CN107902678A - A kind of sulfuric acid baking processing lepidolite ore is except the method for aluminium production lithium carbonate - Google Patents
A kind of sulfuric acid baking processing lepidolite ore is except the method for aluminium production lithium carbonate Download PDFInfo
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- CN107902678A CN107902678A CN201711118948.7A CN201711118948A CN107902678A CN 107902678 A CN107902678 A CN 107902678A CN 201711118948 A CN201711118948 A CN 201711118948A CN 107902678 A CN107902678 A CN 107902678A
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- Prior art keywords
- lithium
- sulfuric acid
- solution
- reaction
- carbonate
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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
Abstract
The invention discloses a kind of sulfuric acid baking processing lepidolite ore except the method for aluminium production lithium carbonate, by the way that sulfuric acid extracting sulfuric acid lithium solution will be used after lepidolite concentrate and water for ball milling, with the aluminium ion removed completely with 8 oxyquinolines after sodium hydroxide adjusting lithium sulfate solution in lithium sulfate solution, then lithium sulfate solution is adjusted to neutral with sulfuric acid so as to separate out 8 oxyquinolines, lithium carbonate is made finally by sodium carbonate liquor and lithium sulfate reaction, the battery-level lithium carbonate of production will be free from aluminium；And the whole technique of the present invention is simple and convenient to operate, is swift in response, production efficiency is high, and reaction process does not have side reaction and do not produce poisonous and harmful substance, environmental-friendly.
Description
Technical field
Advanced green battery material manufacture work that the present invention relates to new energy -- new and effective energy conversion and storing technology --
The field such as skill and production technology, particularly a kind of sulfuric acid baking processing lepidolite ore is except the method for aluminium production lithium carbonate.
Background technology
With the fast development of low-carbon economy and green novel energy source industry, in particular with great-capacity power battery technology
Break through and promote and apply, novel lithium battery power vehicle industry emerges rapidly, greatly develops lithium electricity industry as the generally common of people
Know, the tradition that the demand for promoting lithium is walked out to " industrial monosodium glutamate " is limited to, and welcomes the new era of " energy metal ".Lithium carbonate is a kind of
Important industrial chemicals, with the appearance of national new energy development plan, lithium electricity new energy becomes state key and supports development
One of energy industry；And the important foundation raw material that lithium carbonate develops as lithium electricity new energy, its demand are increasing, price
It is higher and higher.
It is an important chemical method for lepidolite extraction lithium, the primary raw material for carrying lithium at present is salt lake bittern and consolidates
Body lithium minerals, the rich reserves of Chinese lepidolite and spodumene.The method that lithium is carried from lithium minerals mainly has sulfate process, chlorination
Thing method, limestone-based process, sulfuric acid process and gas-solid reaction method, these methods are all that lithium minerals is carried out high-temperature calcination, then with not
The same method processing calcining further extracting sulfuric acid lithium solution of slag, obtains lithium sulfate solution, then reacts to obtain electricity with sodium carbonate
Pond level lithium carbonate and sinker mother liquor, but its complex procedures, reaction condition is cumbersome, and production efficiency is low, and needs corresponding
Corollary equipment, production cost is high, and the purity of obtained battery-level lithium carbonate is low, and can influence containing aluminium ion cell performance
Can, it is unsuitable for generating on a large scale.
The content of the invention
The invention aims to solve the deficiency of prior art problem, there is provided a kind of sulfuric acid baking processing lepidolite ore removes
The method that aluminium produces lithium carbonate.
To reach above-mentioned purpose, the present invention is implemented according to following technical scheme：
A kind of sulfuric acid baking processing lepidolite ore comprises the following steps except the method for aluminium production lithium carbonate：
Step 1: lepidolite concentrate and water are carried out ball milling, then sulfuric acid is generated for the sulfuric acid reaction of 30-70% with concentration
The thick solution of lithium, filtration washing remove slag to obtain lithium sulfate solution A；
Step 2: adding excessive sodium hydrate powder into lithium sulfate solution A, after stirring 20-30 minutes, it is centrifuged
Obtain lithium solution B；Sodium hydroxide mainly removes most Ca in lithium sulfate solution A2+、Fe3+、Mg2+、Al3+、Ca2+Etc. miscellaneous
Matter ion, and the pH of lithium solution B is adjusted in alkalescence；
Step 3: adding excessive 8-hydroxyquinoline into lithium solution B, after stirring 20-30 minutes, it is centrifuged obtaining lithium
Solution C；8-hydroxyquinoline is dissolved in after the lithium solution B in alkalescence occurs complex reaction production precipitation 8- hydroxyls with aluminium ion therein
Quinoline aluminum, aluminum ions lithium solution C is removed after filtering completely to obtain the final product；
Step 4: 8- hydroxyl of the sulphur acid for adjusting pH that addition concentration is 30-70% into lithium solution C to neutrality, so excess
Base quinoline is centrifuged obtaining lithium solution D due to that can separate out 8-hydroxyquinoline particle insoluble in neutral solution；
Step 5: adding the sodium carbonate liquor identical with sulfuric acid lithium concentration while stirring into lithium solution D, feed time is
30-180min, charge temperature are 50-100 DEG C, and feed liquid is obtained after reaction；
Step 6: by the feed liquid separation of solid and liquid in step 5, solid is washed, is dry, up to battery-level lithium carbonate.
Further, the reaction time in the step 1：When 1-20 is small, reaction pressure：0.1-1MP.
Preferably, step 6 is to add water in the precipitation obtained after feed liquid is separated, is stirred by solid-to-liquid ratio 1: 3-4 and is washed till few two
It is secondary, stir after washing 10-20 minutes and centrifuge every time, battery-level lithium carbonate is obtained after dry.
Compared with prior art, the present invention will be after lepidolite concentrate and water for ball milling by that will use sulfuric acid extracting sulfuric acid lithium solution,
With the aluminium ion removed completely with 8-hydroxyquinoline after sodium hydroxide adjusting lithium sulfate solution in lithium sulfate solution, sulfuric acid is then used
Lithium sulfate solution is adjusted to neutral so as to separate out 8-hydroxyquinoline, carbonic acid is made finally by sodium carbonate liquor and lithium sulfate reaction
Lithium, the battery-level lithium carbonate of production will be free from aluminium；And the whole technique of the present invention is simple and convenient to operate, is swift in response, and produces
Efficient, reaction process does not have side reaction and does not produce poisonous and harmful substance, environmental-friendly.
Embodiment
With reference to specific embodiment, the invention will be further described, in the illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
Step 1: lepidolite concentrate and water are carried out ball milling, then lithium sulfate is generated for 70% sulfuric acid reaction with concentration
Thick solution, reaction time：1 it is small when, reaction pressure：0.1MP, filtration washing remove slag to obtain lithium sulfate solution A；
Step 2: adding excessive sodium hydrate powder into lithium sulfate solution A, stirring after twenty minutes, is centrifuged
To lithium solution B；
Step 3: add excessive 8-hydroxyquinoline into lithium solution B, stirring after twenty minutes, is centrifuged obtaining lithium molten
Liquid C；
Step 4: add sulphur acid for adjusting pH that concentration is 70% into lithium solution C to neutrality, it is centrifuged obtaining lithium molten
Liquid D；
Step 5: adding the sodium carbonate liquor identical with sulfuric acid lithium concentration while stirring into lithium solution D, feed time is
30min, charge temperature are 50 DEG C, and feed liquid is obtained after reaction；
Step 6: by the feed liquid separation of solid and liquid in step 5, water is added in the precipitation obtained after feed liquid is separated, by solid-to-liquid ratio
Stir wash at least twice at 1: 3, stirs to wash every time and centrifuges after ten minutes, and battery-level lithium carbonate is obtained after dry.
Embodiment 2
Step 1: lepidolite concentrate and water are carried out ball milling, then lithium sulfate is generated for 70% sulfuric acid reaction with concentration
Thick solution, when the reaction time 20 is small, reaction pressure：1MP, filtration washing remove slag to obtain lithium sulfate solution A；
Step 2: adding excessive sodium hydrate powder into lithium sulfate solution A, after stirring 30 minutes, it is centrifuged
To lithium solution B；
Step 3: add excessive 8-hydroxyquinoline into lithium solution B, after stirring 30 minutes, it is centrifuged obtaining lithium molten
Liquid C；
Step 4: add sulphur acid for adjusting pH that concentration is 70% into lithium solution C to neutrality, it is centrifuged obtaining lithium molten
Liquid D；
Step 5: adding the sodium carbonate liquor identical with sulfuric acid lithium concentration while stirring into lithium solution D, feed time is
180min, charge temperature are 100 DEG C, and feed liquid is obtained after reaction；
Step 6: by the feed liquid separation of solid and liquid in step 5, water is added in the precipitation obtained after feed liquid is separated, by solid-to-liquid ratio
Stir wash at least twice at 1: 4, stirs to wash every time and centrifuges after twenty minutes, and battery-level lithium carbonate is obtained after dry.
Embodiment 3
Step 1: lepidolite concentrate and water are carried out ball milling, then lithium sulfate is generated for 60% sulfuric acid reaction with concentration
Thick solution, reaction time：12 it is small when, reaction pressure：0.6MP, filtration washing remove slag to obtain lithium sulfate solution A；
Step 2: adding excessive sodium hydrate powder into lithium sulfate solution A, after stirring 25 minutes, it is centrifuged
To lithium solution B；
Step 3: add excessive 8-hydroxyquinoline into lithium solution B, after stirring 25 minutes, it is centrifuged obtaining lithium molten
Liquid C；
Step 4: add sulphur acid for adjusting pH that concentration is 60% into lithium solution C to neutrality, it is centrifuged obtaining lithium molten
Liquid D；
Step 5: adding the sodium carbonate liquor identical with sulfuric acid lithium concentration while stirring into lithium solution D, feed time is
100min, charge temperature are 70 DEG C, and feed liquid is obtained after reaction；
Step 6: by the feed liquid separation of solid and liquid in step 5, water is added in the precipitation obtained after feed liquid is separated, by solid-to-liquid ratio
Stir wash at least twice at 1: 3.5, stirs after washing 15 minutes and centrifuges every time, and battery-level lithium carbonate is obtained after dry.
Technical scheme is not limited to the limitation of above-mentioned specific embodiment, and every technique according to the invention scheme is done
The technology deformation gone out, each falls within protection scope of the present invention.
Claims (3)
1. a kind of sulfuric acid baking processing lepidolite ore is except the method for aluminium production lithium carbonate, it is characterised in that comprises the following steps：
Step 1: lepidolite concentrate and water are carried out ball milling, it is thick then to generate lithium sulfate with concentration for the sulfuric acid reaction of 30-70%
Solution, filtration washing remove slag to obtain lithium sulfate solution A；
Step 2: adding excessive sodium hydrate powder into lithium sulfate solution A, after stirring 20-30 minutes, it is centrifuged obtaining
Lithium solution B；
Step 3: adding excessive 8-hydroxyquinoline into lithium solution B, after stirring 20-30 minutes, it is centrifuged obtaining lithium solution
C；
Step 4: add sulphur acid for adjusting pH that concentration is 30-70% into lithium solution C to neutrality, it is centrifuged obtaining lithium molten
Liquid D；
Step 5: add the sodium carbonate liquor identical with sulfuric acid lithium concentration, feed time 30- while stirring into lithium solution D
180min, charge temperature are 50-100 DEG C, and feed liquid is obtained after reaction；
Step 6: by the feed liquid separation of solid and liquid in step 5, solid is washed, is dry, up to battery-level lithium carbonate.
2. sulfuric acid baking processing lepidolite ore according to claim 1 is except the method for aluminium production lithium carbonate, it is characterised in that：
Reaction time in the step 1：When 1-20 is small, reaction pressure：0.1-1MP.
3. sulfuric acid baking processing lepidolite ore according to claim 1 is except the method for aluminium production lithium carbonate, it is characterised in that：
Step 6 is in the precipitation obtained after feed liquid is separated plus water, stirs and is washed at least twice by solid-to-liquid ratio 1: 3-4, stirs wash 10-20 every time
Centrifuged after minute, battery-level lithium carbonate is obtained after dry.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711118948.7A CN107902678A (en) | 2017-11-14 | 2017-11-14 | A kind of sulfuric acid baking processing lepidolite ore is except the method for aluminium production lithium carbonate |
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| CN201711118948.7A CN107902678A (en) | 2017-11-14 | 2017-11-14 | A kind of sulfuric acid baking processing lepidolite ore is except the method for aluminium production lithium carbonate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930000A (en) * | 2019-04-26 | 2019-06-25 | 核工业北京化工冶金研究院 | A kind of method of lepidolite purification of leaching liquor removal of impurities |
| RU2749598C1 (en) * | 2020-11-30 | 2021-06-15 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method for processing mica concentrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186968A (en) * | 2006-11-24 | 2008-05-28 | 江西赣锋锂业有限公司 | Method for producing refined lithium sulfate solution used in lepidolite lithium-extracting technique by sulfuric acid process |
| CN102649996A (en) * | 2012-05-24 | 2012-08-29 | 张韵 | Circular acid leaching extraction process for lepidolite |
| CN103708508A (en) * | 2014-01-17 | 2014-04-09 | 长沙有色冶金设计研究院有限公司 | Method for producing cell-grade lithium carbonate from lithium concentrate |
-
2017
- 2017-11-14 CN CN201711118948.7A patent/CN107902678A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186968A (en) * | 2006-11-24 | 2008-05-28 | 江西赣锋锂业有限公司 | Method for producing refined lithium sulfate solution used in lepidolite lithium-extracting technique by sulfuric acid process |
| CN102649996A (en) * | 2012-05-24 | 2012-08-29 | 张韵 | Circular acid leaching extraction process for lepidolite |
| CN103708508A (en) * | 2014-01-17 | 2014-04-09 | 长沙有色冶金设计研究院有限公司 | Method for producing cell-grade lithium carbonate from lithium concentrate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930000A (en) * | 2019-04-26 | 2019-06-25 | 核工业北京化工冶金研究院 | A kind of method of lepidolite purification of leaching liquor removal of impurities |
| CN109930000B (en) * | 2019-04-26 | 2021-01-05 | 核工业北京化工冶金研究院 | Method for purifying lepidolite leaching solution |
| RU2749598C1 (en) * | 2020-11-30 | 2021-06-15 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method for processing mica concentrate |
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Application publication date: 20180413 |