CN106830020A - A kind of preparation method of 4N pure Lithium Carbonates - Google Patents
A kind of preparation method of 4N pure Lithium Carbonates Download PDFInfo
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- CN106830020A CN106830020A CN201710152050.5A CN201710152050A CN106830020A CN 106830020 A CN106830020 A CN 106830020A CN 201710152050 A CN201710152050 A CN 201710152050A CN 106830020 A CN106830020 A CN 106830020A
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- lithium
- lithium hydroxide
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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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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a kind of preparation method of 4N pure Lithium Carbonates, it includes step successively：Lithium hydroxide in industrial grade dissolving refined filtration step, carbonization sinker and separating, washing step.It is an advantage of the invention that：Lithium hydroxide in industrial grade need not carry out recrystallization purification, but be directly used in and obtain the pure Lithium Carbonate product that purity is up to more than 99.99% with carbon dioxide reaction.
Description
Technical field
The present invention relates to the preparing technical field of lithium salts, and in particular to a kind of preparation method of 4N pure Lithium Carbonates.
Background technology
With continuing to develop for new energy, 4N pure Lithium Carbonate demands are increasing, and it is high to produce 4N with lithium hydroxide at present
The method of pure lithium carbonate has two kinds：One be with LITHIUM BATTERY lithium hydroxide be that raw material be carbonized and obtains pure Lithium Carbonate, two is to use
Lithium hydroxide in industrial grade is raw material, and recrystallization purification is first carried out to lithium hydroxide in industrial grade, then through the hydrogen after recrystallization purification
Lithia obtains pure Lithium Carbonate with carbon dioxide reaction.It is raw material, LITHIUM BATTERY hydrogen that former approach uses LITHIUM BATTERY lithium hydroxide
Lithia is expensive, causes relatively costly, and latter method needs to carry out lithium hydroxide in industrial grade recrystallization purification, and operation increases
Plus, yield reduction equally causes high cost.
The content of the invention
The present invention is to overcome problems of the prior art and deficiency, there is provided a kind of preparation side of 4N pure Lithium Carbonates
Method, so as to realize that it is raw material to use lithium hydroxide in industrial grade, it is not necessary to carry out recrystallization purification, directly obtained with carbon dioxide reaction
To purity up to the good result of more than 99.99% pure Lithium Carbonate.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of 4N pure Lithium Carbonates, comprises the following steps：
Step one：Take pure water to mix with any ratio with the carbonization mother liquor that step 2 is obtained, be subsequently adding lithium hydroxide in industrial grade and enter
Row dissolving is configured to lithium hydroxide solution, then secondary filter is carried out to lithium hydroxide solution with film obtains lithium hydroxide refined filtration liquid,
And EDTA is added in lithium hydroxide refined filtration liquid, and stir after an EDTA fully dissolves and obtain lithium hydroxide refined soln；
Step 2：The carbonization mother liquor for first adding a certain amount of pure water to be obtained with step 2 in the carbonization sinker kettle with overfall
Bottom liquid is warmed up to 80~98 DEG C by any mixed liquor than mixing as bottom liquid, then keeps 80~98 DEG C in stirring
Lower synchronization is toward the continuous lithium hydroxide refined soln for adding step one to obtain in the liquid of bottom and continuously toward logical carbon dioxide in the liquid of bottom
Carry out carbonization sinker reaction, the addition speed of lithium hydroxide refined soln and carbon dioxide is controlling the pH value of bottom liquid 10~14
It is advisable, the lithium carbonate slurry that carbonization sinker is obtained overflows into centrifuge from reactor overfall and is centrifuged and washes
Wash, so as to obtain carbonization mother liquor and wet pure Lithium Carbonate solid, wet pure Lithium Carbonate solid obtains purity and reaches after drying
More than 99.99% pure Lithium Carbonate product.
It is preferred that step one described in lithium hydroxide solution in lithium content be 35~45g/L.
It is preferred that step one described in lithium hydroxide refined filtration liquid in add EDTA amount be：Every cubic metre of lithium hydroxide essence
Filtrate adds 0.02~1 kilogram of EDTA.
The carbonization mother liquor generated in preferred step 2 can be used in step one with water arbitrarily than the dissolving lithium hydroxide that dissolves each other,
Also can be used in step 2 plus be used as bottom liquid in a kettle..
Compared with prior art, it is an advantage of the invention that：Present invention lithium hydroxide in industrial grade is raw material, is not required to technical grade hydrogen
Lithia carries out recrystallization purification, but purity up to more than 99.99% pure Lithium Carbonate is directly obtained with carbon dioxide reaction.
Specific embodiment：
Embodiment 1
Step one：3000L pure water is added in the dissolving tank of 5000L, adds lithium hydroxide in industrial grade to be filled after opening stirring
Divide dissolving to be configured to the lithium hydroxide solution containing lithium for 35g/L, secondary filter then is carried out to lithium hydroxide solution with film and is obtained
Lithium hydroxide refined filtration liquid, and add 5 kilograms of EDTA stirring fully to dissolve EDTA in lithium hydroxide refined filtration liquid to obtain hydroxide
Lithium refined soln；
Step 2：The pure water of 500L is first added to make bottom liquid, and stirring in the carbonization sinker kettle with overfall of 1000L
It is lower that bottom liquid is warmed up to 80 DEG C, 80 DEG C are then kept in the synchronous hydrogen-oxygen obtained toward continuous plus step one in the liquid of bottom under stirring
Change lithium refined soln carries out carbonization sinker reaction, control lithium hydroxide refined soln with continuous toward logical carbon dioxide in the liquid of bottom
With the addition speed of carbon dioxide so that it is 14 to maintain the pH value of bottom liquid, from the carbon that the carbonization sinker continuous overflow of kettle overfall goes out
Sour lithium slurry is centrifuged and is washed by centrifuge, just obtains carbonization mother liquor and wet pure Lithium Carbonate solid, wet
Pure Lithium Carbonate solid obtains the pure Lithium Carbonate product that purity is up to more than 99.99% after drying.
Embodiment 2
Step one：The carbonization mother liquor that step 2 is obtained in adding 3000L embodiments 1 in the dissolving tank of 5000L, after opening stirring
Add lithium hydroxide in industrial grade to carry out fully dissolving and be configured to the lithium hydroxide solution for 45g/L containing lithium, then with film to hydrogen-oxygen
Change lithium solution carries out secondary filter and obtains lithium hydroxide refined filtration liquid, and adds 0.1 kilogram of EDTA to stir in lithium hydroxide refined filtration liquid
Mix an EDTA and fully dissolve and obtain lithium hydroxide refined soln；
Step 2：The carbon that step 2 is obtained in first adding 500L embodiments 1 in the carbonization sinker kettle with overfall of 1000L
Change mother liquor and make bottom liquid, and lower bottom liquid of stirring is warmed up to 98 DEG C, then keeps 98 DEG C in synchronous toward bottom liquid under stirring
In the lithium hydroxide refined soln that obtains of continuous plus step one and continuous carry out carbonization sinker toward logical carbon dioxide in the liquid of bottom
The addition speed of reaction, control lithium hydroxide refined soln and carbon dioxide, so that the pH value for maintaining bottom liquid is 12, it is heavy from carbonization
The lithium carbonate slurry that the continuous overflow of lithium kettle overfall goes out is centrifuged and is washed by centrifuge, just obtain carbonization mother liquor and
Wet pure Lithium Carbonate solid, wet pure Lithium Carbonate solid obtains the pure Lithium Carbonate that purity is up to more than 99.99% after drying
Product.
Embodiment 3
Step one：The carbonization that step 2 is obtained in adding 2000L pure water and 1000L embodiments 1 in the dissolving tank of 5000L is female
Liquid, it is the lithium hydroxide of 40g/L lithium hydroxide in industrial grade to be added after unlatching stirring mixing and carry out fully dissolving to be configured to contain lithium
Solution, then carries out secondary filter with film to lithium hydroxide solution and obtains lithium hydroxide refined filtration liquid, and in lithium hydroxide refined filtration liquid
2 kilograms of EDTA stirrings of middle addition are fully dissolved EDTA and obtain lithium hydroxide refined soln；
Step 2：Step in first adding 200L pure water and 300L embodiments 1 in the carbonization sinker kettle with overfall of 1000L
Two carbonization mother liquors for obtaining make bottom liquid, and lower bottom liquid of stirring is warmed up to 90 DEG C, then keep 90 DEG C under stirring
The lithium hydroxide refined soln for synchronously being obtained toward continuous plus step one in the liquid of bottom enters with continuous toward logical carbon dioxide in the liquid of bottom
The addition speed of row carbonization sinker reaction, control lithium hydroxide refined soln and carbon dioxide, so that the pH value for maintaining bottom liquid is
10, the lithium carbonate slurry gone out from the carbonization sinker continuous overflow of kettle overfall is centrifuged and is washed by centrifuge, just
To carbonization mother liquor and wet pure Lithium Carbonate solid, wet pure Lithium Carbonate solid obtains purity up to more than 99.99% after drying
Pure Lithium Carbonate product.
The pure Lithium Carbonate product sampling analysis detection for being obtained to embodiment 1-3 respectively, each component content is as follows in sample：
As seen from the above table, the pure Lithium Carbonate product that preparation method of the present invention is obtained is not required to tie lithium hydroxide in industrial grade again
Crystalline substance purification, but purity up to more than 99.99% pure Lithium Carbonate is directly obtained with carbon dioxide reaction.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (4)
1. a kind of preparation method of 4N pure Lithium Carbonates, it is characterised in that：Comprise the following steps：Step one：Take pure water and step
With any than mixing, be subsequently adding lithium hydroxide in industrial grade carries out dissolving to be configured to lithium hydroxide molten two carbonization mother liquors for obtaining
Liquid, then carry out secondary filter to lithium hydroxide solution with film and obtain lithium hydroxide refined filtration liquid, and in lithium hydroxide refined filtration liquid plus
Enter EDTA, and stir after an EDTA fully dissolves and obtain lithium hydroxide refined soln；
Step 2：The carbonization mother liquor for first adding a certain amount of pure water to be obtained with step 2 in the carbonization sinker kettle with overfall
Bottom liquid is warmed up to 80~98 DEG C by any mixed liquor than mixing as bottom liquid, then keeps 80~98 DEG C in stirring
Lower synchronization is toward the continuous lithium hydroxide refined soln for adding step one to obtain in the liquid of bottom and continuously toward logical carbon dioxide in the liquid of bottom
Carry out carbonization sinker reaction, the addition speed of lithium hydroxide refined soln and carbon dioxide is controlling the pH value of bottom liquid 10~14
It is advisable, the lithium carbonate slurry that carbonization sinker is obtained overflows into centrifuge from reactor overfall and is centrifuged and washes
Wash, so as to obtain carbonization mother liquor and wet pure Lithium Carbonate solid, wet pure Lithium Carbonate solid obtains purity and reaches after drying
More than 99.99% pure Lithium Carbonate product.
2. the preparation method of 4N pure Lithium Carbonates according to claim 1, it is characterised in that：Hydrogen-oxygen described in step one
The content for changing lithium in lithium solution is 35~45g/L.
3. the preparation method of 4N pure Lithium Carbonates according to claim 1, it is characterised in that：Hydrogen-oxygen described in step one
The amount of addition EDTA is in change lithium refined filtration liquid：Every cubic metre of lithium hydroxide refined filtration liquid adds 0.02~1 kilogram of EDTA.
4. the preparation method of 4N pure Lithium Carbonates according to claim 1, it is characterised in that：The carbonization generated in step 2
Mother liquor can be used in step one with water arbitrarily than the dissolving lithium hydroxide that dissolves each other, and also can be used in step 2 plus is used as in a kettle.
Bottom liquid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107792868A (en) * | 2017-12-01 | 2018-03-13 | 响水台舍化工有限公司 | A kind of lithium carbonate refines purifying plant |
| CN110980777A (en) * | 2019-12-25 | 2020-04-10 | 青海奥瑞泰克化工科技有限公司 | Method for preparing purification additive and purification additive prepared by the method |
| CN113003588A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Nuclear pure grade Li2CO3Chemical conversion method |
| CN113651343A (en) * | 2021-08-27 | 2021-11-16 | 中国船舶重工集团公司第七一八研究所 | Method for preparing high-purity lithium carbonate by recycling lithium hydroxide for air purification |
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| CN102020295A (en) * | 2010-12-22 | 2011-04-20 | 四川天齐锂业股份有限公司 | Preparation method of high-purity lithium carbonate |
| CN102030346A (en) * | 2009-09-25 | 2011-04-27 | 上海中锂实业有限公司 | Preparation method for lithium carbonate |
| CN102491377A (en) * | 2011-12-14 | 2012-06-13 | 江南大学 | Lithium hydroxide purifying method |
| CN103408041A (en) * | 2013-08-22 | 2013-11-27 | 四川国理锂材料有限公司 | Lithium carbonate production technology |
| CN105819472A (en) * | 2016-03-09 | 2016-08-03 | 江苏容汇通用锂业股份有限公司 | Method for producing highly-pure battery grade lithium carbonate by using lithium sulfate solution |
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2017
- 2017-03-15 CN CN201710152050.5A patent/CN106830020B/en active Active
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| CN102030346A (en) * | 2009-09-25 | 2011-04-27 | 上海中锂实业有限公司 | Preparation method for lithium carbonate |
| CN102020295A (en) * | 2010-12-22 | 2011-04-20 | 四川天齐锂业股份有限公司 | Preparation method of high-purity lithium carbonate |
| CN102491377A (en) * | 2011-12-14 | 2012-06-13 | 江南大学 | Lithium hydroxide purifying method |
| CN103408041A (en) * | 2013-08-22 | 2013-11-27 | 四川国理锂材料有限公司 | Lithium carbonate production technology |
| CN105819472A (en) * | 2016-03-09 | 2016-08-03 | 江苏容汇通用锂业股份有限公司 | Method for producing highly-pure battery grade lithium carbonate by using lithium sulfate solution |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107792868A (en) * | 2017-12-01 | 2018-03-13 | 响水台舍化工有限公司 | A kind of lithium carbonate refines purifying plant |
| CN113003588A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Nuclear pure grade Li2CO3Chemical conversion method |
| CN110980777A (en) * | 2019-12-25 | 2020-04-10 | 青海奥瑞泰克化工科技有限公司 | Method for preparing purification additive and purification additive prepared by the method |
| CN110980777B (en) * | 2019-12-25 | 2022-09-09 | 青海奥瑞泰克化工科技有限公司 | Method for preparing purification additive and purification additive prepared by the method |
| CN113651343A (en) * | 2021-08-27 | 2021-11-16 | 中国船舶重工集团公司第七一八研究所 | Method for preparing high-purity lithium carbonate by recycling lithium hydroxide for air purification |
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