CN102432043A - Purification method of lithium carbonate - Google Patents
Purification method of lithium carbonate Download PDFInfo
- Publication number
- CN102432043A CN102432043A CN2011102825541A CN201110282554A CN102432043A CN 102432043 A CN102432043 A CN 102432043A CN 2011102825541 A CN2011102825541 A CN 2011102825541A CN 201110282554 A CN201110282554 A CN 201110282554A CN 102432043 A CN102432043 A CN 102432043A
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- Prior art keywords
- quilonum retard
- dissolved
- aqueous solution
- purification
- recrystallize
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
- C01D7/24—Crystallisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
- C01D7/26—Purification by precipitation or adsorption
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Gas Separation By Absorption (AREA)
- Secondary Cells (AREA)
Abstract
The invention provides a purification method of lithium carbonate, which comprises a dissolving step, wherein the lithium carbonate slurry containing impurities is fed with carbonated water with dissolved carbon dioxide circulatedly so as to be dissolved; a filtering step, wherein insoluble components are removed from the aqueous solution with dissolved lithium carbonate; a recrystallization step, wherein the aqueous solution with dissolved lithium carbonate is heated so as to gasify carbon dioxide in the aqueous solution and recrystallize lithium carbonate; and a separating step, wherein recrystallized lithium carbonate is precipitated.
Description
Technical field
The present invention relates to remove impurity and purified method in the Quilonum Retard; In more detail; Be through making the Quilonum Retard that contains impurity in being dissolved with the aqueous solution of dioxide gas, dissolving again, filter, utilizing the recrystallize of heating, thus the method for prepared calcium carbonate lithium.
Background technology
Lithium is as the medium of the electric charge of lithium ion 2 primary cells, and particularly the form with the metal acid lithium is used as positive electrode material.Lithium ion 2 primary cells hope to be used as the power source that automobile is used, and as the power source of PHEV and power truck, can be contemplated to turnout and suddenly increase.The lithium raw material majority that these lithium ion 2 primary cells use is by the Quilonum Retard product processed, but on the characteristic of battery, requires the few highly purified Quilonum Retard of impurity.Yet the refining relation owing to its method and apparatus of Quilonum Retard is so only be used in the extremely limited purposes.
In addition; As the technology that reclaims the lithium composition by lithium ion battery; The method that generates Quilonum Retard and reclaim lithium ion battery and the solution after having separated the lithium composition of handling is arranged; Also may not obtain the good Quilonum Retard of purity but add the sodium composition when separating treatment through the lithium composition, carbonating,, hope the purification techniques of simple and cheap Quilonum Retard from this point.
As one of process for purification of Quilonum Retard; Japanese kokai publication sho 62-252315 (patent documentation 1) disclosed method is arranged; But owing to be to import dioxide gas and make its reaction to the Quilonum Retard slurry that contains impurity; And poor at the dissolved efficiency of normal pressure carbon dioxide gas, the refining desired time is elongated.
Though by japanese kokai publication hei 11-310414 (patent documentation 2), Japanese Patent the 3671148th (patent documentation 3) disclosed method; But in order to improve the dissolved efficiency of dioxide gas; And need pressurized vessel when carrying out being blown into of dioxide gas adding to depress, so the restriction of plant capacity and manufacturing cost thereof can increase.
Patent documentation 1: japanese kokai publication sho 62-252315 " method of manufacture of high purity carbonic acid lithium "
Patent documentation 2: japanese kokai publication hei 11-310414 " method of manufacture of high purity carbonic acid lithium "
Patent documentation 3: Japanese Patent the 3671148th " process for purification of Quilonum Retard "
Summary of the invention
The present invention is the purification techniques to aforesaid Quilonum Retard, provides the simple equipment of a kind of usefulness effectively to carry out the purified method of Quilonum Retard for solving its shortcoming.
The present invention is the invention that has solved the problem the when Quilonum Retard that contains impurity made with extra care.
(1) a kind of process for purification of Quilonum Retard, it comprises following operation: supply is dissolved with the Soda Ash Light 99.2min. of dioxide gas and circulates in the Quilonum Retard slurry that contains impurity, dissolves the dissolution process of Quilonum Retard slurry thus; Remove the not filtration operation of solvent components from the aqueous solution that is dissolved with Quilonum Retard; The aqueous solution that is dissolved with Quilonum Retard of solvent components heats to removing not, makes the carbon dioxide gasification in the aqueous solution, makes the recrystallize operation of Quilonum Retard recrystallize thus; With separate the sedimentary separation circuit of Quilonum Retard of recrystallize from the aqueous solution.
(2) like the process for purification of above-mentioned (1) described Quilonum Retard, in said dissolution process, use the Soda Ash Light 99.2min. of dioxide gas mixed dissolution device preparation use.
Like the process for purification of above-mentioned (1) or above-mentioned (2) described Quilonum Retard, it is characterized in that (3) in said dissolution process, the meltage of the dioxide gas in the Soda Ash Light 99.2min. of using is as more than the 500mg/L.
(4) like the process for purification of each described Quilonum Retard of above-mentioned (1)～(3), in said filtration operation, make aqueous solution round-robin pipe arrangement that strainer is set, implement not removing of solvent components at the container that from dissolution process, uses.
Like the process for purification of each described Quilonum Retard of above-mentioned (1)～above-mentioned (4), it is characterized in that (5) in said recrystallize operation, the temperature that makes the Quilonum Retard recrystallize is 70 ℃～100 ℃, the pH of solution is more than 9.
Through implementing the process for purification of above-mentioned Quilonum Retard,
(1) supply is dissolved with the Soda Ash Light 99.2min. of dioxide gas and circulates in impure Quilonum Retard slurry; Can generate lithium bicarbonate thus; More than the solubleness of Quilonum Retard, make the lithium dissolving, insoluble impurity contained in the Quilonum Retard can be through removing by filter.
(2) heating is removed the Quilonum Retard solution behind the insoluble impurity in above-mentioned (1) and is made its recrystallize, can reduce the absorption of the impurity of stripping in solution thus, and solvability impurity is reduced.
Description of drawings
Fig. 1 illustrates the process chart of an example of expression Quilonum Retard process for purification of the present invention.
Fig. 2 illustrates the synoptic diagram of an example of expression Quilonum Retard dissolver of the present invention.
Reference numeral
1. lixator
2. stirrer
3., 6. pump
4. dioxide gas introducing port
5. multistage segmentation dioxide gas dissolver
7. strainer
Embodiment
The basic working procedure flow process of an expression example of the present invention is recited among Fig. 1, below the present invention is specified.
Of the present invention to liking the many Quilonum Retards of impurity that reclaim with Quilonum Retard, lithium ion battery etc. from general-purpose industrial.
Adjust the Quilonum Retard of said object so that slurry concentration is 25～100g/L, preferred 40～80g/L.Liquid measure is preferably about 2/3 capacity of reaction vessel.
In dissolution process, the limit makes the circulation of said Quilonum Retard slurry, the limit make its part or all import to dioxide gas mixed dissolution device, make the dioxide gas dissolving and make Soda Ash Light 99.2min..
Dioxide gas mixed dissolution device is: the multistage has booster chamber, and imports CO from this booster chamber front
2Gas, and at the indoor CO that makes
2The mechanism of gas dissolving in solution, and be to do one's utmost to improve CO
2The device of the meltage of gas in object liquid.For example, the CO in the Quilonum Retard lysate
2The meltage of gas can easily be 500mg/L.This with the Quilonum Retard lysate of the mode of utilizing common ingress pipe to drop in CO
2The meltage of gas is to compare about 120mg/L, is the value far above it.
The limit imports its circulation limit in reactive tank, and makes the Quilonum Retard dissolving.At this moment, if stirrer is set, then can further promote the dissolving of Quilonum Retard at lixator.Lixator need not be pressurized vessel, so long as common FRP system or resin system groove get final product.Quilonum Retard utilizes the dioxide gas in the solution to carry out the reaction of following formula, generates lithium bicarbonate thus, and is dissolved in the solution.
Li
2CO
3+CO
2→2Li
2HCO
3
Concrete dissolution process device is shown in Fig. 2.
Insoluble impurities is removed in the filtration of in filtering operation, having dissolved the lysate of slurry.Filtration is through at lixator circulation line being set, and built in or rear-mounted strainer are set herein, can carry out cheapness and the good filtration of operation property thus.
Heating Quilonum Retard lysate is separated out the Quilonum Retard crystal in the Crystallization Procedure.The pH of Quilonum Retard lysate drops at 9 o'clock, drops into alkaline agents such as caustic soda, ammoniacal liquor, is adjusted to pH9 when above, the recovery raising of Quilonum Retard.In addition, Heating temperature is preferred 70 ℃～100 ℃.
Solid-liquid separation process is to use the Quilonum Retard after devices such as pressure filter, centrifuge separator reclaim crystallization.This moment, the Quilonum Retard dewatered cake that obtains can be cleaned with ion exchanged water etc.
Drying process can use the Quilonum Retard of recovery vacuum-drying, air stream drying, or make up their drying mode.
[embodiment]
To the present invention, enumerate embodiment and carry out brightly specifically, but the present invention does not receive any restriction of these embodiment.
(embodiment 1) utilizes dioxide gas mixed dissolution device to be blown into.CO in the Quilonum Retard lysate
2The meltage of gas is the situation of 500mg/L
To be blended in the soft water (Na concentration 30ppm) of 4000L in the convert Quilonum Retard 200kg of the Na impurity that contains 1800ppm of Na; Circulate the part of slurry in the limit with 40L/min; The limit is made the flow dissolved carbon dioxide gas of MJM mixed cell with 50NL/min with clear with charcoal acid (strain), and in reactive tank, supplies with Soda Ash Light 99.2min..
The circulation and the stirring of slurry carried out on the limit, and the limit was with 4 hours dissolving Quilonum Retards.
CO in the Quilonum Retard lysate of this moment
2The gas dissolving amount is 500mg/L.
To the post-filter that is arranged on circulation line (filtering accuracy: 1 μ m) lead to the Quilonum Retard lysate, remove insoluble impurity.
Quilonum Retard lysate after having carried out filtering uses caustic soda to be adjusted to pH10, is heated to 80 ℃ then, and the limit is stirred 2 hours limits and made dissolved Quilonum Retard recrystallize.
The Quilonum Retard that obtains deposition is filtered with pressure filter, clean behind the water that adheres under 100 ℃ of drying temperatures and carry out drying, obtained the prepared calcium carbonate lithium.Na content in the prepared calcium carbonate lithium that analysis obtains, the result is as shown in table 1 to be 390ppm.
[table 1]
(comparative example 1) directly is blown into dioxide gas with ingress pipe.CO in the Quilonum Retard lysate
2When the meltage of gas is 120mg/L
CO in the Quilonum Retard lysate
2The meltage of gas is 120mg/L.
To be mixed in the soft water (Na concentration 30ppm) of 4000L in the convert Quilonum Retard 200kg of the Na impurity that contains 1800ppm of Na, limit steel basin inner edge directly was blown into dioxide gas 4 hours with ingress pipe with the flow of 40NL/min.
The limit carries out the circulation of slurry and stirs the limit keeping 8 hours, but has undissolved Quilonum Retard.
CO in the Quilonum Retard lysate of this moment
2The meltage of gas is 120mg/L, is extremely low value when comparing with embodiment 1.
Owing to there is undissolved Quilonum Retard, do not utilize removing of the insoluble impurity that filters tank.
Be dissolved with the slurry of a part of Quilonum Retard, use caustic soda to adjust to pH10, be heated to 80 ℃ then, the limit is stirred 2 hours limits and is made dissolved Quilonum Retard recrystallize.
The Quilonum Retard that obtains deposition is filtered with pressure filter, clean the water that adheres to after, under 100 ℃ of drying temperatures, carry out drying, obtained thinking the Quilonum Retard that generates a part.
Na content in the Quilonum Retard that analysis obtains, the result is as shown in table 1 to be 940ppm.
Claims (5)
1. the process for purification of a Quilonum Retard is characterized in that, comprising:
Dissolution process, it is supplied with in the Quilonum Retard slurry that contains impurity and is dissolved with the Soda Ash Light 99.2min. of dioxide gas and circulates, and dissolves the Quilonum Retard slurry thus;
Filter operation, it removes not solvent components from the aqueous solution that is dissolved with Quilonum Retard;
The recrystallize operation, aqueous solution that is dissolved with Quilonum Retard of solvent components heats to removing not for it, makes the carbon dioxide gasification in the aqueous solution, makes the Quilonum Retard recrystallize thus; With
Separation circuit, it separates the Quilonum Retard deposition of recrystallize from the aqueous solution.
2. the process for purification of Quilonum Retard as claimed in claim 1 is characterized in that,
In said dissolution process, the Soda Ash Light 99.2min. of using the preparation of dioxide gas mixed dissolution device to use.
3. according to claim 1 or claim 2 the process for purification of Quilonum Retard is characterized in that,
In said dissolution process, the meltage of the dioxide gas in the Soda Ash Light 99.2min. of using is as more than the 500mg/L.
4. like the process for purification of each described Quilonum Retard in the claim 1～3, it is characterized in that,
In said filtration operation, the container that in by dissolution process, uses makes on the aqueous solution round-robin pipe arrangement strainer is set, and implements not removing of solvent components.
5. like the process for purification of each described Quilonum Retard in the claim 1～4, it is characterized in that,
In said recrystallize operation, the temperature that makes the Quilonum Retard recrystallize is 70 ℃～100 ℃, and the pH of solution is more than 9.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010230958 | 2010-09-27 | ||
| JP2010-230958 | 2010-09-27 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102432043A true CN102432043A (en) | 2012-05-02 |
Family
ID=45980453
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102825541A Pending CN102432043A (en) | 2010-09-27 | 2011-09-21 | Purification method of lithium carbonate |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP5481450B2 (en) |
| KR (1) | KR101283843B1 (en) |
| CN (1) | CN102432043A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110336016A (en) * | 2019-07-16 | 2019-10-15 | 中钢集团南京新材料研究院有限公司 | A kind of preparation method for mixing aluminium LiMn2O4 |
| CN110997568A (en) * | 2017-08-02 | 2020-04-10 | 捷客斯金属株式会社 | Method for dissolving lithium compound, method for producing lithium carbonate, and method for recovering lithium from lithium ion secondary battery scrap |
| CN111122548A (en) * | 2020-01-06 | 2020-05-08 | 江苏容汇通用锂业股份有限公司 | Method for detecting trace metal copper and zinc in lithium carbonate |
| CN112236396A (en) * | 2018-10-29 | 2021-01-15 | 株式会社安积理研 | Lithium carbonate manufacturing device |
| CN112638826A (en) * | 2018-08-31 | 2021-04-09 | 捷客斯金属株式会社 | Method for producing lithium carbonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6682480B2 (en) * | 2017-08-02 | 2020-04-15 | Ｊｘ金属株式会社 | Method for dissolving lithium compound and method for producing lithium carbonate |
| JP6766014B2 (en) * | 2017-08-02 | 2020-10-07 | Ｊｘ金属株式会社 | Lithium Ion Rechargeable Battery How to recover lithium from scrap |
| JP7345728B2 (en) * | 2019-02-25 | 2023-09-19 | 住友金属鉱山株式会社 | How to purify lithium carbonate |
| KR102253829B1 (en) * | 2020-11-27 | 2021-05-21 | 대진대학교 산학협력단 | REMOVAL OF SULFATE IN Li₂CO₃ |
| KR102552102B1 (en) * | 2022-06-09 | 2023-07-06 | 한국선별기 주식회사 | Method For Producing High Purity Lithium Carbonate From Waste Saggar Using Anion Exchange |
| KR102552101B1 (en) * | 2022-06-09 | 2023-07-06 | 한국선별기 주식회사 | Method For Producing High Purity Lithium Carbonate From Waste Saggar |
| EP4372113A1 (en) * | 2022-11-18 | 2024-05-22 | Ascend Elements, Inc. | Lithium recovery from lithium-ion batteries |
Citations (3)
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|---|---|---|---|---|
| JPS62252315A (en) * | 1986-04-23 | 1987-11-04 | Nippon Chem Ind Co Ltd:The | High-purity lithium carbonate and production thereof |
| GB2190668A (en) * | 1986-05-22 | 1987-11-25 | Metaux Speciaux Sa | Process for removing boron from lithium carbonate |
| US20010028871A1 (en) * | 1997-12-09 | 2001-10-11 | Limtech | Process for the purification of lithium carbonate |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4823698A (en) * | 1972-07-29 | 1973-03-27 | ||
| GB1576130A (en) * | 1976-08-10 | 1980-10-01 | Quebec Ministere Des Richesses | Continuous production of lithium carbonate |
| JPS62161973A (en) * | 1985-08-30 | 1987-07-17 | Sumitomo Chem Co Ltd | Production of high-purity lithium carbonate |
| JPH11310414A (en) * | 1998-04-27 | 1999-11-09 | Mitsui Chem Inc | Production of highly pure lithium carbonate |
| JP2003066023A (en) * | 2001-08-21 | 2003-03-05 | Mitsubishi Rayon Co Ltd | Measurement method and control method of gaseous carbon dioxide concentration of artificial carbonate spring, and apparatus for producing artificial carbonate spring |
| JP2005262019A (en) * | 2004-03-16 | 2005-09-29 | Showa Tansan Co Ltd | Apparatus for preparing carbonated water |
| JP4896109B2 (en) * | 2008-10-24 | 2012-03-14 | 日本化学工業株式会社 | Method for producing high purity lithium carbonate |
| JP4896108B2 (en) * | 2008-10-24 | 2012-03-14 | 日本化学工業株式会社 | Method for producing high purity lithium carbonate |
| JP2011032151A (en) * | 2009-08-04 | 2011-02-17 | Kee:Kk | Method of converting lithium carbonate to lithium hydroxide |
-
2011
- 2011-09-14 JP JP2011200762A patent/JP5481450B2/en active Active
- 2011-09-21 CN CN2011102825541A patent/CN102432043A/en active Pending
- 2011-09-26 KR KR1020110096829A patent/KR101283843B1/en active IP Right Grant
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62252315A (en) * | 1986-04-23 | 1987-11-04 | Nippon Chem Ind Co Ltd:The | High-purity lithium carbonate and production thereof |
| GB2190668A (en) * | 1986-05-22 | 1987-11-25 | Metaux Speciaux Sa | Process for removing boron from lithium carbonate |
| US20010028871A1 (en) * | 1997-12-09 | 2001-10-11 | Limtech | Process for the purification of lithium carbonate |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110997568A (en) * | 2017-08-02 | 2020-04-10 | 捷客斯金属株式会社 | Method for dissolving lithium compound, method for producing lithium carbonate, and method for recovering lithium from lithium ion secondary battery scrap |
| TWI718398B (en) * | 2017-08-02 | 2021-02-11 | 日商Ｊｘ金屬股份有限公司 | Method for recovering lithium from lithium ion secondary battery waste |
| CN115433826A (en) * | 2017-08-02 | 2022-12-06 | 捷客斯金属株式会社 | Method for dissolving lithium compound, method for producing lithium carbonate, and method for recovering lithium from lithium ion secondary battery scrap |
| CN112638826A (en) * | 2018-08-31 | 2021-04-09 | 捷客斯金属株式会社 | Method for producing lithium carbonate |
| US11970405B2 (en) | 2018-08-31 | 2024-04-30 | Jx Metals Corporation | Method for producing lithium carbonate |
| CN112236396A (en) * | 2018-10-29 | 2021-01-15 | 株式会社安积理研 | Lithium carbonate manufacturing device |
| CN110336016A (en) * | 2019-07-16 | 2019-10-15 | 中钢集团南京新材料研究院有限公司 | A kind of preparation method for mixing aluminium LiMn2O4 |
| CN111122548A (en) * | 2020-01-06 | 2020-05-08 | 江苏容汇通用锂业股份有限公司 | Method for detecting trace metal copper and zinc in lithium carbonate |
Also Published As
| Publication number | Publication date |
|---|---|
| KR101283843B1 (en) | 2013-07-08 |
| JP5481450B2 (en) | 2014-04-23 |
| KR20120031906A (en) | 2012-04-04 |
| JP2012091999A (en) | 2012-05-17 |
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Application publication date: 20120502 |