CN116143149A - Method for preparing industrial grade lithium carbonate by using lithium-containing ore reclaimed material - Google Patents
Method for preparing industrial grade lithium carbonate by using lithium-containing ore reclaimed material Download PDFInfo
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- CN116143149A CN116143149A CN202211704294.7A CN202211704294A CN116143149A CN 116143149 A CN116143149 A CN 116143149A CN 202211704294 A CN202211704294 A CN 202211704294A CN 116143149 A CN116143149 A CN 116143149A
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for preparing industrial grade lithium carbonate by utilizing a lithium-containing ore reclaimed material, which belongs to the technical field of electrolyte preparation of lithium battery electrolyte and comprises the following process steps: A. roasting sulfate; B. adding acid for leaching; C. lime removes magnesium; D. carbonizing and removing impurities; E. precipitating lithium with sodium carbonate. The method for preparing the industrial grade lithium carbonate by using the recovered lithium-containing ore material has the advantages of simple process, high yield, high economic value, little environmental pollution and high production safety.
Description
Technical Field
The invention relates to a method for preparing industrial grade lithium carbonate, in particular to a method for preparing industrial grade lithium carbonate by utilizing a lithium-containing ore reclaimed material.
Background
Lithium belongs to rare elements, and along with the great development of new energy automobiles, the application scale of lithium is also larger and larger, so that lithium resources are smaller and smaller. In particular, the current global lithium minerals occupy less and less lithium total amount, and the development difficulty is greater and greater. Therefore, how to effectively increase lithium in minerals becomes more and more important, wherein many slag materials existing during the exploitation of lithium ores and recovery materials after the extraction of lithium from ores contain a lot of lithium, and in order to utilize the lithium in ore resources to the maximum effect, a method for preparing industrial grade lithium carbonate from the recovery materials of the lithium-containing ores is developed.
Disclosure of Invention
Aiming at increasingly more lithium-containing ore reclaimed materials, the invention provides a method for preparing industrial lithium carbonate by using the lithium-containing ore reclaimed materials, which can rapidly, efficiently and safely extract lithium in the lithium-containing ore reclaimed materials and produce the lithium into the industrial lithium carbonate, thereby solving the problems of shortage of lithium ore resources and insufficient productivity at present.
The invention aims to solve the defects in the prior art, and the invention aims to provide the method for preparing the industrial grade lithium carbonate by utilizing the recovered lithium-containing ore material, which has the advantages of simple process, low production cost of raw materials, high lithium recovery rate, high economic value, little environmental pollution and high production safety.
The method for preparing the industrial grade lithium carbonate by utilizing the lithium-containing ore reclaimed material comprises the following steps:
A. roasting sulfate: crushing and fully grinding a lithium-containing ore reclaimed material, adding a mixture of potassium sulfate and magnesium sulfate, and burning in a muffle furnace at 1000-1100 ℃ for 1-2 hours to obtain a lithium-containing clinker;
B. acid leaching is carried out by adding: adding 98% sulfuric acid and pure water into the lithium-containing clinker obtained in the step A, leaching for 1-2 hours in a water bath at 60-80 ℃ under stirring, filtering to obtain a leaching solution, adding 1-2 times of pure water in mass, stirring for 0.5-1 hour, and filtering to obtain a stirring solution;
C. lime magnesium removal: mixing the leaching solution obtained in the step C with the stirring solution, adding quicklime to adjust the pH of the solution to 10.5-11.5, stirring for 0.5-1 h, and filtering to obtain a lime impurity-removing solution;
D. carbonization impurity removal: introducing CO into the lime impurity removal solution obtained in the step D 2 After adjusting the pH value to 9-10, stirring and reacting for 0.5-1 h to obtain carbonized impurity-removing solution;
E. precipitating lithium by sodium carbonate: concentrating the acidified impurity-removed solution obtained in the step E to a concentration of 20-30 g/L of Li, adding liquid alkali to adjust the pH to 11-12, and adding a sodium carbonate solution (namely a molar ratio Na) with a concentration of 180-230 g/L in terms of 5% of molar excess of Li at a temperature of about 85-95 DEG C 2 CO 3 Li=2.1:1), stirring and reacting for 0.5-1 h, filtering, leaching and drying to obtain the industrial lithium carbonate.
Further, in the step A, the potassium sulfate and the magnesium sulfate are both high-purity (more than 99.9%) anhydrous sulfate.
Further, the adding ratio of the reclaimed materials, the potassium sulfate and the magnesium sulfate in the step A is 3-5:1-2:1-2.
Further, the addition amount of sulfuric acid is 5-10% of the mass of the lithium-containing clinker, and the mass of pure water is 2-3 times of the mass of the lithium-containing clinker.
Further, the quicklime added in the step C is 80% of industrial lime.
Further, the liquid alkali in the step E is water-soluble strong alkali.
Further, the liquid alkali in the step E is sodium hydroxide, and the mass concentration is 32%.
The specific reaction principle is analyzed as follows: roasting at 1000-1100 ℃ by using a muffle furnace to replace Li in the lithium-containing ore reclaimed material by cations in sulfate, adding sulfuric acid to leach out Li which cannot be replaced, leaching with stirring in a water bath at 60-80 ℃ for 1-2 h, dissolving Li into the solution, removing impurities by using cheap quicklime aiming at redundant Mg, removing redundant sulfate in the solution by Ca, and introducing CO 2 Removing excessive Ca, controlling pH to prevent Li from precipitating, and finally utilizing solubility differenceLithium was precipitated using soda ash, the reaction equation is as follows (ore structure is represented by X):
X·Li+K + → X·K+Li + ；
X·Li+Mg 2+ → X·Mg + +Li + ；
Mg 2+ +SO 4 - +CaO+H 2 O=Mg(OH) 2 ↓+CaSO 4 ↓
Ca 2+ +CO 2 +2OH=H 2 O+CaCO 3 ↓
aiming at the problem of insufficient resources of the existing ore, the invention synchronously uses sulfate to replace lithium by high-temperature burning and purifying raw materials, extracts Li by sulfuric acid, and removes Mg and SO by using quicklime 4 2- Reducing the content of impurities by using CO 2 The removal of excess lime opens up a route for extracting lithium from the recovery of lithium-containing ores with more complex components and higher impurity content. The method for preparing the industrial grade lithium carbonate by utilizing the lithium-containing ore reclaimed material has the following advantages compared with the prior art: simple process, low production cost of raw materials, high lithium yield, high economic value, little environmental pollution and high production safety.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying examples in order to facilitate an understanding of the invention, however, the invention may be embodied in many different forms and is not limited to the examples described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The invention provides a method for preparing industrial grade lithium carbonate by using a lithium-containing ore reclaimed material, which comprises the following steps:
A. roasting sulfate: crushing 30-50 g of lithium-containing ore reclaimed materials, fully grinding, adding 10-20 g of potassium sulfate and 10-20 g of magnesium sulfate, and burning in a muffle furnace at 1000-1100 ℃ for 1-2 hours to obtain lithium-containing clinker;
B. acid leaching is carried out by adding: adding 4-8 g of 98% sulfuric acid and 160-240 mL of pure water into the lithium-containing clinker obtained in the step A, leaching for 1-2 hours in a water bath at 60-80 ℃ under stirring, filtering to obtain a leaching solution, adding 80-160 mL of pure water into a filter cake, stirring for 0.5-1 hour, and filtering to obtain a stirring solution;
C. lime magnesium removal: mixing the leaching solution obtained in the step C with the stirring solution, adding quicklime to adjust the pH of the solution to 10.5-11.5, stirring for 0.5-1 h, and filtering to obtain a lime impurity-removing solution;
D. carbonization impurity removal: introducing CO into the lime impurity removal solution obtained in the step D 2 After adjusting the pH value to 9-10, stirring and reacting for 0.5-1 h to obtain carbonized impurity-removing solution;
E. precipitating lithium by sodium carbonate: concentrating the acidified impurity-removed solution obtained in the step E to a concentration of 20-30 g/L of Li, adding liquid alkali to adjust the pH to 11-12, and adding a sodium carbonate solution (namely a molar ratio Na) with a concentration of 180-230 g/L in terms of 5% of molar excess of Li at a temperature of about 85-95 DEG C 2 CO 3 Li=2.1:1), stirring and reacting for 0.5-1 h, filtering, leaching and drying to obtain the industrial lithium carbonate.
Further, in the step A, the potassium sulfate and the magnesium sulfate are both high-purity (more than 99.9%) anhydrous sulfate, and the ratio of the reclaimed materials to the potassium sulfate to the magnesium sulfate is 3-5: 1-2: 1-2, wherein the firing temperature is 1000-1100 ℃ and the firing time is 1-2 hours, so that cations in sulfate can fully replace Li contained in reclaimed materials, and the lithium extraction operation of subsequent procedures is facilitated.
Further, in the step B, the addition amount of sulfuric acid is 5-10% of the mass of the lithium-containing clinker, the mass of pure water is 2-3 times of the mass of the lithium-containing clinker, and a sand core funnel with a diameter of 3-5 um is adopted for filtering, so that the main body of reclaimed materials and other impurities can be removed through filtering.
Further, the quicklime added in the step C is 80% of industrial lime so as to remove superfluous Mg 2+ And SO 4 2- The filtering adopts a sand core funnel with the diameter of 3-5 um,to ensure that the filtration removes the Mg (OH) formed 2 、CaSO 4 And other alkaline insolubles.
Further, the liquid alkali water-soluble strong base in the step E is represented by substances capable of adjusting the pH of the solution to be alkaline without introducing other impurity elements or capable of reacting with sodium carbonate, such as potassium hydroxide and sodium hydroxide. Sodium hydroxide is preferred, with a mass concentration of 32%.
The invention relates to a method for preparing industrial grade lithium carbonate by using a lithium-containing ore reclaimed material, which comprises the first step of sulfate roasting, namely, mixing potassium sulfate and magnesium sulfate with the reclaimed material and then roasting at a high temperature to replace Li in the reclaimed material with K and Mg. And in the second step, acid leaching is carried out, and Li substituted by sulfate is leached under an acidic condition. And thirdly, precipitating lithium by sodium carbonate, adding calcined lime to remove alkaline insoluble substances, adding sodium carbonate under alkaline conditions to obtain lithium carbonate precipitate by utilizing solubility difference, and obtaining the industrial grade lithium carbonate after simple leaching and drying.
The specific reaction principle is analyzed as follows: roasting at 1000-1100 ℃ by using a muffle furnace to replace Li in the lithium-containing ore reclaimed material by positive ions K and Mg in sulfate, leaching for 1-2 hours in a water bath at 60-80 ℃ by stirring, dissolving the replaced Li into a solution, removing impurities by using cheaper quicklime aiming at synchronously leached Mg, and simultaneously removing redundant SO in the solution 4 2- CO is introduced into 2 Excess quicklime is removed, and then sodium carbonate is used to precipitate lithium using the difference in solubility. Compared with the prior art, the method has the advantages that: simple process, low production cost of raw materials, high Li yield, high economic value, little environmental pollution and high production safety.
Example 1
A. Roasting sulfate: crushing and fully grinding 30g of lithium-containing ore reclaimed materials, adding 10g of potassium sulfate and 15g of magnesium sulfate, and burning in a muffle furnace at 1000 ℃ for 1.5h to obtain lithium-containing clinker;
B. acid leaching is carried out by adding: adding 4g of 98% sulfuric acid and 160mL of pure water into the lithium-containing clinker obtained in the step A, stirring and leaching in a water bath at 70 ℃ for 1h, filtering to obtain a leaching solution, adding 80mL of pure water into a filter cake, stirring for 0.5h, and filtering to obtain a stirring and washing solution;
C. lime magnesium removal: mixing the leaching solution obtained in the step C with the stirring solution, adding quicklime to adjust the pH of the solution to 10.5, stirring for 0.5h, and filtering to obtain a lime impurity-removing solution;
D. carbonization impurity removal: introducing CO into the lime impurity removal solution obtained in the step D 2 After regulating the pH value to 9, stirring and reacting for 0.5h to obtain carbonized impurity-removing solution;
E. precipitating lithium by sodium carbonate: concentrating the acidified impurity-removed solution obtained in the step E to a concentration of 20g/L of Li, adding liquid alkali to adjust the pH to 12, adding a sodium carbonate solution with a concentration of 230g/L in terms of molar excess of 5% of Li at 90 ℃ 2 CO 3 Li=2.1:1) is stirred for reaction for 0.5h, then is filtered, and is leached and dried to obtain the technical grade lithium carbonate.
Example 2
A. Roasting sulfate: crushing 50g of recovered lithium-containing ore, fully grinding, adding 15g of potassium sulfate and 20g of magnesium sulfate, and burning in a muffle furnace at 1050 ℃ for 2 hours to obtain lithium-containing clinker;
B. acid leaching is carried out by adding: adding 8g of 98% sulfuric acid and 240mL of pure water into the lithium-containing clinker obtained in the step A, stirring and leaching in a water bath at 80 ℃ for 2 hours, filtering to obtain a leaching solution, adding 160mL of pure water into a filter cake, stirring for 0.75 hour, and filtering to obtain a stirring and washing solution;
C. lime magnesium removal: mixing the leaching solution obtained in the step C with the stirring solution, adding quicklime to adjust the pH value of the solution to 11, stirring for 0.75h, and filtering to obtain a lime impurity-removing solution;
D. carbonization impurity removal: introducing CO into the lime impurity removal solution obtained in the step D 2 After adjusting the pH value to 9.5, stirring and reacting for 1h to obtain carbonized impurity-removing solution;
E. precipitating lithium by sodium carbonate: concentrating the acidified impurity-removed solution obtained in the step E to the concentration of Li of 25g/L, adding liquid alkali to adjust the pH to 11, adding a sodium carbonate solution with the concentration of 210g/L in terms of molar excess of 5% of Li at the temperature of 85 ℃ 2 CO 3 Li=2.1:1) is stirred for reaction for 0.75h, then is filtered, and is leached and dried to obtain the technical grade lithium carbonate.
Example 3
A. Roasting sulfate: crushing 40g of recovered lithium-containing ore, fully grinding, adding 20g of potassium sulfate and 10g of magnesium sulfate, and burning in a muffle furnace at 1100 ℃ for 1h to obtain lithium-containing clinker;
B. acid leaching is carried out by adding: adding 6g of 98% sulfuric acid and 200mL of pure water into the lithium-containing clinker obtained in the step A, leaching for 1.5h in a water bath at 60 ℃ under stirring, filtering to obtain a leaching solution, adding 120mL of pure water into a filter cake, stirring for 1h, and filtering to obtain a stirring solution;
C. lime magnesium removal: mixing the leaching solution obtained in the step C with the stirring solution, adding quicklime to adjust the pH of the solution to 11.5, stirring for 1h, and filtering to obtain a lime impurity-removing solution;
D. carbonization impurity removal: introducing CO into the lime impurity removal solution obtained in the step D 2 After regulating the pH value to 10, stirring and reacting for 0.75h to obtain carbonized impurity-removing solution;
E. precipitating lithium by sodium carbonate: concentrating the acidified impurity-removed solution obtained in the step E to a concentration of Li of 30g/L, adding liquid alkali to adjust the pH to 11.5, adding a 5% molar excess of sodium carbonate solution (namely molar ratio Na) with a concentration of 180g/L at about 95 DEG C 2 CO 3 Li=2.1:1), stirring and reacting for 1h, filtering, leaching and drying to obtain the technical grade lithium carbonate.
The foregoing description of the embodiments of the present invention should not be taken as limiting the scope of the invention, but rather should be construed in view of the following detailed description.
Claims (5)
1. The method for preparing the industrial grade lithium carbonate by using the lithium-containing ore reclaimed materials is characterized by comprising the following steps:
A. roasting sulfate: crushing and fully grinding a lithium-containing ore reclaimed material, adding a mixture of potassium sulfate and magnesium sulfate, and burning in a muffle furnace at 1000-1100 ℃ for 1-2 hours to obtain a lithium-containing clinker;
B. acid leaching is carried out by adding: adding 98% sulfuric acid and pure water into the lithium-containing clinker obtained in the step A, leaching for 1-2 hours in a water bath at 60-80 ℃ under stirring, filtering to obtain a leaching solution, adding 1-2 times of pure water in mass, stirring for 0.5-1 hour, and filtering to obtain a stirring solution;
C. lime magnesium removal: mixing the leaching solution obtained in the step C with the stirring solution, adding quicklime to adjust the pH of the solution to 10.5-11.5, stirring for 0.5-1 h, and filtering to obtain a lime impurity-removing solution;
D. carbonization impurity removal: introducing CO into the lime impurity removal solution obtained in the step D 2 After adjusting the pH value to 9-10, stirring and reacting for 0.5-1 h to obtain carbonized impurity-removing solution;
E. precipitating lithium by sodium carbonate: concentrating the acidified impurity-removed solution obtained in the step E to a concentration of 20-30 g/L of Li, adding liquid alkali to adjust the pH to 11-12, and adding a sodium carbonate solution (namely a molar ratio Na) with a concentration of 180-230 g/L in terms of 5% of molar excess of Li at a temperature of about 85-95 DEG C 2 CO 3 Li=2.1:1), stirring and reacting for 0.5-1 h, filtering, leaching and drying to obtain the industrial lithium carbonate.
2. The method for preparing technical grade lithium carbonate by using recovered lithium-containing ore according to claim 1, wherein: the ratio of the reclaimed materials, the potassium sulfate and the magnesium sulfate added in the step A is 3-5: 1-2: 1-2, wherein the ignition temperature of the muffle furnace is 1000-1100 ℃, and the ignition time is 1-2 hours, so that Li in the lithium-containing ore reclaimed material is fully replaced by K and Mg, and organic impurities are completely removed.
3. The method for preparing technical grade lithium carbonate by using recovered lithium-containing ore according to claim 1, wherein: the adding amount of sulfuric acid in the step B is 5-10% of the mass of the lithium-containing clinker, so that lithium which cannot be replaced by a sulfate method in the reclaimed material is ensured to be discharged in an acidification mode, and the adding amount of pure water is 2-3 times of the mass of the lithium-containing clinker.
4. The method for preparing technical grade lithium carbonate by using recovered lithium-containing ore according to claim 1, wherein: and C, adjusting the pH value of the solution at the end point to be 10.5-11.5, ensuring that Mg in the solution can be completely removed, and simultaneously removing redundant sulfate radical by adopting quicklime.
5. Root of Chinese characterThe method for preparing technical grade lithium carbonate by using recovered lithium-containing ore as claimed in claim 1, wherein: the molar ratio of sodium carbonate to lithium added in the step E is Na 2 CO 3 Li=2.1:1, ensuring that Li precipitates as completely as possible.
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Citations (6)
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| FR766161A (en) * | 1932-12-29 | 1934-06-22 | Hans Heinrich Huette G M B H | Process for collecting lithium contained in lithiniferous minerals |
| CN101609888A (en) * | 2009-07-10 | 2009-12-23 | 江西赣锋锂业股份有限公司 | A kind of method of utilizing lithium chloride solution to prepare battery-level lithium carbonate |
| CN109455744A (en) * | 2018-12-28 | 2019-03-12 | 江西赣锋锂业股份有限公司 | The method for preparing industrial level lithium carbonate using spodumene calcium and magnesium slag recycling lithium |
| RU2749598C1 (en) * | 2020-11-30 | 2021-06-15 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method for processing mica concentrate |
| CN114368764A (en) * | 2022-02-18 | 2022-04-19 | 华东理工大学 | Method for directly preparing lithium sulfate from hard rock type lithium ore |
| CN114507779A (en) * | 2022-02-18 | 2022-05-17 | 华东理工大学 | Method for producing lithium sulfate solution by spodumene sulfate roasting method |
-
2022
- 2022-12-29 CN CN202211704294.7A patent/CN116143149A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR766161A (en) * | 1932-12-29 | 1934-06-22 | Hans Heinrich Huette G M B H | Process for collecting lithium contained in lithiniferous minerals |
| CN101609888A (en) * | 2009-07-10 | 2009-12-23 | 江西赣锋锂业股份有限公司 | A kind of method of utilizing lithium chloride solution to prepare battery-level lithium carbonate |
| CN109455744A (en) * | 2018-12-28 | 2019-03-12 | 江西赣锋锂业股份有限公司 | The method for preparing industrial level lithium carbonate using spodumene calcium and magnesium slag recycling lithium |
| RU2749598C1 (en) * | 2020-11-30 | 2021-06-15 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Method for processing mica concentrate |
| CN114368764A (en) * | 2022-02-18 | 2022-04-19 | 华东理工大学 | Method for directly preparing lithium sulfate from hard rock type lithium ore |
| CN114507779A (en) * | 2022-02-18 | 2022-05-17 | 华东理工大学 | Method for producing lithium sulfate solution by spodumene sulfate roasting method |
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