CN108658099A - A kind of battery-stage monohydrate lithium hydroxide purifying technique - Google Patents
A kind of battery-stage monohydrate lithium hydroxide purifying technique Download PDFInfo
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- CN108658099A CN108658099A CN201810506790.9A CN201810506790A CN108658099A CN 108658099 A CN108658099 A CN 108658099A CN 201810506790 A CN201810506790 A CN 201810506790A CN 108658099 A CN108658099 A CN 108658099A
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- lithium hydroxide
- battery
- lithium
- monohydrate lithium
- purifying technique
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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
- C01D15/02—Oxides; Hydroxides
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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 present invention provides a kind of battery-stage monohydrate lithium hydroxide purifying techniques, mainly comprise the technical steps that:A, ball milling:Lithium carbonate raw ore is crushed and ball milling;B, causticization:White lime is added in lithium carbonate slurry and carries out causticizing reaction;C, it filters;D, ion exchange;E, evaporative crystallization;F, it is separated by solid-liquid separation washing;G, drying:The monohydrate lithium hydroxide that step F is obtained is dried containing wet crystal and is sieved to get battery-stage monohydrate lithium hydroxide.Battery-stage monohydrate lithium hydroxide purifying technique of the present invention is used obtains refined solution by clear lithium hydroxide solution after ion-exchange purification, have the characteristics that impurity content is low, solution purity is high, then can be obtained the high product of purity by flush distillation condensing crystallizing;With conventional multi recrystallizing technology ratio, have the characteristics that flow is short, product quality is stablized.
Description
Technical field
The invention belongs to lithium hydroxide preparing technical fields, are related to a kind of battery-stage monohydrate lithium hydroxide purifying technique.
Background technology
In the purification technique of battery-stage monohydrate lithium hydroxide, according to its production method, the technology that uses at present mainly just like
Lower two kinds of routes:
(1)Repeated recrystallize method
It is that 5-10% postcoolings are cooled to 30-40 DEG C that lithium hydroxide solution, which is evaporated, and is concentrated into magma solid content, and single water is precipitated
Lithium hydroxide crystal;Magma is separated by solid-liquid separation, and is washed to obtain monohydrate lithium hydroxide containing wet crystal to crystal;It obtains
Monohydrate lithium hydroxide product purity it is inadequate, the production process of recrystallization is repeated, until obtain single water of qualified product
Lithium hydroxide crystal.Although the method is simple, there are unstable product quality, duplication of production operation, low production efficiency are needed
Problem, and energy consumption is higher, the opposite production cost for improving lithium hydroxide.
(2)EDTA method of purifications
By EDTA(Ethylenediamine tetra-acetic acid)It is added in lithium hydroxide solution, liquid is purified after filtering, then by scavenging solution
It is that 5-10% postcoolings are cooled to 30-40 DEG C to be evaporated and be concentrated into magma solid content, and monohydrate lithium hydroxide crystal is precipitated;It will be brilliant
Slurry is separated by solid-liquid separation, and is washed to obtain monohydrate lithium hydroxide containing wet crystal to crystal;The monohydrate lithium hydroxide that will be obtained
It is dried containing wet crystal, obtains battery-stage monohydrate lithium hydroxide.Although such method is simple, product quality shakiness is equally existed
Calmly, the problem of low production efficiency, in addition, containing EDTA in the water body generated in production process, it need to subsequently increase sewage disposal and arrange
It applies, the opposite production cost for improving lithium hydroxide.
Develop that a kind of product quality is stable and the lower lithium hydroxide method of purification of production cost is current lithium hydroxide system
The problem of standby field urgent need to resolve.
Invention content
It is an object of the invention in view of the problems of the existing technology, provide a kind of battery-stage monohydrate lithium hydroxide purification
Technique, present invention process have many advantages, such as that easy to operate, easy to implement, product purity is high, product quality is stablized.
For this purpose, the present invention adopts the following technical scheme that:
A kind of battery-stage monohydrate lithium hydroxide purifying technique, comprises the technical steps that:
A, ball milling:Lithium carbonate raw ore is crushed, ball milling, obtains the powder that granularity is 3-100um;When ball milling, raw ore wet-milling
Material more powder is better, and contact area is bigger when next step reacts, and reaction efficiency is higher, and reaction conversion ratio is higher.
B, causticization:It is configured to lithium carbonate slurry after the obtained powders of step A are added water, it is anti-that white lime progress causticization is added
It answers, the reaction time is 3.5-4.5 hours, heats and stirs in reaction process, and heating temperature is 90-95 DEG C, and mixing speed is
700-900rpm obtains lithium hydroxide solution and slurry liquid that precipitation of calcium carbonate mixes after reaction;When reaction, lithium carbonate is controlled
Molar ratio with white lime is 1:1.0-1.2 preferably 1:1.1;
The reaction equation of lithium carbonate raw ore and white lime is:
Li2CO3+Ca(OH)2→CaCO3↓+2LiOH
There are materials to wrap up phenomenon for above-mentioned reaction, it is therefore desirable to which high-speed stirred and low granularity material are added, is conducive to improve in this way
Reaction efficiency and materials conversion rate avoid lithium carbonate and white lime from reacting incomplete.
C, it filters:The slurry liquid that step B is obtained is filtered, settle, is filtered again, is obtained after being cooled to 30-45 DEG C
Clear lithium hydroxide solution;
Filtrate is filtered again after sedimentation, and purpose obtains clear hydrogen to further decrease the solid content in feed liquid
Lithia solution.Clear lithium hydroxide solution enters back into next step after cooling, it is therefore an objective to meet pipeline and ion is handed over
Change the requirement of resin temperature in use.
D, ion exchange:Removal of impurities processing is carried out to the clarification lithium hydroxide solution that step C is obtained using ion exchange resin,
Refined solution after being purified;
In step D, containing calcium, magnesium, iron, copper, aluminium plasma impurity in clear lithium hydroxide solution pre-purified solution, always contain
Amount is generally less than 10ppm, to ensure purification efficiency and effect, improves production efficiency, therefore is cleaned using ion exchange resin
Processing.Wherein, ion exchange resin preferred acidic cation macropore chelate resin, it is therefore an objective to the ion that impurity is saturated can be handed over
It changes resin and carries out repeated reproducibility, and chelate resin exchange capacity is high, and service life can be improved;
The preferred 12-15m of ion-exchange resin purification flow velocity3/ h meets production effect to improve the purification effect of ion exchange resin
The needs of rate.
E, evaporative crystallization:The obtained refined solutions of step D are concentrated by evaporation after being 5-10% to magma solid content and are cooled to 30-
40 DEG C, monohydrate lithium hydroxide crystal is precipitated.
F, it is separated by solid-liquid separation washing:The obtained magmas of step E are separated by solid-liquid separation, and crystal is washed to obtain single water
Lithium hydroxide contains wet crystal;
In step F, the wash water obtained after washing is used for causticizing reaction in step B, and the mother liquor after separation of solid and liquid is back in step E
It is evaporated concentration.
G, drying:The monohydrate lithium hydroxide that step F is obtained is dried containing wet crystal and is sieved to get LITHIUM BATTERY list water hydrogen-oxygen
Change lithium;
Drying and screening in this step are routine techniques in the art, do not illustrate and limit herein.
Compared with existing purification technique, the invention has the advantages that:
(1)Battery-stage monohydrate lithium hydroxide purifying technique of the present invention uses clear lithium hydroxide solution is pure by ion exchange
Refined solution is obtained after change, has the characteristics that impurity content is low, solution purity is high, and then passing through flush distillation condensing crystallizing can obtain
The product high to purity.With conventional multi recrystallizing technology ratio, have the characteristics that flow is short, product quality is stablized.
(2)With addition EDTA purifying techniques ratio, the present invention will not pollute water body, increase water process ring without additional
Facility is protected, while this process increases product purities, stabilize product quality, improve production efficiency, overall cost is low.
Specific implementation mode
Present invention process is further detailed with reference to specific embodiment.
Embodiment 1
A kind of battery-stage monohydrate lithium hydroxide purifying technique, comprises the technical steps that:
A, ball milling:Lithium carbonate raw ore is crushed, ball milling, obtains the powder that granularity is 40-60um;
B, causticization:It is configured to lithium carbonate slurry after the obtained powders of step A are added water, by lithium carbonate:White lime=1:1.0 rub
You carry out causticizing reaction than white lime is added, and heat and stir, reaction time 4.5h, heating temperature 90- in reaction process
95 DEG C, mixing speed 700rpm, lithium hydroxide solution is obtained after reaction and slurry liquid that precipitation of calcium carbonate mixes;In reaction
The conversion ratio of lithium is 86%;
C, it filters:The slurry liquid that step B is obtained is filtered, settle, is filtered again, is clarified after being cooled to 30-45 DEG C
Lithium hydroxide solution;
D, ion exchange:The clarification lithium hydroxide solution that step C is obtained using acid cation macropore chelating type exchanger resin
Removal of impurities processing is carried out, the refined solution after being purified;Ion-exchange resin purification flow control is 12m3/h;
E, evaporative crystallization:By the obtained refined solutions of step D be concentrated by evaporation be 5% to magma solid content after be cooled to 30-40 DEG C, analysis
Go out monohydrate lithium hydroxide crystal;
F, it is separated by solid-liquid separation washing:The obtained magmas of step E are separated by solid-liquid separation, and crystal is washed to obtain single water hydrogen-oxygen
Change lithium and contains wet crystal;The wash water obtained after washing is used for causticizing reaction in step B, and the mother liquor after separation of solid and liquid is back to step E
In be evaporated concentration;
G, drying:The monohydrate lithium hydroxide that step F is obtained is dried containing wet crystal and is sieved to get LITHIUM BATTERY list water hydroxide
Lithium.
Embodiment 2
A kind of battery-stage monohydrate lithium hydroxide purifying technique, comprises the technical steps that:
A, ball milling:Lithium carbonate raw ore is crushed, ball milling, obtains the powder that granularity is 60-100um;
B, causticization:It is configured to lithium carbonate slurry after the obtained powders of step A are added water, by lithium carbonate:White lime=1:1.2 rub
You carry out causticizing reaction than white lime is added, and heat and stir, reaction time 4h, heating temperature 90-95 in reaction process
DEG C, mixing speed 900rpm obtains lithium hydroxide solution and slurry liquid that precipitation of calcium carbonate mixes after reaction;Lithium in reaction
Conversion ratio be 81%;
C, it filters:The slurry liquid that step B is obtained is filtered, settle, is filtered again, is clarified after being cooled to 30-45 DEG C
Lithium hydroxide solution;
D, ion exchange:The clarification lithium hydroxide solution that step C is obtained using acid cation macropore chelating type exchanger resin
Removal of impurities processing is carried out, the refined solution after being purified;Ion-exchange resin purification flow control is 15m3/h;
E, evaporative crystallization:By the obtained refined solutions of step D be concentrated by evaporation be 10% to magma solid content after be cooled to 30-40 DEG C, analysis
Go out monohydrate lithium hydroxide crystal;
F, it is separated by solid-liquid separation washing:The obtained magmas of step E are separated by solid-liquid separation, and crystal is washed to obtain single water hydrogen-oxygen
Change lithium and contains wet crystal;The wash water obtained after washing is used for causticizing reaction in step B, and the mother liquor after separation of solid and liquid is back to step E
In be evaporated concentration;
G, drying:The monohydrate lithium hydroxide that step F is obtained is dried containing wet crystal and is sieved to get LITHIUM BATTERY list water hydroxide
Lithium.
Embodiment 3
A kind of battery-stage monohydrate lithium hydroxide purifying technique, comprises the technical steps that:
A, ball milling:Lithium carbonate raw ore is crushed, ball milling, obtains the powder that granularity is 3-40um;
B, causticization:It is configured to lithium carbonate slurry after the obtained powders of step A are added water, by lithium carbonate:White lime=1:1.1 rub
You carry out causticizing reaction than white lime is added, and heat and stir, reaction time 3.5h, heating temperature 90- in reaction process
95 DEG C, mixing speed 800rpm, lithium hydroxide solution is obtained after reaction and slurry liquid that precipitation of calcium carbonate mixes;In reaction
The conversion ratio of lithium is 90%;
C, it filters:The slurry liquid that step B is obtained is filtered, settle, is filtered again, is clarified after being cooled to 30-45 DEG C
Lithium hydroxide solution;
D, ion exchange:The clarification lithium hydroxide solution that step C is obtained using acid cation macropore chelating type exchanger resin
Removal of impurities processing is carried out, the refined solution after being purified;Ion-exchange resin purification flow control is 13m3/h;
E, evaporative crystallization:By the obtained refined solutions of step D be concentrated by evaporation be 8% to magma solid content after be cooled to 30-40 DEG C, analysis
Go out monohydrate lithium hydroxide crystal;
F, it is separated by solid-liquid separation washing:The obtained magmas of step E are separated by solid-liquid separation, and crystal is washed to obtain single water hydrogen-oxygen
Change lithium and contains wet crystal;The wash water obtained after washing is used for causticizing reaction in step B, and the mother liquor after separation of solid and liquid is back to step E
In be evaporated concentration;
G, drying:The monohydrate lithium hydroxide that step F is obtained is dried containing wet crystal and is sieved to get LITHIUM BATTERY list water hydroxide
Lithium.
The battery-stage monohydrate lithium hydroxide that battery-stage monohydrate lithium hydroxide purifying technique of the present invention is prepared is produced below
Product are measured.
LITHIUM BATTERY lithium hydroxide prepared by D-1 grades of quality standards of 1 battery-stage monohydrate lithium hydroxide of table and embodiment 1-3
Product composition, content
As shown in Table 1, the LITHIUM BATTERY list water hydroxide being prepared using battery-stage monohydrate lithium hydroxide purifying technique of the present invention
Lithium product can reach LITHIUM BATTERY lithium hydroxide(LiOH·H2O)The quality requirement of D-1 ranks.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (6)
1. a kind of battery-stage monohydrate lithium hydroxide purifying technique, which is characterized in that comprise the technical steps that:
A, ball milling:Lithium carbonate raw ore is crushed, ball milling, obtains the powder that granularity is 3-100um;
B, causticization:It is configured to lithium carbonate slurry after the obtained powders of step A are added water, white lime is added and carries out causticizing reaction, instead
Should during heat and strong stirring, lithium hydroxide solution is obtained after reaction and slurry liquid that precipitation of calcium carbonate mixes;
C, it filters:The slurry liquid that step B is obtained is filtered, settle, is filtered again, clear hydroxide is obtained by cooling
Lithium solution;
D, ion exchange:Removal of impurities processing is carried out to the clarification lithium hydroxide solution that step C is obtained using ion exchange resin, is obtained
Refined solution after purification;
E, evaporative crystallization:The obtained refined solutions of step D are concentrated by evaporation after being 5-10% to magma solid content and are cooled to 30-40 DEG C,
Monohydrate lithium hydroxide crystal is precipitated;
F, it is separated by solid-liquid separation washing:The obtained magmas of step E are separated by solid-liquid separation, and crystal is washed to obtain single water hydrogen-oxygen
Change lithium and contains wet crystal;
G, drying:The monohydrate lithium hydroxide that step F is obtained is dried containing wet crystal and is sieved to get LITHIUM BATTERY list water hydroxide
Lithium.
2. a kind of battery-stage monohydrate lithium hydroxide purifying technique according to claim 1, which is characterized in that in step B, carbon
The molar ratio of sour lithium and white lime is 1:1.0-1.2.
3. a kind of battery-stage monohydrate lithium hydroxide purifying technique according to claim 1, which is characterized in that in step B, instead
It is 3.5-4.5 hours between seasonable, reaction temperature is 90-95 DEG C, mixing speed 700-900rpm.
4. a kind of battery-stage monohydrate lithium hydroxide purifying technique according to claim 1, which is characterized in that in step C, drop
The temperature of gained lithium hydroxide solution is 30-45 DEG C after temperature.
5. a kind of battery-stage monohydrate lithium hydroxide purifying technique according to claim 1, which is characterized in that in step D, institute
It is 12-15m to state ion exchange resin and use acid cation macropore chelate resin, ion-exchange resin purification flow velocity3/h。
6. a kind of battery-stage monohydrate lithium hydroxide purifying technique according to claim 1, which is characterized in that in step F, wash
The wash water obtained after washing is used for causticizing reaction in step B, and the mother liquor after separation of solid and liquid, which is back in step E, is evaporated concentration.
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CN109485077A (en) * | 2019-01-15 | 2019-03-19 | 宁德叁源技术有限公司 | A kind of technique for extracting lithium from lithium ore |
CN109485078A (en) * | 2019-01-15 | 2019-03-19 | 宁德叁源技术有限公司 | The technique of lithium is extracted from lithium ore |
CN109502611A (en) * | 2018-11-16 | 2019-03-22 | 湖南众德新材料科技有限公司 | A kind of device preparing lithium hydroxide micro nano powder |
CN109518008A (en) * | 2019-01-15 | 2019-03-26 | 宁德叁源技术有限公司 | A method of extracting lithium from containing lithium minerals |
CN109517981A (en) * | 2019-01-15 | 2019-03-26 | 宁德叁源技术有限公司 | The method of lithium is extracted from spodumene |
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CN110950363A (en) * | 2019-12-25 | 2020-04-03 | 广西天源新能源材料有限公司 | Production process of battery-grade lithium hydroxide monohydrate by applying novel combined calcium removal |
CN111170342A (en) * | 2019-11-06 | 2020-05-19 | 江西赣锋锂业股份有限公司 | Preparation method of battery-grade anhydrous lithium hydroxide |
CN111302365A (en) * | 2020-02-13 | 2020-06-19 | 雅化锂业(雅安)有限公司 | Production process of battery-grade lithium hydroxide |
CN112110462A (en) * | 2020-08-31 | 2020-12-22 | 荆门市格林美新材料有限公司 | Method for producing battery-grade lithium hydroxide by continuous freezing elution crystallization mode |
CN112939035A (en) * | 2021-04-07 | 2021-06-11 | 重庆天海电池材料有限公司 | Preparation method of lithium hydroxide monohydrate |
CN114604880A (en) * | 2022-04-21 | 2022-06-10 | 江西金辉锂业有限公司 | Preparation and purification device for battery-grade lithium hydroxide |
CN115849412A (en) * | 2022-12-27 | 2023-03-28 | 江西东鹏新材料有限责任公司 | Preparation method of battery-grade fine-grain lithium hydroxide monohydrate |
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Cited By (16)
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CN109502611A (en) * | 2018-11-16 | 2019-03-22 | 湖南众德新材料科技有限公司 | A kind of device preparing lithium hydroxide micro nano powder |
CN109485077A (en) * | 2019-01-15 | 2019-03-19 | 宁德叁源技术有限公司 | A kind of technique for extracting lithium from lithium ore |
CN109485078A (en) * | 2019-01-15 | 2019-03-19 | 宁德叁源技术有限公司 | The technique of lithium is extracted from lithium ore |
CN109518008A (en) * | 2019-01-15 | 2019-03-26 | 宁德叁源技术有限公司 | A method of extracting lithium from containing lithium minerals |
CN109517981A (en) * | 2019-01-15 | 2019-03-26 | 宁德叁源技术有限公司 | The method of lithium is extracted from spodumene |
CN109609786A (en) * | 2019-01-15 | 2019-04-12 | 宁德叁源技术有限公司 | A method of extracting lithium from lithium ore |
JP7442617B2 (en) | 2019-07-19 | 2024-03-04 | ウン チョン | Method for producing lithium hydroxide |
CN110330041A (en) * | 2019-07-22 | 2019-10-15 | 重庆锦弘建设工程有限公司 | A kind of higher value application method of low grade lithium carbonate |
CN111170342A (en) * | 2019-11-06 | 2020-05-19 | 江西赣锋锂业股份有限公司 | Preparation method of battery-grade anhydrous lithium hydroxide |
CN110950363A (en) * | 2019-12-25 | 2020-04-03 | 广西天源新能源材料有限公司 | Production process of battery-grade lithium hydroxide monohydrate by applying novel combined calcium removal |
CN111302365A (en) * | 2020-02-13 | 2020-06-19 | 雅化锂业(雅安)有限公司 | Production process of battery-grade lithium hydroxide |
CN112110462A (en) * | 2020-08-31 | 2020-12-22 | 荆门市格林美新材料有限公司 | Method for producing battery-grade lithium hydroxide by continuous freezing elution crystallization mode |
CN112110462B (en) * | 2020-08-31 | 2023-05-12 | 荆门市格林美新材料有限公司 | Method for producing battery-grade lithium hydroxide by continuous freezing and dialysis crystallization mode |
CN112939035A (en) * | 2021-04-07 | 2021-06-11 | 重庆天海电池材料有限公司 | Preparation method of lithium hydroxide monohydrate |
CN114604880A (en) * | 2022-04-21 | 2022-06-10 | 江西金辉锂业有限公司 | Preparation and purification device for battery-grade lithium hydroxide |
CN115849412A (en) * | 2022-12-27 | 2023-03-28 | 江西东鹏新材料有限责任公司 | Preparation method of battery-grade fine-grain lithium hydroxide monohydrate |
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