CN107804861A - A kind of method that battery-level lithium carbonate is manufactured using industrial level lithium carbonate - Google Patents
A kind of method that battery-level lithium carbonate is manufactured using industrial level lithium carbonate Download PDFInfo
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- CN107804861A CN107804861A CN201711118950.4A CN201711118950A CN107804861A CN 107804861 A CN107804861 A CN 107804861A CN 201711118950 A CN201711118950 A CN 201711118950A CN 107804861 A CN107804861 A CN 107804861A
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- lithium carbonate
- sodium hydroxide
- acetic acid
- level lithium
- hydroxide solution
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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 that battery-level lithium carbonate is manufactured using industrial level lithium carbonate, comprise the following steps:Take industrial level lithium carbonate to be dissolved in distilled water and be configured to lithium carbonate slurry;At normal temperatures, ethylenediamine tetra-acetic acid and sodium hydroxide solution is taken to be well mixed and obtain ethylenediamine tetra-acetic acid and sodium hydroxide mixed solution;Lithium carbonate slurry be sent into it is rotary packed bed in, and to being passed through CO in rotary packed bed2Gas, feed liquid is obtained after carrying out carburizing reagent;Ethylenediamine tetra-acetic acid and sodium hydroxide solution mixed solution are added in feed liquid, are sufficiently stirred to obtain mixed liquor;Separation of solid and liquid is carried out to mixed liquor, obtains lithia water;Lithia water is added in negative pressure device, decomposes lithium bicarbonate, is settled out battery-level lithium carbonate.Compared with prior art, present invention process is simple, simple operation, is advantageous to produce in batches;Reaction time is short, and transformation efficiency is high, and the utilization of resources is efficient, has broad application prospects.
Description
Technical field
Advanced green battery material manufacture work that the present invention relates to new energy -- new and effective energy conversion and storing technology --
The field such as skill and production technology, particularly a kind of method that battery-level lithium carbonate is manufactured using industrial level lithium carbonate.
Background technology
With the fast development of low-carbon economy and green novel energy source industry, in particular with great-capacity power battery technology
Break through and popularization and application, novel lithium battery power vehicle industry emerge rapidly, greatly develop lithium electricity industry as the generally common of people
Know, the tradition that the demand for promoting lithium is walked out to " industrial monosodium glutamate " is limited to, and welcomes the New Times of " energy metal ".Lithium carbonate is a kind of
Important industrial chemicals, with the appearance of national new energy development plan, lithium electricity new energy turns into state key and supports development
One of energy industry;And the important foundation raw material that lithium carbonate develops as lithium electricity new energy, its demand are increasing, price
More and more higher.
It is an important chemical method for lepidolite extraction lithium, the primary raw material for carrying lithium at present is salt lake bittern and consolidated
Body lithium minerals, the rich reserves of Chinese lepidolite and spodumene.The method that lithium is carried from lithium minerals mainly has sulfate process, chlorination
Thing method, limestone-based process, sulfuric acid process and gas-solid reaction method, these methods are all that lithium minerals is carried out into high-temperature calcination, then with not
The same method processing calcining further extracting sulfuric acid lithium solution of slag, obtains lithium sulfate solution, then reacts to obtain electricity with sodium carbonate
Pond level lithium carbonate and sinker mother liquor.All it is generally at present to use industrial level lithium carbonate to produce battery-level lithium carbonate in enormous quantities
Further to produce battery-level lithium carbonate, industrial level lithium carbonate is as production lithium metal and the critical product of secondary lithium salts, in glass
The essential industry fields such as glass ceramics, petrochemical industry, medicine, battery are all indispensable raw material.In recent years, as low-carbon passes through
Ji and the high speed development of the heating, especially lithium battery industry of New Energy Industry so that Li2CO3 demand is growing, should
Constantly expanded with scope, but the also more and more higher of the purity requirement to it, therefore to prepare high-purity Li2CO3 imperative for purification.
But the existing complex procedures that battery-level lithium carbonate is produced with industrial level lithium carbonate, reaction condition is cumbersome, production efficiency
Lowly, and corresponding corollary equipment is needed, production cost is high, and the purity of obtained battery-level lithium carbonate is low, is unsuitable for extensive
Generation.
The content of the invention
The invention aims to solve the deficiency of prior art problem, there is provided one kind utilizes industrial level lithium carbonate production system
The method for making battery-level lithium carbonate.
To reach above-mentioned purpose, the present invention is implemented according to following technical scheme:
A kind of method that battery-level lithium carbonate is manufactured using industrial level lithium carbonate, is comprised the following steps:
Step 1: taking industrial level lithium carbonate to be dissolved in is configured to material concentration as 90-100g/L's in the distilled water of 40-60 degree
Lithium carbonate slurry;
Step 2: at normal temperatures, ethylenediamine tetra-acetic acid and sodium hydroxide solution is taken to be well mixed and obtain ethylenediamine tetra-acetic acid
With sodium hydroxide mixed solution, ethylenediamine tetra-acetic acid and sodium hydroxide solution mass ratio are 0.5:6, the concentration of sodium hydroxide solution
It is standby for 25g/L;
Step 3:Lithium carbonate slurry be sent into it is rotary packed bed in, and to being passed through CO in rotary packed bed2Gas, carry out 40-
Feed liquid is obtained after 100min carburizing reagent;Wherein, the charging rate for controlling lithium carbonate slurry is 100-400mL/min, rotation
The rotating speed of packed bed is not higher than 50Hz, and CO2Gas flow is 0.1-0.2m3/L;
Step 4: ethylenediamine tetra-acetic acid and sodium hydroxide solution mixed solution are added in the feed liquid of step 3, second two
The weight of amine tetraacethyl and the feed liquid of sodium hydroxide solution mixed solution and step 3 ratio is 1:1, being sufficiently stirred 10-15 minutes obtains
Mixed liquor;
Step 5:Separation of solid and liquid is carried out to the mixed liquor of step 4, obtains lithia water;
Step 6: lithia water is added into temperature in 80-180 DEG C of negative pressure device, container negative pressure is in 0.01-
Stirred under conditions of 0.10MPa, decompose lithium bicarbonate, be settled out battery-level lithium carbonate.
Further, the feed rate in the step 3 is 250-350mL/min.
Preferably, the carburizing reagent time in the step 3 is 50-90min.
Compared with prior art, the reaction condition of the invention by adjusting lithium carbonate carbonisation, than prior art significantly
Improve lithium carbonate and be converted into the transformation efficiency of lithium bicarbonate, while also shorten the reaction time, with ethylenediamine tetra-acetic acid and hydrogen
Sodium oxide molybdena mixed solution is complexed the Mg in lithium sulfate solution again2+Ion is easy to prepare low-magnesium battery level lithium carbonate, then uses
Heatable negative pressure device, rate of deposition are high, and the single rate of deposition of lithium carbonate is up to more than 90%.Present invention process is simple, and operation is just
Victory, be advantageous to produce in batches;Reaction time is short, and transformation efficiency is high, and the utilization of resources is efficient, has broad application prospects.
Embodiment
With reference to specific embodiment, the invention will be further described, the illustrative examples and explanation invented herein
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
Step 1: industrial level lithium carbonate is taken to be dissolved in the lithium carbonate for being configured to that material concentration is 90g/L in 40 degree of distilled water
Slurry;
Step 2: at normal temperatures, ethylenediamine tetra-acetic acid and sodium hydroxide solution is taken to be well mixed and obtain ethylenediamine tetra-acetic acid
With sodium hydroxide mixed solution, ethylenediamine tetra-acetic acid and sodium hydroxide solution mass ratio are 0.5:6, the concentration of sodium hydroxide solution
It is standby for 25g/L;
Step 3:Lithium carbonate slurry be sent into it is rotary packed bed in, and to being passed through CO in rotary packed bed2Gas, carry out
Feed liquid is obtained after 40min carburizing reagent;Wherein, control the charging rate of lithium carbonate slurry rotary packed bed for 100mL/min
Rotating speed be 30Hz, and CO2Gas flow is 0.1m3/L;
Step 4: ethylenediamine tetra-acetic acid and sodium hydroxide solution mixed solution are added in the feed liquid of step 3, second two
The weight of amine tetraacethyl and the feed liquid of sodium hydroxide solution mixed solution and step 3 ratio is 1:1, being sufficiently stirred 10 minutes to mix
Close feed liquid;
Step 5:Separation of solid and liquid is carried out to the mixed liquor of step 4, obtains lithia water;
Step 6: lithia water is added into temperature in 80 DEG C of negative pressure device, container negative pressure is 0.01MPa's
Under the conditions of stir, decompose lithium bicarbonate, be settled out battery-level lithium carbonate.
Embodiment 2
Step 1: industrial level lithium carbonate is taken to be dissolved in the lithium carbonate for being configured to that material concentration is 100g/L in 60 degree of distilled water
Slurry;
Step 2: at normal temperatures, ethylenediamine tetra-acetic acid and sodium hydroxide solution is taken to be well mixed and obtain ethylenediamine tetra-acetic acid
With sodium hydroxide mixed solution, ethylenediamine tetra-acetic acid and sodium hydroxide solution mass ratio are 0.5:6, the concentration of sodium hydroxide solution
It is standby for 25g/L;
Step 3:Lithium carbonate slurry be sent into it is rotary packed bed in, and to being passed through CO in rotary packed bed2Gas, carry out
Feed liquid is obtained after 100min carburizing reagent;Wherein, control the charging rate of lithium carbonate slurry rotary packed bed for 400mL/min
Rotating speed be 50Hz, and CO2Gas flow is 0.2m3/L;
Step 4: ethylenediamine tetra-acetic acid and sodium hydroxide solution mixed solution are added in the feed liquid of step 3, second two
The weight of amine tetraacethyl and the feed liquid of sodium hydroxide solution mixed solution and step 3 ratio is 1:1, being sufficiently stirred 15 minutes to mix
Close feed liquid;
Step 5:Separation of solid and liquid is carried out to the mixed liquor of step 4, obtains lithia water;
Step 6: lithia water is added into temperature in 180 DEG C of negative pressure device, container negative pressure is in 0.10MPa
Under conditions of stir, decompose lithium bicarbonate, be settled out battery-level lithium carbonate.
Embodiment 3
Step 1: industrial level lithium carbonate is taken to be dissolved in the lithium carbonate for being configured to that material concentration is 95g/L in 50 degree of distilled water
Slurry;
Step 2: at normal temperatures, ethylenediamine tetra-acetic acid and sodium hydroxide solution is taken to be well mixed and obtain ethylenediamine tetra-acetic acid
With sodium hydroxide mixed solution, ethylenediamine tetra-acetic acid and sodium hydroxide solution mass ratio are 0.5:6, the concentration of sodium hydroxide solution
It is standby for 25g/L;
Step 3:Lithium carbonate slurry be sent into it is rotary packed bed in, and to being passed through CO in rotary packed bed2Gas, carry out
Feed liquid is obtained after 50min carburizing reagent;Wherein, control the charging rate of lithium carbonate slurry rotary packed bed for 250mL/min
Rotating speed be 50Hz, and CO2Gas flow is 0.1m3/L;
Step 4: ethylenediamine tetra-acetic acid and sodium hydroxide solution mixed solution are added in the feed liquid of step 3, second two
The weight of amine tetraacethyl and the feed liquid of sodium hydroxide solution mixed solution and step 3 ratio is 1:1, being sufficiently stirred 10 minutes to mix
Close feed liquid;
Step 5:Separation of solid and liquid is carried out to the mixed liquor of step 4, obtains lithia water;
Step 6: lithia water is added into temperature in 100 DEG C of negative pressure device, container negative pressure is in 0.01MPa
Under conditions of stir, decompose lithium bicarbonate, be settled out battery-level lithium carbonate.
Embodiment 4
Step 1: industrial level lithium carbonate is taken to be dissolved in the lithium carbonate for being configured to that material concentration is 100g/L in 60 degree of distilled water
Slurry;
Step 2: at normal temperatures, ethylenediamine tetra-acetic acid and sodium hydroxide solution is taken to be well mixed and obtain ethylenediamine tetra-acetic acid
With sodium hydroxide mixed solution, ethylenediamine tetra-acetic acid and sodium hydroxide solution mass ratio are 0.5:6, the concentration of sodium hydroxide solution
It is standby for 25g/L;
Step 3:Lithium carbonate slurry be sent into it is rotary packed bed in, and to being passed through CO in rotary packed bed2Gas, carry out
Feed liquid is obtained after 90min carburizing reagent;Wherein, control the charging rate of lithium carbonate slurry rotary packed bed for 350mL/min
Rotating speed be 50Hz, and CO2Gas flow is 0.2m3/L;
Step 4: ethylenediamine tetra-acetic acid and sodium hydroxide solution mixed solution are added in the feed liquid of step 3, second two
The weight of amine tetraacethyl and the feed liquid of sodium hydroxide solution mixed solution and step 3 ratio is 1:1, being sufficiently stirred 15 minutes to mix
Close feed liquid;
Step 5:Separation of solid and liquid is carried out to the mixed liquor of step 4, obtains lithia water;
Step 6: lithia water is added into temperature in 120 DEG C of negative pressure device, container negative pressure is in 0.10MPa
Under conditions of stir, decompose lithium bicarbonate, be settled out battery-level lithium carbonate.
Embodiment 5
Step 1: industrial level lithium carbonate is taken to be dissolved in the lithium carbonate for being configured to that material concentration is 95g/L in 50 degree of distilled water
Slurry;
Step 2: at normal temperatures, ethylenediamine tetra-acetic acid and sodium hydroxide solution is taken to be well mixed and obtain ethylenediamine tetra-acetic acid
With sodium hydroxide mixed solution, ethylenediamine tetra-acetic acid and sodium hydroxide solution mass ratio are 0.5:6, the concentration of sodium hydroxide solution
It is standby for 25g/L;
Step 3:Lithium carbonate slurry be sent into it is rotary packed bed in, and to being passed through CO in rotary packed bed2Gas, carry out
Feed liquid is obtained after 60min carburizing reagent;Wherein, control the charging rate of lithium carbonate slurry rotary packed bed for 300mL/min
Rotating speed be not higher than 50Hz, and CO2Gas flow is 0.1m3/L;
Step 4: ethylenediamine tetra-acetic acid and sodium hydroxide solution mixed solution are added in the feed liquid of step 3, second two
The weight of amine tetraacethyl and the feed liquid of sodium hydroxide solution mixed solution and step 3 ratio is 1:1, being sufficiently stirred 12 minutes to mix
Close feed liquid;
Step 5:Separation of solid and liquid is carried out to the mixed liquor of step 4, obtains lithia water;
Step 6: lithia water is added into temperature in 140 DEG C of negative pressure device, container negative pressure is in 0.10MPa
Under conditions of stir, decompose lithium bicarbonate, be settled out battery-level lithium carbonate.
Technical scheme is not limited to the limitation of above-mentioned specific embodiment, and every technique according to the invention scheme is done
The technology deformation gone out, each falls within protection scope of the present invention.
Claims (3)
- A kind of 1. method that battery-level lithium carbonate is manufactured using industrial level lithium carbonate, it is characterised in that comprise the following steps:Step 1: industrial level lithium carbonate is taken to be dissolved in the carbonic acid for being configured to that material concentration is 90-100g/L in the distilled water of 40-60 degree Lithium slurry;Step 2: at normal temperatures, ethylenediamine tetra-acetic acid and sodium hydroxide solution is taken to be well mixed and obtain ethylenediamine tetra-acetic acid and hydrogen Sodium oxide molybdena mixed solution, ethylenediamine tetra-acetic acid and sodium hydroxide solution mass ratio are 0.5:6, the concentration of sodium hydroxide solution is 25g/L, it is standby;Step 3:Lithium carbonate slurry be sent into it is rotary packed bed in, and to being passed through CO in rotary packed bed2Gas, carry out 40- Feed liquid is obtained after 100min carburizing reagent;Wherein, the charging rate for controlling lithium carbonate slurry is 100-400mL/min, rotation The rotating speed of packed bed is not higher than 50Hz, and CO2Gas flow is 0.1-0.2m3/L;Step 4: ethylenediamine tetra-acetic acid and sodium hydroxide solution mixed solution are added in the feed liquid of step 3, ethylenediamine tetraacetic The weight of acetic acid and the feed liquid of sodium hydroxide solution mixed solution and step 3 ratio is 1:1, being sufficiently stirred 10-15 minutes must mix Feed liquid;Step 5:Separation of solid and liquid is carried out to the mixed liquor of step 4, obtains lithia water;Step 6: lithia water is added into temperature in 80-180 DEG C of negative pressure device, container negative pressure is in 0.01- Stirred under conditions of 0.10MPa, decompose lithium bicarbonate, be settled out battery-level lithium carbonate.
- 2. the method according to claim 1 that battery-level lithium carbonate is manufactured using industrial level lithium carbonate, its feature are existed In:Feed rate in the step 3 is 250-350mL/min.
- 3. the method according to claim 1 that battery-level lithium carbonate is manufactured using industrial level lithium carbonate, its feature are existed In:The carburizing reagent time in the step 3 is 50-90min.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109437254A (en) * | 2018-11-16 | 2019-03-08 | 湖南众德新材料科技有限公司 | A kind of lithium carbonate purifying technique device |
CN110078099A (en) * | 2019-04-26 | 2019-08-02 | 核工业北京化工冶金研究院 | A method of scavenging solution, which is leached, from lepidolite prepares lithium carbonate |
CN110357129A (en) * | 2019-07-30 | 2019-10-22 | 广西融兴沃能锂业科技有限公司 | A method of battery-level lithium carbonate is prepared from Crude lithium Carbonate purification |
CN111547748A (en) * | 2020-06-17 | 2020-08-18 | 赣州有色冶金研究所 | Method for preparing battery-grade lithium carbonate by efficiently decarbonizing lithium bicarbonate solution |
CN114361431A (en) * | 2021-08-20 | 2022-04-15 | 山东瑞福锂业有限公司 | Process and method for regulating and controlling structure of regular micron sheet lithium carbonate material for ternary positive electrode material in lithium ion battery |
CN115504490A (en) * | 2022-09-29 | 2022-12-23 | 江西闪凝科技有限公司 | Method for preparing battery-grade lithium carbonate by aid of external field |
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CN102583453A (en) * | 2011-08-31 | 2012-07-18 | 四川长和华锂科技有限公司 | Industrial method for producing battery-grade lithium carbonate or high-purity lithium carbonate |
CN104326495A (en) * | 2014-07-15 | 2015-02-04 | 多氟多化工股份有限公司 | Method for preparing high-purity lithium carbonate with co-production of lithium fluoride by employing crude lithium carbonate |
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Patent Citations (2)
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CN102583453A (en) * | 2011-08-31 | 2012-07-18 | 四川长和华锂科技有限公司 | Industrial method for producing battery-grade lithium carbonate or high-purity lithium carbonate |
CN104326495A (en) * | 2014-07-15 | 2015-02-04 | 多氟多化工股份有限公司 | Method for preparing high-purity lithium carbonate with co-production of lithium fluoride by employing crude lithium carbonate |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109437254A (en) * | 2018-11-16 | 2019-03-08 | 湖南众德新材料科技有限公司 | A kind of lithium carbonate purifying technique device |
CN110078099A (en) * | 2019-04-26 | 2019-08-02 | 核工业北京化工冶金研究院 | A method of scavenging solution, which is leached, from lepidolite prepares lithium carbonate |
CN110357129A (en) * | 2019-07-30 | 2019-10-22 | 广西融兴沃能锂业科技有限公司 | A method of battery-level lithium carbonate is prepared from Crude lithium Carbonate purification |
CN110357129B (en) * | 2019-07-30 | 2021-08-13 | 广西融兴沃能锂业科技有限公司 | Method for preparing battery-grade lithium carbonate by purifying crude lithium carbonate |
CN111547748A (en) * | 2020-06-17 | 2020-08-18 | 赣州有色冶金研究所 | Method for preparing battery-grade lithium carbonate by efficiently decarbonizing lithium bicarbonate solution |
CN114361431A (en) * | 2021-08-20 | 2022-04-15 | 山东瑞福锂业有限公司 | Process and method for regulating and controlling structure of regular micron sheet lithium carbonate material for ternary positive electrode material in lithium ion battery |
CN115504490A (en) * | 2022-09-29 | 2022-12-23 | 江西闪凝科技有限公司 | Method for preparing battery-grade lithium carbonate by aid of external field |
CN115504490B (en) * | 2022-09-29 | 2023-12-19 | 江西闪凝科技有限公司 | Method for preparing battery-grade lithium carbonate by external field assistance |
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