CN109264749A - The comprehensive recovering process of the fluorination slag containing lithium - Google Patents
The comprehensive recovering process of the fluorination slag containing lithium Download PDFInfo
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- CN109264749A CN109264749A CN201811148387.XA CN201811148387A CN109264749A CN 109264749 A CN109264749 A CN 109264749A CN 201811148387 A CN201811148387 A CN 201811148387A CN 109264749 A CN109264749 A CN 109264749A
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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
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/02—Fluorides
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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 comprehensive recovering process of fluorination slag containing lithium, method includes the following steps: the fluorination slag containing lithium adds water slurrying, then sulfuric acid are added into slurry, are heated to 100-200 DEG C, react 1-10h；Collect and react gas generated, be passed through in strong alkali solution, can gradually there is solid precipitation in strong alkali solution, solid is filtered, washed, dry after obtain sodium fluoride；The solution obtained after reaction is crude lithium sulfate solution, adds alkaline reagent to adjust solution ph to 12, obtains refined sulfuric acid lithium solution after being filtered to remove impurity, saturated sodium carbonate solution is added thereto, obtain crude lithium carbonate, prepared calcium carbonate lithium is obtained after washing and drying.The method of the present invention realizes the synthetical recovery containing lithium and fluorine in lithium fluorination slag, and no waste residue generates, and the lithium rate of recovery is high, at low cost, has considerable economic benefit.
Description
Technical field
The invention belongs to the recycling fields of high value waste resource, and in particular to the synthetical recovery side of the fluorination slag containing lithium
Method.
Background technique
Lithium carbonate is a kind of important lithium compound, for producing the compound, lithium metal and its isotope of various lithiums；Also
It is used to prepare the catalyst of chemical reaction；Semiconductor, ceramics, TV, medicine and atomic energy industry also have application.In analytical chemistry
In be used as analytical reagent；Also there is application in lithium ion battery；It is used in cement additive as coagulant.
Sodium fluoride is a kind of important fluoride salt, is the raw material for manufacturing other fluorides.Sodium fluoride tool has been widely used:
It can be used as the fluxing agent and shading of agricultural fungicides, fungicide, timber preservative, drinking water treatment agent and glass-ceramic and enamel
Agent；It can also be used in the cleaning of steel or other metals；It can also be used to manufacture ceramic paint, boiling steel；It can also be used in leather industry
Rawhide and epidermis processing；Furthermore sodium fluoride applies also for enamel medical industry and paper production and construction material etc..
There are individual reports (such as 104,241,724 102,515,203 107777712 A of B, CN of A, CN of CN) to be related to containing at present
Lithium is fluorinated the recovery processing technique of slag, but is all only conceived to the recycling of lithium, and the recycling of fluorine resource is not paid attention to and closed
Note, results in waste of resources, being far from being is comprehensive recovery method.
104787784 B of Chinese invention patent CN discloses a kind of method that recycling waste material containing lithium fluoride prepares lithium salts, should
Method will contain lithium fluoride waste material and add the slurrying of water acid adding plus calcium salt conversion plus alkaline matter neutralization, tone pitch, purification, evaporation and concentration,
Lithium fluoride is transformed into calcium fluoride precipitate and corresponding lithium salt solution.But the patented technology process route is long, gained byproduct fluorine
It is low to change calcium added value, it is at high cost.
Summary of the invention
In order to overcome the above-mentioned prior art containing disadvantage in lithium fluorination slag for comprehensive recycling and insufficient, it is an object of the invention to
A kind of comprehensive recovering process of fluorination slag containing lithium is provided.
The purpose of the invention is achieved by the following technical solution:
A kind of comprehensive recovering process of the fluorination slag containing lithium, comprising the following steps:
(1) the fluorination slag containing lithium adds water slurrying, then sulfuric acid is added into slurry, is heated to 100-200 DEG C, reacts 1-10h；
The fluorination slag containing lithium mostlys come from lithium electricity recycling industry, lithium salts industry, glass industry and pharmaceutical industry etc.,
Wherein lithium content is 3-30%wt, other cations summations are 3-30%wt；Other described cations include hydrogen, sodium,
Potassium, ammonium, calcium, magnesium, aluminium, iron, nickel, cobalt, manganese, titanium and vanadium；
The dosage of the sulfuric acid is 0.5-5.0 times of lithium mole, the preferred 30-98% of the concentration of sulfuric acid (V/V)；Herein only
Sulfuric acid, hydrochloric acid, nitric acid high volatility can be used, meeting preferential volatilization is not suitable for；
The preferred oil bath heating of the heating；
(2) collection step (1) reacts gas generated, is passed through in strong alkali solution, can gradually have in strong alkali solution
Solid be precipitated, solid is filtered, washed, dry after obtain sodium fluoride；
The aqueous solution of the preferred sodium hydroxide of the strong alkali solution or sodium carbonate；
(3) obtained solution is crude lithium sulfate solution after step (1) reaction, add alkaline reagent adjust solution ph to
12, refined sulfuric acid lithium solution is obtained after being filtered to remove impurity, saturated sodium carbonate solution is added thereto, obtains crude lithium carbonate,
Prepared calcium carbonate lithium is obtained after washing and drying；
The preferred sodium carbonate of the alkaline reagent and/or lithium carbonate, effect are to remove the impurity such as nickel cobalt manganese calcium and magnesium.
Mechanism of the invention is, with lithium fluoride and sulfuric acid reaction, using the volatility for generating hydrogen fluoride in product, by it
It volatilizees in gaseous form, uses alkaline solution absorption afterwards, it is small using sodium fluoride solubility, obtain sodium fluoride product.
2LiF+H2SO4=Li2SO4+2HF↑
HF+NaOH=NaF ↓+H2O
2HF+Na2CO3=2NaF ↓+H2O+CO2↑
The present invention has the following advantages and effects with respect to the prior art:
1, using lithium carbonate made from the method for the present invention, purity 99.5% or more, aluminium, iron, copper, magnesium, nickel, manganese, zinc,
Lead, potassium content 0.002% hereinafter, sodium content 0.025% hereinafter, having reached battery-level lithium carbonate quality standard.
2, using sodium fluoride made from the method for the present invention, purity reaches industrial grade standard 98% or more.
3, the method for the present invention realizes the synthetical recovery containing lithium and fluorine in lithium fluorination slag, and no waste residue generates, and the lithium rate of recovery is high,
It is at low cost, there is considerable economic benefit.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
A kind of comprehensive recovering process of the fluorination slag containing lithium, comprising the following steps:
(1) the fluorination slag of lithium content 13.6%wt, sodium content 3.5%wt, nickel content 4.1%wt, content of magnesium 4.9%wt are taken
100g adds water 100ml stirring pulping；
(2) sulfuric acid that 400ml concentration is 50% is slowly added into slurry；
(3) 120 DEG C are warming up to, 6h is stirred to react；
(4) gas collected above reactor is passed through in 30% sodium hydroxide solution and is absorbed；
(5) after fully reacting, sodium hydroxide solution is filtered, obtained white precipitate washing and drying, obtains sodium fluoride production
Product, reach technical grade requirement, and specific ingredient see the table below 1.
(6) sodium carbonate is added into the crude lithium sulfate solution that fluorine removal obtains after complete, adjusts pH value to 12, is obtained by filtration
Refined sulfuric acid lithium solution；
(7) saturated sodium carbonate solution is added into refined sulfuric acid lithium solution, obtains crude lithium carbonate, is obtained after washing and drying
Prepared calcium carbonate lithium product, reaches LITHIUM BATTERY requirement, and specific ingredient see the table below 2.
The purity and impurity content of 1 embodiment of table, 1 gained sodium fluoride
| Ingredient | NaF | SiO2 | Na2CO3 | SO4 2- | Acidity | Water-insoluble | Moisture |
| Content/% | 99.26 | 0.01 | 0.01 | 0.01 | 0 | 0.02 | 0.31 |
The purity and impurity content of 2 embodiment of table, 1 gained lithium carbonate
| Ingredient | Li2CO3 | Na | K | Si | Al | Ca | Mg | Fe |
| Content/% | 99.82 | 0.0121 | 0.0005 | 0.0021 | 0.0001 | 0.0031 | 0.0007 | 0.0004 |
| Ingredient | Cu | Ni | Mn | Zn | Pb | Cl- | SO4 2- | |
| Content/% | 0.0005 | 0.0002 | 0.0003 | 0.0008 | 0.0007 | 0.0025 | 0.0243 |
Embodiment 2
A kind of comprehensive recovering process of the fluorination slag containing lithium, comprising the following steps:
(1) the fluorination slag 100g for taking lithium content 23.4%wt, cobalt content 5.1%wt, adds water 100ml stirring pulping；
(2) sulfuric acid that 200ml concentration is 98% is slowly added into slurry；
(3) 160 DEG C are warming up to, 4h is stirred to react；
(4) gas collected above reactor is passed through in 15% sodium carbonate liquor and is absorbed；
(5) after fully reacting, sodium carbonate liquor is filtered, obtained white precipitate washing and drying obtains sodium fluoride product,
Reach technical grade requirement, specific ingredient see the table below 3.
(6) sodium carbonate is added into the crude lithium sulfate solution that fluorine removal obtains after complete, adjusts pH value to 12, is obtained by filtration
Refined sulfuric acid lithium solution；
(7) saturated sodium carbonate solution is added into refined sulfuric acid lithium solution, obtains crude lithium carbonate, is obtained after washing and drying
Prepared calcium carbonate lithium product, reaches LITHIUM BATTERY requirement, and specific ingredient see the table below 4.
The purity and impurity content of 3 embodiment of table, 2 gained sodium fluoride
| Ingredient | NaF | SiO2 | Na2CO3 | SO4 2- | Acidity | Water-insoluble | Moisture |
| Content/% | 98.61 | 0.01 | 0.35 | 0.01 | 0 | 0.02 | 0.29 |
The purity and impurity content of 4 embodiment of table, 2 gained lithium carbonate
| Ingredient | Li2CO3 | Na | K | Si | Al | Ca | Mg | Fe |
| Content/% | 99.77 | 0.0089 | 0.0006 | 0.0024 | 0.0001 | 0.0027 | 0.0005 | 0.0002 |
| Ingredient | Cu | Ni | Mn | Zn | Pb | Cl- | SO4 2- | |
| Content/% | 0.0003 | 0.0001 | 0.0003 | 0.0009 | 0.0007 | 0.0022 | 0.0187 |
Embodiment 3
A kind of comprehensive recovering process of the fluorination slag containing lithium, comprising the following steps:
(1) the fluorination slag of lithium content 7.6%wt, sodium content 3.8%wt, manganese content 5.7%wt, calcium content 3.5%wt are taken
100g adds water 100ml stirring pulping；
(2) sulfuric acid that 100ml concentration is 75% is slowly added into slurry；
(3) 140 DEG C are warming up to, 8h is stirred to react；
(4) gas collected above reactor is passed through in 30% sodium hydroxide solution and is absorbed；
(5) after fully reacting, sodium hydroxide solution is filtered, obtained white precipitate washing and drying, obtains sodium fluoride production
Product, reach technical grade requirement, and specific ingredient see the table below 5.
(6) sodium carbonate is added into the crude lithium sulfate solution that fluorine removal obtains after complete, adjusts pH value to 12, is obtained by filtration
Refined sulfuric acid lithium solution；
(7) saturated sodium carbonate solution is added into refined sulfuric acid lithium solution, obtains crude lithium carbonate, is obtained after washing and drying
Prepared calcium carbonate lithium product, reaches LITHIUM BATTERY requirement, and specific ingredient see the table below 6.
The purity and impurity content of 5 embodiment of table, 3 gained sodium fluoride
| Ingredient | NaF | SiO2 | Na2CO3 | SO4 2- | Acidity | Water-insoluble | Moisture |
| Content/% | 99.35 | 0.01 | 0.01 | 0.01 | 0 | 0.01 | 0.23 |
The purity and impurity content of 6 embodiment of table, 3 gained lithium carbonate
| Ingredient | Li2CO3 | Na | K | Si | Al | Ca | Mg | Fe |
| Content/% | 99.84 | 0.096 | 0.0004 | 0.0028 | 0.0002 | 0.0025 | 0.0004 | 0.0001 |
| Ingredient | Cu | Ni | Mn | Zn | Pb | Cl- | SO4 2- | |
| Content/% | 0.0004 | 0.0001 | 0.0003 | 0.0006 | 0.0006 | 0.0017 | 0.0126 |
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. a kind of comprehensive recovering process of the fluorination slag containing lithium, it is characterised in that the following steps are included:
(1) the fluorination slag containing lithium adds water slurrying, then sulfuric acid is added into slurry, is heated to 100-200 DEG C, reacts 1-10h；
(2) collection step (1) reacts gas generated, is passed through in strong alkali solution, can gradually there is solid in strong alkali solution
Be precipitated, solid is filtered, washed, dry after obtain sodium fluoride；
Strong alkali solution described in step (2) is the aqueous solution of sodium hydroxide or sodium carbonate；
(3) obtained solution is crude lithium sulfate solution after step (1) reaction, adds alkaline reagent to adjust solution ph to 12, mistake
Refined sulfuric acid lithium solution is obtained after filtering out decontamination, saturated sodium carbonate solution is added thereto, obtains crude lithium carbonate, washing is dried
Prepared calcium carbonate lithium is obtained after dry；
Alkaline reagent described in step (3) is sodium carbonate and/or lithium carbonate.
2. according to the method described in claim 1, wherein lithium content is it is characterized by: being fluorinated slag containing lithium described in step (1)
3-30%wt.
3. according to the method described in claim 1, it is characterized by: described in step (1) containing lithium be fluorinated slag, wherein other sun from
Sub- content summation is 3-30%wt；Other described cations include hydrogen, sodium, potassium, ammonium, calcium, magnesium, aluminium, iron, nickel, cobalt, manganese, titanium
And vanadium.
4. according to the method described in claim 1, it is characterized by: the dosage of step (1) described sulfuric acid is lithium mole
0.5-5.0 times.
5. according to the method described in claim 1, it is characterized by: the concentration of step (1) described sulfuric acid is 30-98% (V/V).
6. according to the method described in claim 1, it is characterized by: being heated to be oil bath heating described in step (1).
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Cited By (6)
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| CN110451535A (en) * | 2019-08-15 | 2019-11-15 | 湖南顺华锂业有限公司 | A kind of method of lithium sulfate solution purification and impurity removal |
| CN110736805A (en) * | 2019-08-28 | 2020-01-31 | 广西银亿高新技术研发有限公司 | method for measuring content of aluminum ions in lithium solution containing fluorine and aluminum |
| CN112320820A (en) * | 2020-10-27 | 2021-02-05 | 贵州省化工研究院 | Method for producing high-purity sodium fluoride by utilizing fluosilicic acid in phosphoric acid |
| CN112897558A (en) * | 2021-02-23 | 2021-06-04 | 四川思达能环保科技有限公司 | Method for preparing lithium carbonate by taking lithium fluoride mother liquor as raw material |
| CN115246651A (en) * | 2022-08-12 | 2022-10-28 | 广州天赐高新材料股份有限公司 | Method for preparing lithium carbonate by recovering fluorine-containing lithium tailings |
| WO2023071353A1 (en) * | 2021-10-26 | 2023-05-04 | 广东邦普循环科技有限公司 | Method for removing fluorine in positive electrode leachate of lithium batteries |
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| CN110451535A (en) * | 2019-08-15 | 2019-11-15 | 湖南顺华锂业有限公司 | A kind of method of lithium sulfate solution purification and impurity removal |
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| CN112897558A (en) * | 2021-02-23 | 2021-06-04 | 四川思达能环保科技有限公司 | Method for preparing lithium carbonate by taking lithium fluoride mother liquor as raw material |
| WO2023071353A1 (en) * | 2021-10-26 | 2023-05-04 | 广东邦普循环科技有限公司 | Method for removing fluorine in positive electrode leachate of lithium batteries |
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