CN106830020B - 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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- CN106830020B CN106830020B CN201710152050.5A CN201710152050A CN106830020B CN 106830020 B CN106830020 B CN 106830020B CN 201710152050 A CN201710152050 A CN 201710152050A CN 106830020 B CN106830020 B CN 106830020B
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- lithium hydroxide
- lithium
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- bottom liquid
- carbonization
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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
Abstract
The present invention relates to a kind of preparation methods of 4N pure Lithium Carbonates, include step successively：Lithium hydroxide in industrial grade dissolves refined filtration step, carbonization sinker and separating, washing step.It is an advantage of the invention that：Lithium hydroxide in industrial grade is directly used in without carrying out recrystallization purification and obtains purity up to 99.99% or more pure Lithium Carbonate product with carbon dioxide reaction.
Description
Technical field
The present invention relates to the preparing technical fields of lithium salts, and in particular to a kind of preparation method of 4N pure Lithium Carbonates.
Background technology
With the continuous development of new energy, 4N pure Lithium Carbonate demands are increasing, produce 4N high with lithium hydroxide at present
There are two ways to pure lithium carbonate：First, with LITHIUM BATTERY lithium hydroxide it is that raw material is carbonized to obtain pure Lithium Carbonate, second is that with
Lithium hydroxide in industrial grade is raw material, first carries out recrystallization purification to lithium hydroxide in industrial grade, then the hydrogen after recrystallization purifies
Lithia obtains pure Lithium Carbonate with carbon dioxide reaction.Former approach uses LITHIUM BATTERY lithium hydroxide for raw material, LITHIUM BATTERY hydrogen
Lithia is expensive, causes cost higher, and latter method needs to carry out recrystallization purification to lithium hydroxide in industrial grade, and process increases
Add, yield reduces, and equally causes of high cost.
Invention content
The present invention is to overcome problems of the prior art and deficiency, provides a kind of preparation side of 4N pure Lithium Carbonates
Method uses lithium hydroxide in industrial grade for raw material to realize, need not carry out recrystallization purification, directly be obtained with carbon dioxide reaction
To purity up to the good result of 99.99% or more 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, includes the following steps：
Step 1：It takes the carbonization mother liquor that pure water is obtained with step 2 to be mixed with arbitrary ratio, technical grade hydroxide is then added
Lithium carries out dissolving and is configured to lithium hydroxide solution, then carries out secondary filter to lithium hydroxide solution with film and obtain 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 that a certain amount of pure water is obtained with step 2 is first added in the carbonization sinker kettle with overflow port
Bottom liquid is warming up to 80~98 DEG C by mother liquor arbitrarily than mixed mixed liquor as bottom liquid, and then 80~98 DEG C of holding is in stirring
The lithium hydroxide refined soln for continuously adding step 1 to obtain into bottom liquid and continuous carbon dioxide logical into bottom liquid are synchronized under state
Gas carries out carbonization sinker and reacts, and the addition speed of lithium hydroxide refined soln and carbon dioxide is to control the pH value of bottom liquid 10
~14 are advisable, the obtained lithium carbonate slurry of carbonization sinker overflowed into from reaction kettle overflow port to centrifuge be centrifuged and
Washing, to obtain carbonization mother liquor and wet pure Lithium Carbonate solid, wet pure Lithium Carbonate solid obtains purity after drying
Up to 99.99% or more pure Lithium Carbonate product.
The content of lithium is 35~45g/L in lithium hydroxide solution described in preferred step 1.
The amount of addition EDTA is in lithium hydroxide refined filtration liquid described in preferred step 1：Every cubic metre of lithium hydroxide essence
0.02~1 kilogram of EDTA is added in filtrate.
The carbonization mother liquor generated in preferred step 2 can be used in step 1 arbitrarily dissolves lithium hydroxide with water than dissolving each other,
Also it can be used in step 2 plus be used as in a kettle bottom liquid.
Compared with prior art, it is an advantage of the invention that：The present invention is raw material with lithium hydroxide in industrial grade, is not required to industry
Grade lithium hydroxide carries out recrystallization purification, but purity is directly obtained with carbon dioxide reaction up to 99.99% or more high-purity carbonic acid
Lithium.
Specific implementation mode：
Embodiment 1
Step 1：In the dissolving tank of 5000L be added 3000L pure water, open stirring after be added lithium hydroxide in industrial grade into
Row fully dissolving is configured to, containing the lithium hydroxide solution that lithium is 35g/L, then carry out secondary filter to lithium hydroxide solution with film
It obtains lithium hydroxide refined filtration liquid, and in lithium hydroxide refined filtration liquid 5 kilograms of EDTA stirrings is added EDTA is fully dissolved and obtain hydrogen
Lithia refined soln；
Step 2：The pure water that 500L is first added in the carbonization sinker kettle with overflow port of 1000L makees bottom liquid, and stirs
Lower bottom liquid of state is warming up to 80 DEG C, then keeps 80 DEG C to be synchronized under stirring and continuously step 1 is added to obtain into bottom liquid
Lithium hydroxide refined soln and the continuous carbon dioxide gas that leads into bottom liquid carry out carbonization sinker reaction, and control lithium hydroxide is refined
The addition speed of solution and carbon dioxide is 14 to maintain the pH value of bottom liquid, goes out from the carbonization continuous overflow of sinker kettle overflow port
Lithium carbonate slurry be centrifuged and wash by centrifuge, just obtain carbonization mother liquor and wet pure Lithium Carbonate solid,
Wet pure Lithium Carbonate solid obtains purity up to 99.99% or more pure Lithium Carbonate product after drying.
Embodiment 2
Step 1：The carbonization mother liquor that step 2 obtains in 3000L embodiments 1 is added in the dissolving tank of 5000L, unlatching is stirred
Lithium hydroxide in industrial grade is added after mixing to carry out fully dissolving the lithium hydroxide solution being configured to containing lithium for 45g/L, then with film pair
Lithium hydroxide solution carries out secondary filter and obtains lithium hydroxide refined filtration liquid, and 0.1 kilogram is added in lithium hydroxide refined filtration liquid
EDTA stirrings, which fully dissolve EDTA, obtains lithium hydroxide refined soln；
Step 2：Step 2 in 500L embodiments 1 is first added in the carbonization sinker kettle with overflow port of 1000L to obtain
Carbonization mother liquor make bottom liquid, and lower bottom liquid of stirring is warming up to 98 DEG C, then keep 98 DEG C synchronized under stirring it is past
The lithium hydroxide refined soln that step 1 obtains continuously is added to be carbonized with the continuous carbon dioxide gas that leads into bottom liquid in the liquid of bottom
Sinker reacts, and controls the addition speed of lithium hydroxide refined soln and carbon dioxide, is 12 to maintain the pH value of bottom liquid, from carbon
Change the lithium carbonate slurry that the continuous overflow of sinker kettle overflow port goes out to be centrifuged and wash by centrifuge, it is female just to obtain carbonization
Liquid and wet pure Lithium Carbonate solid, wet pure Lithium Carbonate solid obtain purity up to 99.99% or more high-purity carbon after drying
Sour lithium product.
Embodiment 3
Step 1：The carbonization that step 2 obtains in 2000L pure water and 1000L embodiments 1 is added in the dissolving tank of 5000L
Mother liquor, unlatching add lithium hydroxide in industrial grade and carry out fully dissolving the hydroxide being configured to containing lithium for 40g/L after being stirred
Then lithium solution carries out secondary filter to lithium hydroxide solution with film and obtains lithium hydroxide refined filtration liquid, and in lithium hydroxide refined filtration
2 kilograms of EDTA stirrings of addition, which fully dissolve EDTA, in liquid obtains lithium hydroxide refined soln；
Step 2：It is first added in 200L pure water and 300L embodiments 1 in the carbonization sinker kettle with overflow port of 1000L
The carbonization mother liquor that step 2 obtains makees bottom liquid, and lower bottom liquid of stirring is warming up to 90 DEG C, and then 90 DEG C of holding is in stirring shape
The lithium hydroxide refined soln for continuously adding step 1 to obtain into bottom liquid and continuous carbon dioxide gas logical into bottom liquid are synchronized under state
Body carries out carbonization sinker reaction, the addition speed of lithium hydroxide refined soln and carbon dioxide is controlled, to maintain the pH of bottom liquid
Value is 10, and the lithium carbonate slurry gone out from the carbonization continuous overflow of sinker kettle overflow port is centrifuged and is washed by centrifuge,
Just carbonization mother liquor and wet pure Lithium Carbonate solid are obtained, wet pure Lithium Carbonate solid obtains purity up to 99.99% after drying
Above pure Lithium Carbonate product.
The pure Lithium Carbonate product sampling analysis that embodiment 1-3 is obtained is detected 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 obtains is not required to carry out lithium hydroxide in industrial grade
Recrystallization purification, but purity is directly obtained with carbon dioxide reaction up to 99.99% or more pure Lithium Carbonate.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (1)
1. a kind of preparation method of 4N pure Lithium Carbonates, it is characterised in that：Include the following steps：Step 1：Add in dissolving tank
Enter pure water, addition lithium hydroxide in industrial grade carries out dissolving to be configured to the content of lithium being 35~45g/L lithium hydroxides after opening stirring
Solution, then secondary filter is carried out to lithium hydroxide solution with film and obtains lithium hydroxide refined filtration liquid, and in every cubic metre of lithium hydroxide
0.02~1 kilogram of EDTA is added in refined filtration liquid, and stirs after an EDTA fully dissolves and obtains lithium hydroxide refined soln；
Step 2：A certain amount of pure water is first added in the carbonization sinker kettle with overflow port and makees bottom liquid, and bottom liquid is warming up to
80~98 DEG C, 80~98 DEG C are then kept to synchronize the lithium hydroxide essence for continuously adding step 1 to obtain into bottom liquid under stirring
Solution processed and the continuous carbon dioxide gas that leads into bottom liquid carry out carbonization sinker reaction, lithium hydroxide refined soln and carbon dioxide
Addition speed be advisable 10~14 with the pH value for controlling bottom liquid, the obtained lithium carbonate slurry of carbonization sinker is from reaction kettle overflow port
Centrifuge is overflowed into be centrifuged and wash, it is wet to obtain carbonization mother liquor and wet pure Lithium Carbonate solid
Pure Lithium Carbonate solid obtains purity up to 99.99% or more pure Lithium Carbonate product after drying；It is generated in the step 2
Carbonization mother liquor is in step 1 with water arbitrarily than the bottom liquid for dissolving lithium hydroxide or adding in step 2 in a kettle that dissolves each other.
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| 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 |
| 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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| 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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Patent Citations (5)
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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 |
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