CN108383140A - A kind of clearer production technology and method of lithium sulfate - Google Patents
A kind of clearer production technology and method of lithium sulfate Download PDFInfo
- Publication number
- CN108383140A CN108383140A CN201810437673.1A CN201810437673A CN108383140A CN 108383140 A CN108383140 A CN 108383140A CN 201810437673 A CN201810437673 A CN 201810437673A CN 108383140 A CN108383140 A CN 108383140A
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- China
- Prior art keywords
- lithium
- roasting
- production
- lithium sulfate
- immersion
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Classifications
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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
- C01D15/06—Sulfates; Sulfites
-
- 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 clearer production technology and its production method of lithium sulfate, including process and roasting additive.Wherein, production technology includes the heavy miscellaneous crystallizing and drying of screening batch mixing granulating roasting immersion, and roasting additive is by Na2SO4、K2SO4、CaCO3It is constituted with components such as CaO.The present invention can not only improve the roasting conversion rate and leaching rate of lithium, but also few without dopant species in acid, leachate and impurity content, and follow-up removal of impurities process is simple, acid and alkali consumption is small.Simple production process, lithium recovery rate height, the energy and Matter Transfer of the present invention use, and are a kind of clearer production technologies and method of suitable large-scale production.
Description
Technical field
The present invention relates to a kind of clearer production technology of lithium sulfate and its production methods.
Background technology
Currently, the raw material of extraction lithium is mainly brine containing lithium and lithium ore.Lithium is carried using brine, is limited by technical reason,
So that the extraction of magnesium, boron is difficult, production procedure is complicated, and the product purity after extraction is not high, therefore, current country's LITHIUM BATTERY carbon
The production of sour lithium relies primarily on lithium ore and carries lithium.However, to produce the sulphur that battery-level lithium carbonate has to obtain high-purity in advance
Sour lithium.Lithium ore carries lithium raw material and relies on import, price height, and in order to obtain higher recovery rate, preamble is largely strong with concentrated sulfuric acid etc.
Acid leaching is improving lithium leaching rate while the also impurity such as a large amount of potassium of leaching rate, sodium, aluminium, boron, iron, magnesium, calcium, follow-up and a large amount of use
Alkali cleans, and not only requires height to the corrosion resistance of equipment, but also process route is elongated, the energy and soda acid largely waste, and are produced into
Originally it remains high.
Invention content
The problems such as proposing long lithium process route, soda acid waste for ore, is produced the present invention provides a kind of using lithium ore
The clearer production technology and its production method of lithium sulfate, realize water circulation use, zero-emission, and potassium sulfate, sulfuric acid is precipitated in crystallization
Sodium is supplemented as additive and is used, and solves the problems, such as environmental protection and waste in production process, with good economic efficiency.
The present invention provides a kind of clearer production technology and its production method producing lithium sulfate using lithium ore, the skills
Art and method include the following steps：
Screening：Lithium ore is sieved with 80~100 mesh iron sieve, bulky grain is crushed and reaches requirement；
Batch mixing：By lithium ore, roasting additive according to mass ratio 1:(0.2~0.6) it is uniformly mixed；
It is granulated：Above-mentioned batch mixing water or recirculated water are granulated balling-up；
Roasting：Above-mentioned pellet is roasted, 850~1200 DEG C of calcination temperature, 10~120min of time；
It impregnates：Above-mentioned baked pellet is impregnated, soaking solution can be the water being newly added, and can also be production
Recirculated water in the process.Immersion total time is 0.2~16h.
It is heavy miscellaneous：Suitable sodium hydroxide is added, so that aluminium, boron, iron, magnesium, calcium etc. is reacted and generates precipitation, pass through solid-liquid point
From removing.
Crystallization：By it is heavy it is miscellaneous after solution separation, using cryogenic freezing and be concentrated by evaporation the method for crystallising being combined and make sulfuric acid
Sodium, potassium sulfate crystallize at different temperatures, then detach and obtain lithium sulfate clear liquid；
It is dry：Lithium sulfate clear liquid is dried, is crushed, lithium sulfate product is obtained.
Preferably, the roasting additive constituent mass ratio is Na2SO4、K2SO4、CaCO3And CaO, each component mass ratio
For：1：(0.3~0.6)：(0~0.5)：(0~0.3) is 0 when both rear different.
Preferably, described to be not more than 15mm at bulb diameter.
Preferably, the temperature of the roasting is 900~1100 DEG C, and roasting time is 20~60min.
Preferably, the immersion total time is 0.5~4h.
Preferably, the immersion can once impregnate, and can also repeatedly impregnate.
Preferably, the roasting additive component can be technical grade product, can also be the mixture containing corresponding ingredient
Or unclassified stores.
Preferably, the lithium ore can be spodumene, lepidolite, and can also be that petalite etc. is other contains lithium ore.
The present invention provides a kind of clearer production technology of lithium sulfate and production methods, in entire production process, roasting
The flue gas heat that process excludes can be used for impregnating, crystallize and the evaporation condensed water of drying process, crystallization and drying process can be used for
Be granulated and impregnate process, the potassium sulfate sodium sulphate of Crystallization Procedure can be supplemented into roasting additive, realize the energy and material
It recycles, is typical clearer production technology.The present invention can not only improve the roasting conversion rate and leaching rate of lithium, but also not
Greatly reduced with dopant species and impurity content in acid, leachate, follow-up removal of impurities process is simple, acid and alkali consumption is small.In conclusion
Simple production process of the present invention, soda acid dosage are small, lithium synthesis recovery rate is high, are suitble to large-scale industrial production.
Description of the drawings
Fig. 1 show a kind of clearer production technology of lithium sulfate provided by the invention and its technological process of production method
Figure.
Specific implementation mode
Present invention process process is simple, soda acid dosage is small, material and heat recovery, realizes industrial wastewater cycle profit
With, zero-emission, potassium sulfate is precipitated in crystallization, sodium sulphate is supplemented as additive and used, and is typical practical clearer production technology.Under
Face is illustrated with specific example：
1. screening：Lepidolite ore is sieved with 100 mesh iron sieve, if any bulky grain, is then crushed bulky grain
After be sieved, obtain satisfactory lepidolite miberal powder.
2. batch mixing：By after sieving lepidolite, roasting additive is according to mass ratio 1:0.5 is mixed, and is stirred evenly.
3. being granulated：Batch mixing is stirred with suitable quantity of water, is granulated with comminutor, at bulb diameter 10mm.
4. roasting：Pellet is put into calcining kiln to roast, calcination temperature is 920 DEG C, roasting time 20min.
5. impregnating：It after roasting pellet kiln discharge cooling, is impregnated with 60 DEG C of water, point 2 immersions, each 40min, and
Timing agitation makes it impregnate abundant.
6. heavy miscellaneous：Solution after immersion is detached, Mg in solution is measured2+、Fe2+、Al3+Content, be added it is suitable
NaOH obtains sediment, and centrifuges away and precipitate.
7. crystallization：Solution is first cooled to -10 DEG C, aqueous sulfuric acid sodium and potassium sulfate crystallization is precipitated, be heated to 36 DEG C by
Sodium sulphate is precipitated in step, and sodium sulphate and potassium sulfate salt-mixture can be precipitated by continuing to be concentrated by evaporation, and cooling down to room temperature obtains potassium sulfate
Crystallization.Crystallization is detached respectively from solution in different phase, just obtains lithium sulfate clear liquid；
8. drying：Lithium sulfate clear liquid is dried, is crushed, lithium sulfate product is obtained.
The above is the specific implementation mode of the present invention, it is noted that for those skilled in the art
For, without departing from the principle of the present invention, several improve and perfects can also be made, these improve and perfects are also considered as
Protection scope of the present invention.
Claims (9)
1. the clearer production technology and its production method of a kind of lithium sulfate, it is characterised in that：Described method includes following steps：
Screening：Lithium ore is sieved with 80~100 mesh iron sieve, bulky grain crushing reaches requirement；
Batch mixing：By lithium ore, roasting additive according to mass ratio 1:(0.2~0.6) it is uniformly mixed；
It is granulated：Above-mentioned batch mixing water or recirculated water are granulated balling-up；
Roasting：Above-mentioned granulation pellet is roasted；
It impregnates：Above-mentioned baked pellet is impregnated；
It is heavy miscellaneous：Appropriate sodium hydroxide is added, removes aluminium, iron, magnesium, calcium plasma in solution；
Crystallization：Using cryogenic freezing and the potassium being concentrated by evaporation in the method removing solution being combined, sodium plasma, lithium sulfate is obtained
Clear liquid；
It is dry：Lithium sulfate clear liquid is dried, is crushed, lithium sulfate product is obtained.
2. the method as described in right 1, it is characterised in that：The roasting additive group is divided into Na2SO4、K2SO4、CaCO3And CaO,
Each component mass ratio is：1：(0.3~0.6)：(0~0.5)：(0~0.3) is 0 when both rear different.
3. the method as described in claim 1, it is characterised in that：It is granulated into bulb diameter after the batch mixing and is not more than 20mm.
4. the method as described in claim 1, it is characterised in that：The temperature of the roasting is 850~1200 DEG C, the time 10~
120min；
5. the method as described in claim 1, it is characterised in that：The solution for roasting pellet immersion can be newly added
Clear water, can also be the recirculated water in production process.
6. the method as described in claim 1, it is characterised in that：The immersion total time is 0.2~16h.
7. the method as described in claim 1, it is characterised in that：The immersion can once impregnate, and can also impregnate several times.
8. the method as described in claim 1, it is characterised in that：The lithium ore can be spodumene, lepidolite, can also be lithium
Feldspar contains lithium ore including but not limited to above-mentioned.
9. roasting additive as claimed in claim 2, it is characterised in that：The roasting additive component can be technical grade production
Product can also be mixture or unclassified stores containing corresponding ingredient.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810437673.1A CN108383140A (en) | 2018-05-09 | 2018-05-09 | A kind of clearer production technology and method of lithium sulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810437673.1A CN108383140A (en) | 2018-05-09 | 2018-05-09 | A kind of clearer production technology and method of lithium sulfate |
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| Publication Number | Publication Date |
|---|---|
| CN108383140A true CN108383140A (en) | 2018-08-10 |
Family
ID=63071484
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810437673.1A Withdrawn CN108383140A (en) | 2018-05-09 | 2018-05-09 | A kind of clearer production technology and method of lithium sulfate |
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| CN (1) | CN108383140A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673377A (en) * | 2017-11-23 | 2018-02-09 | 大余县旭日矿业科技有限公司 | A kind of clean method for producing of battery-level lithium carbonate |
| CN109929993A (en) * | 2019-04-26 | 2019-06-25 | 核工业北京化工冶金研究院 | A kind of pretreatment of lepidolite ore and leaching method |
| CN109943713A (en) * | 2019-04-26 | 2019-06-28 | 核工业北京化工冶金研究院 | A kind of leaching method of lepidolite ore |
| CN110395751A (en) * | 2019-04-15 | 2019-11-01 | 江西南氏锂电新材料有限公司 | A method of lithium sulfate is extracted from lepidolite |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502440A (en) * | 2015-12-04 | 2016-04-20 | 中国科学院青海盐湖研究所 | Method for purifying lithium sulfate crude ore |
| CN106587116A (en) * | 2016-12-05 | 2017-04-26 | 天津二八科技股份有限公司 | Method for extracting lithium carbonate and aluminum hydroxide through lepidolite and fly ash |
-
2018
- 2018-05-09 CN CN201810437673.1A patent/CN108383140A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502440A (en) * | 2015-12-04 | 2016-04-20 | 中国科学院青海盐湖研究所 | Method for purifying lithium sulfate crude ore |
| CN106587116A (en) * | 2016-12-05 | 2017-04-26 | 天津二八科技股份有限公司 | Method for extracting lithium carbonate and aluminum hydroxide through lepidolite and fly ash |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673377A (en) * | 2017-11-23 | 2018-02-09 | 大余县旭日矿业科技有限公司 | A kind of clean method for producing of battery-level lithium carbonate |
| CN110395751A (en) * | 2019-04-15 | 2019-11-01 | 江西南氏锂电新材料有限公司 | A method of lithium sulfate is extracted from lepidolite |
| CN109929993A (en) * | 2019-04-26 | 2019-06-25 | 核工业北京化工冶金研究院 | A kind of pretreatment of lepidolite ore and leaching method |
| CN109943713A (en) * | 2019-04-26 | 2019-06-28 | 核工业北京化工冶金研究院 | A kind of leaching method of lepidolite ore |
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Application publication date: 20180810 |
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