange coloum, 9, transferpump, 10, heating chamber, 11, the product receiving flask.
[embodiment]
The present invention below is provided a kind of embodiment for preparing the method for pure Lithium Carbonate ultra-fine micropowder.
Present embodiment comprises that mainly Quilonum Retard carbonization, lithia water purify and dry three steps are decomposed in the lithia water spraying:
(1) Quilonum Retard carburising step: the present embodiment operation adopts falling-film tower (wet-wall tower) to carry out carbonization, and concrete experimental installation is seen Fig. 1.Operation steps is following: in the tower still, add 300～500ml deionized water, open mechanical stirring, recycle pump and water bath with thermostatic control.Stirring velocity is 0～1000rpm, and the liquid circulation flow is: 0.1～10L/min.When the deionized water homo(io)thermism is 5～55 ℃, add 10～50g Li
2CO
3Powder is opened CO
2Steel cylinder picks up counting.At 0.2～2L/min, falling-film tower (wet-wall tower) working pressure is a normal pressure through pressure maintaining valve and gas meter adjustments of gas apparent velocity., lithium concentration stops carburizing reagent when reaching requirement;
(2) lithium bicarbonate purifying step: the slip after the carbonization is filtered, remove insoluble impurities.With filtrating successively through the yin, yang ion exchange column to remove the wherein foreign ion (see figure 2) of solubility;
(3) drying step is decomposed in spraying: the lithia water after will purifying is transported in the spray drying device, sprays and decomposes drying, and service temperature is 60-560 ℃.Directly obtain Quilonum Retard ultra-fine micropowder product (see figure 3).
Product characterizes:
Adopt X-ray diffraction analysis (XRD) that the product of the pure Lithium Carbonate ultra-fine micropowder of present embodiment preparation has been carried out structural characterization.Its XRD figure spectrum (see figure 4) and Quilonum Retard standard x RD collection of illustrative plates are identical.
Adopt scanning electron microscope (SEM) that the product of the pure Lithium Carbonate ultra-fine micropowder of present embodiment preparation has been carried out the pattern sign and (see Fig. 5 a, 5b).The SEM pictorial display, the Quilonum Retard micro mist has the porous hollow spherical structure, and its secondary structure is the Quilonum Retard crystal grain of rice in about 200.
(Mastersizer 2000, and Malvren UK) has carried out granularity to the product of originally executing the routine pure Lithium Carbonate ultra-fine micropowder for preparing and characterized (see figure 6), D to adopt the Ma Erwen particle-size analyzer
0.5It is 4.00 microns.What it should be noted that the reflection of these particle size distribution figures only is the information of macroscopical hollow ball, and the small crystalline dimension information of secondary structure must depend on instruments such as ESEM, transmission electron microscope and observes.
(TriStar 3000, and Micromeritics US) has carried out the specific surface area sign to the product of originally executing the routine pure Lithium Carbonate ultra-fine micropowder for preparing to adopt BET specific surface area analysis appearance.The BET specific surface area is 7.24m
2More than/the g, (the highest BET specific surface area of having reported is 2.79m to be higher than the specific surface area that has the prepared product of method far away
2/ g).
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the present invention's design; Can also make some improvement and retouching, these improvement and retouching also should be regarded as in protection scope of the present invention.
Claims (6)
1. a method for preparing the pure Lithium Carbonate ultra-fine micropowder is characterized in that, concrete steps are: with first level lithium carbonate and CO
2Gas is raw material, adopts carbonizing apparatus, changes the Quilonum Retard of indissoluble into solubleness bigger lithium bicarbonate; Remove insoluble impurities through filtering slip, remove the foreign ion that is dissolved in the filtrating through IX; The decomposition drying process of the lithia water after the purification, in spray drying device, a step accomplishes, and directly obtains Quilonum Retard ultra-fine micropowder product.
2. a kind of method for preparing the pure Lithium Carbonate ultra-fine micropowder as claimed in claim 1 is characterized in that described Quilonum Retard raw material carries out pulverization process, and breaking method is ball mill pulverizing, comminution by gas stream and sonicated.
3. a kind of method for preparing the pure Lithium Carbonate ultra-fine micropowder as claimed in claim 1 is characterized in that, in carbonizing apparatus, and elementary lithium carbonate aqueous solution slip and CO
2Gas carries out carburizing reagent and generates lithium bicarbonate.
4. a kind of method for preparing the pure Lithium Carbonate ultra-fine micropowder as claimed in claim 1 is characterized in that described carbonizing apparatus comprises falling-film tower, spray tower, bubble tower, rotating disk reactor drum; Working pressure is 0～1.0Mpa, and service temperature is 5～65 ℃; [Li during the carbonization terminal point
+] concentration should be more than 0.5mol/L.
5. a kind of method for preparing the pure Lithium Carbonate ultra-fine micropowder as claimed in claim 1; It is characterized in that, in spray drying device, the lithia water after purifying is transported in the spray drying device; Spraying, it is dry to decompose, and service temperature is 60～600 ℃.
6. a kind of method for preparing the pure Lithium Carbonate ultra-fine micropowder as claimed in claim 1 is characterized in that described Quilonum Retard micro mist has the porous hollow spherical structure, and its secondary structure is 200 nano-calcium carbonate crystalline lithium particles, and its BET specific surface area can reach 7m
2More than/the g.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539169A (en) * | 2013-10-24 | 2014-01-29 | 中国地质科学院郑州矿产综合利用研究所 | Method for preparing battery-grade lithium carbonate or high-purity lithium carbonate by using industrial-grade lithium carbonate |
| CN106430260A (en) * | 2016-12-13 | 2017-02-22 | 宜春银锂新能源有限责任公司 | Method for preparing high-purity lithium carbonate from Lizhimu |
| CN106517259A (en) * | 2016-12-19 | 2017-03-22 | 天齐锂业股份有限公司 | Spherical lithium carbonate and preparation method thereof |
| CN108011150A (en) * | 2017-12-28 | 2018-05-08 | 许昌学院 | A kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder |
| CN110563009A (en) * | 2019-09-29 | 2019-12-13 | 华东理工大学 | Method for preparing battery-grade lithium carbonate from fly ash by carbonization decomposition method |
| CN110817908A (en) * | 2018-08-13 | 2020-02-21 | 中国石油化工股份有限公司 | System and method for preparing high-purity lithium carbonate by using lithium-containing waste material |
| CN111439761A (en) * | 2020-02-19 | 2020-07-24 | 江西赣锋锂业股份有限公司 | Method for preparing high-purity lithium carbonate through continuous carbonization and decomposition |
| CN111547734A (en) * | 2020-05-11 | 2020-08-18 | 蒋达金 | Preparation method of carbon-doped lithium iron borate |
| CN112479235A (en) * | 2020-12-23 | 2021-03-12 | 江苏容汇通用锂业股份有限公司 | Preparation method of hollow spherical lithium carbonate |
| CN113636577A (en) * | 2021-08-25 | 2021-11-12 | 金川集团股份有限公司 | Preparation method of low-magnetism spherical high-purity lithium carbonate |
| CN114368765A (en) * | 2021-08-20 | 2022-04-19 | 山东泰普锂业科技有限公司 | Morphology control process and method of lithium carbonate nanosheet with smooth surface for lithium supplement of positive electrode in lithium ion battery |
| CN115321564A (en) * | 2022-08-31 | 2022-11-11 | 天齐创锂科技(深圳)有限公司 | Long rod-shaped lithium carbonate and preparation method thereof |
| CN115784190A (en) * | 2022-11-30 | 2023-03-14 | 湖北万润新能源科技股份有限公司 | Preparation method of lithium iron phosphate |
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| CN103539169A (en) * | 2013-10-24 | 2014-01-29 | 中国地质科学院郑州矿产综合利用研究所 | Method for preparing battery-grade lithium carbonate or high-purity lithium carbonate by using industrial-grade lithium carbonate |
| CN106430260A (en) * | 2016-12-13 | 2017-02-22 | 宜春银锂新能源有限责任公司 | Method for preparing high-purity lithium carbonate from Lizhimu |
| CN106517259A (en) * | 2016-12-19 | 2017-03-22 | 天齐锂业股份有限公司 | Spherical lithium carbonate and preparation method thereof |
| CN106517259B (en) * | 2016-12-19 | 2018-07-10 | 天齐锂业股份有限公司 | A kind of spherical Lithii carbonate and preparation method thereof |
| CN108011150A (en) * | 2017-12-28 | 2018-05-08 | 许昌学院 | A kind of method that lithium carbonate is produced from waste and old ternary lithium ion cell electrode powder |
| CN110817908A (en) * | 2018-08-13 | 2020-02-21 | 中国石油化工股份有限公司 | System and method for preparing high-purity lithium carbonate by using lithium-containing waste material |
| CN110563009A (en) * | 2019-09-29 | 2019-12-13 | 华东理工大学 | Method for preparing battery-grade lithium carbonate from fly ash by carbonization decomposition method |
| CN111439761A (en) * | 2020-02-19 | 2020-07-24 | 江西赣锋锂业股份有限公司 | Method for preparing high-purity lithium carbonate through continuous carbonization and decomposition |
| CN111547734A (en) * | 2020-05-11 | 2020-08-18 | 蒋达金 | Preparation method of carbon-doped lithium iron borate |
| CN112479235A (en) * | 2020-12-23 | 2021-03-12 | 江苏容汇通用锂业股份有限公司 | Preparation method of hollow spherical lithium carbonate |
| CN114368765A (en) * | 2021-08-20 | 2022-04-19 | 山东泰普锂业科技有限公司 | Morphology control process and method of lithium carbonate nanosheet with smooth surface for lithium supplement of positive electrode in lithium ion battery |
| CN114368765B (en) * | 2021-08-20 | 2023-09-22 | 山东泰普锂业科技有限公司 | Morphology control method of smooth-surface lithium carbonate nanosheets for lithium supplementing of positive electrode in lithium ion battery |
| CN113636577A (en) * | 2021-08-25 | 2021-11-12 | 金川集团股份有限公司 | Preparation method of low-magnetism spherical high-purity lithium carbonate |
| CN115321564A (en) * | 2022-08-31 | 2022-11-11 | 天齐创锂科技(深圳)有限公司 | Long rod-shaped lithium carbonate and preparation method thereof |
| CN115321564B (en) * | 2022-08-31 | 2024-01-30 | 天齐创锂科技(深圳)有限公司 | Long rod-shaped lithium carbonate and preparation method thereof |
| CN115784190A (en) * | 2022-11-30 | 2023-03-14 | 湖北万润新能源科技股份有限公司 | Preparation method of lithium iron phosphate |
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