CN107935000A - A kind of method for preparing high-purity ultrafine lithium-carbonate micro powder - Google Patents
A kind of method for preparing high-purity ultrafine lithium-carbonate micro powder Download PDFInfo
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- CN107935000A CN107935000A CN201711384872.2A CN201711384872A CN107935000A CN 107935000 A CN107935000 A CN 107935000A CN 201711384872 A CN201711384872 A CN 201711384872A CN 107935000 A CN107935000 A CN 107935000A
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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
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Abstract
The invention discloses a kind of method for preparing high-purity ultrafine lithium-carbonate micro powder, comprise the following steps that：Step 1：The preparation of lithia water；Step 2：The preparation of high-purity ultrafine lithium-carbonate micro powder：Lithia water is added in spray drying device, spraying is carried out and decomposes drying, the temperature of spray drying device is 650~680 DEG C, has just obtained high-purity ultrafine lithium-carbonate micro powder.Preparation method of the invention is simple, cost is low, energy consumption consumption is low, is easy to produce in enormous quantities, its preparation process is easily controllable; raw material is easy to get, and cost is relatively low, suitable for industrialized production; product fine, purity is high, and particle is fine; stable quality; the rate of recovery is high, pollution-free, can good environmental protection; it is safe and non-toxic, can be safe to use.
Description
Technical field
The present invention relates to a kind of method for preparing high-purity ultrafine lithium-carbonate micro powder.
Background technology
Based on lithium salts, lithium carbonate suffers from industries such as glass, ceramics, aluminium metallurgy, information, atomic energy industry, medicine
It is widely applied.It is also manufacture lithium metal and its isotope, various fine lithium salts (lithium molybdate, lithium hydroxide, lithium bromide etc.)
Primary raw material.The lithium carbonate (being more than 99.9%) of high-purity is lithium ion battery, magnetic material, electronic material and optical instrument
Necessity, into after 21 century, with New Energy Industry and the high speed development of information industry, both at home and abroad to pure Lithium Carbonate
Demand is growing.Therefore, the lithium carbonate of high-purity just increasingly attracts attention, and has powerful growth momentum.
Some high-tech applications to lithium carbonate purity except having strict requirements, to the granularity and shape of lithium carbonate particle
Looks also very high requirement.Such as in recent years, with increasingly prominent, the lithium ion battery of energy problem, especially power type lithium from
The development of sub- battery is in the ascendant.Lithium carbonate is the master of anode material for lithium-ion batteries (LiMn2O4, cobalt acid lithium, LiFePO4 etc.)
Want raw material；Lithium carbonate is added in battery as the additive of electrolyte, can improve the filming performance of battery, so as to improve electricity
The cycle performance and low temperature performance in pond.Battery carbon acid lithium requires of both at least meeting：Lithium carbonate will have first
Very high purity, secondly the granularity of lithium carbonate is small as far as possible.
The preparation method of pure Lithium Carbonate mainly include Zint1-Harder-Dauth methods, recrystallization method, caustic precipitation method,
The decomposition method that is carbonized etc..Wherein, carbonization decomposition method is most expected, and the method raw material is relatively inexpensive to be easy to get, and technique is simple, process ring
Protect, obtained Li2CO3 particle diameters are big, and the rate of recovery is high, has higher operation possibility.It mainly include carbonisation and
Thermal decomposition process, its principle can be expressed as：
Li2CO3+CO2+H2O→2LiHCO3
2LiHCO3→Li2CO3↓+CO2↑+H2O
Its technical process is as follows.Primary Li2CO3 (purity is less than 95%) is mixed into water-soluble liquid material with deionized water
Slurry, in the case of stirring, leads to the gas of the high-purity CO2 of people thereto.Control appropriate reaction temperature, mixing speed and CO2
Speed is passed through, controls the appropriate reaction time, the lithium carbonate of indissoluble is changed into the larger lithium bicarbonate of solubility.Then filter
Slurry is to remove insoluble impurity.The impurity being dissolved in filtrate can be removed by the methods of ion exchange and extraction.Another
Purified lithia water is heated in a reactor, constant temperature stirring removes CO2 gases, and lithium bicarbonate will decompose precipitation generation
Li2CO3.Again through cooling, precipitation is filtered out, then drying obtains the Li2CO3 products of high-purity at a proper temperature.
Currently, the carbonization technique and thermal decomposition process for the decomposition method that is carbonized there are it is certain the defects of, need to further improve.It is right
For carbonisation, mainly it is carbonized at present using mechanical agitating tank, in order to improve production efficiency, just increases operating pressure.
It is carbonized using higher pressurized equipment, adds equipment investment and operating cost, is not easy to production control and continuous operation.
Theoretical according to gas liquid reaction, partial pressure and gas-liquid interface be an important factor for influencing body series gas liquid reaction speed, thus can
Increase gas-liquid interface in the form of by improving gas-liquid reactor (carbonizer), with reach under the conditions of moderate pressure obtain compared with
High carbonization efficiency.For thermal decomposition process, pyrolysis carries out in heating stirring kettle, and Li2CO3 particles are assembled each other
Seriously, granularity is larger, is not easy to directly apply, it is necessary to by crushing the industries such as lithium ion battery could be met to lithium carbonate product
Demand.During pyrolysis, Li2CO3 crystal wall sticking phenomenons are extremely serious, the generation of brilliant dirt reduce heat transfer efficiency and
Production efficiency, adds energy consumption and cleaning and maintenance cost.
The method for obtaining fine granularity lithium carbonate in the prior art, mainly including mechanical crushing method, solid phase method, mixed phase method, liquid
Phase method (precipitation method) and vapor phase method.But control of the prior art to lithium carbonate final products granularity still relies primarily on disintegrating apparatus
To realize.CN 1267636A disclose a kind of preparation method of Production By Sulfuric Acid Process battery-level lithium carbonate.Its production technology is by lithium
Concentrate carry out transition roasting, acidizing fired, leaching, purified treatment, concentration, sinker processing, cleaning, drying process, crushing,
Packaging is process.This method may not then be applicable in lithium resource existing in the form of salt lake bittern using lithium concentrate as raw material.To the greatest extent
The purity for the lithium carbonate that pipe is obtained by this method disclosure satisfy that the requirement of battery, it is apparent that this method is very cumbersome, production technology
It is too complicated, and due to the limitation of disintegrating apparatus grindability, the degree of obtained lithium carbonate primary particle is micron order.CN
101209846A discloses a kind of preparation method of nano-scale lithium carbonate for battery, and this method is included in aqueous, by hydrogen-oxygen
Change lithium or water-soluble lithium salts and carbon dioxide or water soluble carbonate haptoreaction.Haptoreaction carries out in the presence of dispersants,
The dispersant is water soluble anionic surfactant and/or organic amine with carboxylic acid ester groups and/or sulfonate group.The party
Method can obtain the granularity of thinner lithium carbonate, but purity requirement of this method to raw material lithium hydroxide or water-soluble lithium salts compared with
It is high；Operation cycle it is very long (CN101209846A provide specific embodiment in the gas liquid reaction time be typically up to 20-40 it is small when,
Digestion time up to 24 it is small when, drying time up to 48 it is small when)；In gas-liquid reaction process, lithium carbonate easily assembles blocking vent line；
And gained lithium carbonate product is still needed by filtering, washing, the subsequent treatment such as drying.So research purpose of the invention
Based on the decomposition method principle that is carbonized, to seek a kind of simple efficient process, high-purity ultrafine lithium-carbonate micro powder is prepared, with
Meets the needs of industries such as lithium ion battery are to high-end lithium carbonate product.
The content of the invention
The purpose of the present invention is overcome the shortcomings of in existing product, there is provided a kind of side for preparing high-purity ultrafine lithium-carbonate micro powder
Method.
In order to achieve the above object, the present invention is achieved by the following technical solutions：
A kind of method for preparing high-purity ultrafine lithium-carbonate micro powder, comprises the following steps that：
Step 1：The preparation of lithia water：First first level lithium carbonate is crushed, primary carbonic acid after then crushing
Lithium is added in reactor, then first is slowly added dropwise untill temperature reaches 90-95 DEG C in heating response device into reactor
Acid, obtains lithium formate solution, and carbon amide solution is then added into lithium formate solution and is passed through carbon dioxide, obtains lithium bicarbonate
Solution；
Step 2：The preparation of high-purity ultrafine lithium-carbonate micro powder：Lithia water is added in spray drying device, into
Drying is decomposed in row spraying, and the temperature of spray drying device is 650~680 DEG C, has just obtained high-purity ultrafine lithium-carbonate micro powder.
Preferably, the method for the crushing is ball mill grinding or air-flow crushing or Ultrasonic Pulverization.
Preferably, the reactor is heated to be heating water bath.
Preferably, the formic acid rate of addition is 6-10d/s.
Preferably, the temperature of the spray drying device is 670 DEG C.
Advantageous effect of the invention is as follows：
Preparation method of the invention is simple, cost is low, energy consumption consumption is low, is easy to produce in enormous quantities, its preparation process is easy to
Control, raw material are easy to get, and cost is relatively low, and high suitable for industrialized production, product fine, purity, particle is fine, stable quality, return
High income, it is pollution-free, can good environmental protection, it is safe and non-toxic, can be safe to use.
Embodiment
Technical scheme is described further below：
Embodiment 1：
A kind of method for preparing high-purity ultrafine lithium-carbonate micro powder, comprises the following steps that：
Step 1：The preparation of lithia water：First first level lithium carbonate is crushed, primary carbonic acid after then crushing
Lithium is added in reactor, then first is slowly added dropwise untill temperature reaches 90-95 DEG C in heating response device into reactor
Acid, obtains lithium formate solution, and carbon amide solution is then added into lithium formate solution and is passed through carbon dioxide, obtains lithium bicarbonate
Solution；
Step 2：The preparation of high-purity ultrafine lithium-carbonate micro powder：Lithia water is added in spray drying device, into
Drying is decomposed in row spraying, and the temperature of spray drying device is 650~680 DEG C, has just obtained high-purity ultrafine lithium-carbonate micro powder.
Preparation method of the invention is simple, cost is low, energy consumption consumption is low, is easy to produce in enormous quantities, its preparation process is easy to
Control, raw material are easy to get, and cost is relatively low, and high suitable for industrialized production, product fine, purity, particle is fine, stable quality, return
High income, it is pollution-free, can good environmental protection, it is safe and non-toxic, can be safe to use.
Embodiment 2：
A kind of method for preparing high-purity ultrafine lithium-carbonate micro powder, comprises the following steps that：
Step 1：The preparation of lithia water：First first level lithium carbonate is crushed, the method for crushing is ball mill grinding
Or air-flow crushing or Ultrasonic Pulverization.Then first level lithium carbonate after crushing is added in reactor, passes through heating in water bath for reaction device
Untill temperature reaches 90-95 DEG C, formic acid is then slowly added dropwise into reactor, formic acid rate of addition obtains for 6-10d/s
Lithium formate solution, carbon amide solution is then added into lithium formate solution and is passed through carbon dioxide, obtains lithia water；
Step 2：The preparation of high-purity ultrafine lithium-carbonate micro powder：Lithia water is added in spray drying device, into
Drying is decomposed in row spraying, and the temperature of spray drying device is 670 DEG C, has just obtained high-purity ultrafine lithium-carbonate micro powder.
Preparation method of the invention is simple, cost is low, energy consumption consumption is low, is easy to produce in enormous quantities, its preparation process is easy to
Control, raw material are easy to get, and cost is relatively low, and high suitable for industrialized production, product fine, purity, particle is fine, stable quality, return
High income, it is pollution-free, can good environmental protection, it is safe and non-toxic, can be safe to use.
It should be noted that listed above is only a kind of specific embodiment of the invention.It is clear that the invention is not restricted to
Upper embodiment, can also there is many deformations, in short, those of ordinary skill in the art can directly lead from present disclosure
All deformations for going out or associating, are considered as protection scope of the present invention.
Claims (5)
- A kind of 1. method for preparing high-purity ultrafine lithium-carbonate micro powder, it is characterised in that comprise the following steps that：Step 1：The preparation of lithia water：First first level lithium carbonate is crushed, then by just level lithium carbonate adds after crushing Enter into reactor, then formic acid is slowly added dropwise untill temperature reaches 90-95 DEG C in heating response device into reactor, obtain To lithium formate solution, carbon amide solution is then added into lithium formate solution and is passed through carbon dioxide, obtains lithia water；Step 2：The preparation of high-purity ultrafine lithium-carbonate micro powder：Lithia water is added in spray drying device, is sprayed Mist decomposes drying, and the temperature of spray drying device is 650~680 DEG C, has just obtained high-purity ultrafine lithium-carbonate micro powder.
- 2. the method for high-purity ultrafine lithium-carbonate micro powder is prepared according to claim 1, it is characterised in that the method for the crushing For ball mill grinding or air-flow crushing or Ultrasonic Pulverization.
- 3. the method for high-purity ultrafine lithium-carbonate micro powder is prepared according to claim 1, it is characterised in that the reactor adds Heat is heating water bath.
- 4. the method for high-purity ultrafine lithium-carbonate micro powder is prepared according to claim 1, it is characterised in that speed is added dropwise in the formic acid Spend for 6-10d/s.
- 5. the method for high-purity ultrafine lithium-carbonate micro powder is prepared according to claim 1, it is characterised in that the spray drying is set Standby temperature is 670 DEG C.
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| CN201711384872.2A CN107935000A (en) | 2017-12-20 | 2017-12-20 | A kind of method for preparing high-purity ultrafine lithium-carbonate micro powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863496A (en) * | 2009-12-29 | 2010-10-20 | 昆明理工大学 | Method for preparing battery grade lithium carbonate by purifying industrial grade lithium carbonate |
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- 2017-12-20 CN CN201711384872.2A patent/CN107935000A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863496A (en) * | 2009-12-29 | 2010-10-20 | 昆明理工大学 | Method for preparing battery grade lithium carbonate by purifying industrial grade lithium carbonate |
Non-Patent Citations (1)
| Title |
|---|
| 范景莲编著: "《钨合金及其制备新技术》", 30 April 2006 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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