CN113998715A - Method for extracting lithium from high-calcium lithium-containing raw material - Google Patents
Method for extracting lithium from high-calcium lithium-containing raw material Download PDFInfo
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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
- C01D15/04—Halides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
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Abstract
A method for extracting lithium from a high-calcium lithium-containing raw material comprises the following steps: (1) calcium deposition: adding a calcium-containing lithium-containing raw material into a reaction container, adding a calcium precipitator, stirring to generate calcium sulfate crystals, and performing solid-liquid separation to obtain a decalcified lithium-containing mother solution; (2) and (4) nanofiltration: nano-filtering the decalcified lithium-containing mother liquor obtained in the step (1) by a nano-filtering system to further decalcify and remove other ions with valence more than or equal to 2 to obtain lithium-containing filtrate; (3) and (3) evaporation and concentration: and (3) evaporating and concentrating the lithium-containing filtrate obtained in the step (2) to obtain a lithium-rich concentrated solution. The method has the advantages of simple and convenient operation steps, mild working conditions, low energy consumption, safe operation and little environmental pollution; all the operation processes are carried out according to the conditions of safety, energy conservation and environmental protection. It is suitable for extracting lithium from various lithium-containing materials containing calcium, and is especially suitable for extracting lithium from high-calcium lithium-containing materials.
Description
Technical Field
The invention relates to a method for extracting lithium from a lithium-containing raw material, in particular to a method for extracting lithium salt from a high-calcium lithium-containing raw material.
Background art:
lithium is an important strategic resource and one of the indispensable important raw materials of modern high-tech products.
Lithium chloride is one of the lithium compounds and can be used to make dry cells and lithium metal. The industrial production is mainly extracted from lepidolite, spodumene and brine after extracting sodium chloride and potassium chloride. If the content of calcium in the lithium raw material is high, the quality of a product obtained by lithium precipitation is affected, so that the calcium needs to be removed before a lithium-rich solution is obtained.
CN 109735709a discloses a method for recovering lithium from calcium and magnesium removing slag and preparing a ternary precursor material in 2019, 5, month and 10, which comprises the following steps: (1) converting magnesium salt, namely preparing the calcium-magnesium-removed slag and a magnesium salt solution with the magnesium ion concentration of 30-100g/L into slurry, adding inorganic acid, adjusting the pH of the system to 1.0-5.0, heating and stirring for 1-5h, and filtering to obtain a conversion liquid and calcium magnesium fluoride slag; (2) precipitating cobalt, nickel and manganese, adding a precipitator into the transformation liquid, and controlling the system temperature to be 25-100 ℃ to obtain nickel, cobalt and manganese slag and crude lithium liquid; (3) acid leaching the nickel-cobalt-manganese slag, mixing the nickel-cobalt-manganese slag with tap water to obtain slurry, adding inorganic acid into the slurry, adjusting the pH to 0-5, and stirring for 0.5-1h to obtain acid leaching solution and acid leaching slag; (4) removing calcium and magnesium: adding soluble fluoride salt into the pickle liquor, controlling the system temperature at 50-100 ℃, stirring for 0.5-2h, and filtering to obtain calcium-magnesium-removed liquor and calcium-magnesium-removed slag; (5) and (3) extraction: extracting metal cobalt, nickel and manganese in the calcium-magnesium-removed solution by using an organic extractant, and performing back extraction to obtain a back extraction solution containing cobalt, nickel and manganese; (6) synthesizing a precursor: adding soluble cobalt nickel manganese salt into the stripping solution, adding sodium hydroxide and ammonia water, controlling the pH of the system to 9-12, keeping the reaction temperature at 60-70 ℃, and stirring for 1-5 hours to obtain spherical nickel cobalt manganese hydroxide; (7) drying: drying the spherical nickel, cobalt and manganese hydroxide at the high temperature of 100-500 ℃ for 2-5h to obtain the ternary precursor material. The method has complex operation steps; the heating needs to be carried out for many times, and the energy consumption is high; the acid and the alkali are used for many times, so that the environment is polluted; the method of adding soluble fluoride salt into the pickle liquor, controlling the temperature of the system to be 50-100 ℃, stirring for 0.5-2h, and filtering the calcium-magnesium-removed slag to remove calcium is adopted, so that the energy consumption is high, the operation is very troublesome, and the generated calcium-magnesium slag is difficult to treat; the production cost is high.
CN 112593094A discloses a method for extracting lithium from salt lake brine in 2021, 4.2.4.A method for extracting lithium hydroxide from carbonate type salt lake brine is disclosed, the invention utilizes a coupling membrane method of an adsorption method to prepare lithium hydroxide from carbonate type salt lake brine, and the method is only suitable for extracting lithium from salt lake brine with low calcium content because the raw material salt lake brine used in the method contains carbonate and has low calcium content.
CN 112624155a at 2021, 4/9 discloses a method for preparing battery-grade anhydrous lithium chloride by purifying old halogen, which comprises the following steps: a, heating the brine to 40-60 ℃, keeping the temperature constant, adding active carbon, stirring for 30-60 minutes, filtering, and removing organic matters, suspended matters, solid silt and the like in the brine; b, heating the solution obtained in the step A to 90-110 ℃, adding 30-35% of liquid alkali, adjusting the pH value to 6-9, separating magnesium slag, adding 30-35% of liquid alkali again into clear liquid, adjusting the pH value to 12-14, reacting for 20 minutes, and separating calcium magnesium slag again; c, exchanging and adsorbing boron ions in the solution obtained in the step B to reduce the concentration of the boron ions to below 10 ppm; d, introducing carbon dioxide into the solution obtained in the step C to remove calcium, and separating calcium slag when the pH value of the solution is 6-7; e, preparing 20% of soda ash solution by using steam condensate water, adding 30-35% of liquid caustic soda to adjust the PH value to 12-14, adding EDTA (ethylene diamine tetraacetic acid) to complex divalent metal ions, adding the soda ash solution, heating to 90-100 ℃, slowly adding the old brine purification solution obtained in the step D, and keeping the temperature for 0.5-2 hours; f, separating the solid obtained in the step E by a horizontal scraper centrifuge, and washing for 2-3 times on line by using steam condensed water; g, adding deionized water or purified water and EDTA into the solid obtained in the step F, introducing carbon dioxide for carbonization, maintaining the pressure for 30 minutes, and separating insoluble substances from the carbonized clear liquid through a filter press; h, heating the clear liquid obtained in the step G to 90-110 ℃, pyrolyzing for 30 minutes at constant temperature, separating the solid by a centrifugal machine, and washing for 2-3 times by using steam condensate; i, adding hydrochloric acid into the solid obtained in the step H for acidification and transformation, keeping the pH value constant for 2-3 for at least 20 minutes, and then adjusting the pH value to 7-9 by using lithium hydroxide solid; j, evaporating, concentrating and crystallizing the pure lithium chloride solution obtained in the step I to obtain a solid, keeping the solid content in an evaporator to be 5-30%, separating the lithium chloride solid from the slurry by using a centrifugal machine, and recycling according to the impurity content in the mother solution; and K, continuously drying and dehydrating the lithium chloride wet material obtained in the step J at the temperature of 150-180 ℃. The method has complex operation steps; the heating needs to be carried out for many times, and the energy consumption is high; liquid caustic soda, soda ash and hydrochloric acid are required to be used for many times, and the environment is also polluted; carbon dioxide is also needed to be respectively introduced for calcium removal and carbonization, so that the operation has safety risk; the production cost is high.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide a method which has the advantages of simple operation steps, mild working conditions, low energy consumption, simple and convenient calcium removal method, low production cost and safe operation and is particularly suitable for extracting lithium from high-calcium lithium-containing raw materials.
The technical scheme adopted for solving the technical problems is that the method for extracting lithium from the high-calcium lithium-containing raw material comprises the following steps:
(1) calcium deposition: adding a calcium-containing lithium-containing raw material into a reaction container, adding a calcium precipitator, stirring to generate calcium sulfate crystals, and performing solid-liquid separation to obtain a decalcified lithium-containing mother solution; the calcium sulfate crystals can be used for manufacturing building materials;
(2) and (4) nanofiltration: further removing divalent ions and multivalent ions such as calcium, magnesium and the like from the decalcified lithium-containing mother liquor obtained in the step (1) through a nanofiltration system, namely further removing calcium and removing ions with valence more than or equal to 2 to obtain lithium-containing filtrate;
(3) and (3) evaporation and concentration: and (3) evaporating and concentrating the lithium-containing filtrate obtained in the step (2) to obtain a lithium-rich concentrated solution.
Further, in the step (1), the calcium-containing lithium-containing raw material may be spodumene leaching solution, lepidolite leaching solution or salt lake brine; in the calcium-containing raw material, the content of calcium can be more than or equal to 10 g/L.
Further, in the step (1), the calcium precipitator may be an anhydrous sodium sulfate solution, a sodium sulfate decahydrate solution, or Na2SO4One of the solutions of (a); more preferably, the concentration of sodium sulfate in the solution reaches a saturated state, i.e. the calcium precipitator solution is a saturated sodium sulfate solution, so as to reduce the influence on the volume of the reaction system.
Further, the mass content of sodium sulfate in the calcium precipitator solution is Ca according to the reaction principle2+ + SO4 2- 
CaSO4 
Adding; preferably, in the calcium precipitator solution, the mass content of the sodium sulfate is 1.00-5.00 times of the mass of the calcium contained in the raw materials. The addition of excessive sodium sulfate is beneficial to improving the efficiency of calcium precipitation.
Further, the adding speed of the high-calcium lithium-containing raw material solution and the calcium precipitator solution is set according to the volume of the reaction container and the concentration of reactants; more preferably, the flow rate of the high calcium lithium-containing raw material solution is 2 times or more the flow rate of the calcium precipitant solution. The stirring speed in the reaction zone depends on the volume of the reactor and is preferably such that it is dispersible.
Further, in the step (1), the reaction vessel may be a common vessel, preferably a crystallization reactor.
Further, in the step (1), the separation device may be a conventional separation device such as a circulating water type vacuum pump, a centrifuge, a thickener, a plate-and-frame filter, a belt filter, a cyclone separator, or the like.
Further, in the step (2), the nanofiltration system can be a one-stage or multi-stage nanofiltration device and a matched backwashing device; preferably, the total salt concentration of the divalent ions and the multivalent ions in the discharged concentrated solution is more than 80 g/L.
Further, in the step (2), the nanofiltration membrane used has the following characteristics: the pore diameter of the nanofiltration membrane is nano-scale (10)-9m) suitable for trapping substances with a particle size of about 1nlTl and a molecular weight of 200-l 000. Preferably, the charge effect of the nanofiltration membrane, namely the south-of-the-road effect, is the greatest characteristic of the nanofiltration membrane compared with other membrane technologies, and due to the fact that the surface of the nanofiltration membrane is provided with negative charged groups, through the electrostatic effect, the rejection rate of the nanofiltration membrane on divalent ions and multivalent ions is much higher than that of the divalent ions, and even under very low operating pressure (the pressure is generally 0.5-2.0 MPa, and is 0.5-3.0 MPa lower than the pressure difference required by reverse osmosis separation for achieving the same permeation flux), the nanofiltration membrane still has high desalination performance. Further, in the step (3), the evaporation concentration may be a general heating evaporation device; in mass production, MVR evaporation devices are preferred.
Further, in the step (3), the evaporation time can be determined according to the subsequent processing or application of the obtained concentrated solution, and the required Li is obtained+The concentration requirement of (2) is determined.
Further, in the step (3), the lithium-rich concentrated solution is Li+The concentration of (b) is more than or equal to 12 g/L.
The preferred Mechanical Vapor Recompression (MVR) evaporation technique of the present invention has the following characteristics: an energy-saving technology for reusing the energy of secondary steam generated in an evaporator to reduce the requirement on external energy. The specific process is that secondary steam generated in the evaporation process is compressed by a mechanical steam compressor (the compression medium is generally steam), so that the temperature and the pressure are increased, the heat value is increased, the compressed steam can be used as a heating source and directly enters a heating outer pipe to heat the solution, the latent heat of the secondary steam is released and condensed into condensed water, the feed liquid absorbs the latent heat to generate new secondary steam, the secondary steam is sucked into the mechanical steam compressor to be compressed, and the cyclic evaporation is continuously performed.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, a mirabilite solution is added into a calcium-containing and lithium-containing raw material solution, and the mixture reacts with calcium ions in the calcium-containing and lithium-containing raw material solution to generate calcium sulfate crystal precipitate (which can be used for producing building materials), so that most of calcium ions in the lithium-containing raw material are removed; the mirabilite is low in price, the step is simple to operate, the working condition is mild, the energy consumption is low, the operation is safe, and the environmental pollution is less; all operation processes of the invention are carried out according to safe, energy-saving and environment-friendly conditions; it is suitable for extracting lithium from various lithium-containing materials containing calcium, and is especially suitable for extracting lithium from high-calcium lithium-containing materials.
The specific implementation mode is as follows:
the following examples are provided to illustrate specific embodiments of the present invention.
Example 1
(1) Calcium deposition: the raw material high calcium lithium-containing solution used in this example consisted of: ca2+ 11.93g/L， Li+ 0.79 g/L; adding 10.0kg of the high-calcium lithium-containing solution into a crystallizer with the volume of 10L, and then adding 2.45kg of sodium sulfate solution with the mass concentration of 20%; the feeding flow rate of the high-calcium lithium-containing solution is 111g/min, the feeding flow rate of the sodium sulfate solution is 28g/min, and the rotating speed of a reaction zone of the crystallizer is 12 r/min; after the reaction is finished, calcium sulfate crystal sediment is generated; performing suction filtration by using a circulating water type vacuum pump to perform solid-liquid separation, wherein 0.599kg of solid is obtained in a funnel, the average value of the solid particle size is 280 mu m, and the median value is 300 mu m, namely the obtained solid particles through crystallization are large, the mother liquor entrainment is small, and the loss to lithium is small; pumping the filtrate bottle to obtain 11.75kg of lithium-containing mother liquor; the composition was analyzed as follows: ca2+ 0.20 g/L，Li+0.67g/L, the calcium removal rate is 98.03 percent, and the lithium yield is 98.67 percent;
(2) and (4) nanofiltration: leading the lithium-containing mother liquor obtained in the step (1) into a nanofiltration device (manufacturer: Sanda membrane), leading the strong brine into a nanofiltration liquid storage tank again through an internal pipeline, and circulating for three times through a nanofiltration membrane; the total concentration of divalent and multivalent ions in the discharged concentrated solution is 85 g/L; the total mass of the obtained lithium-containing filtrate was 10.93kg, and the composition thereof was： Ca2+ 0.001 g/L,Li+0.64 g/L; wherein Li+The yield is 87.28%;
(3) and (3) evaporation and concentration: placing the container containing the lithium-containing filtrate obtained in step (2) on an electric hot plate for heating and evaporation at the highest temperature of 105 ℃ for 10 hours to obtain 0.313kg of lithium-rich concentrated solution, wherein Li is contained in the lithium-rich concentrated solution+The concentration of (A) is 19.53 g/L; li+The yield thereof was found to be 87.4%.
Example 2
(1) Calcium deposition: the raw material high-calcium lithium-containing solution used in this example was composed of: ca2+ 18.04g/L，Li+ 0.83 g/L. Adding 10.0kg of the high-calcium lithium-containing solution into a crystallizer with the volume of 10L, and then adding 2.0kg of sodium sulfate solution with the mass concentration of 30%; the feeding flow rate of the high-calcium lithium-containing solution is 166g/min, the feeding flow rate of the sodium sulfate solution is 33g/min, and the rotating speed of a reaction zone of the crystallizer is 15 r/min; after the reaction is finished, calcium sulfate crystal sediment is generated; carrying out suction filtration by using a circulating water type vacuum pump for carrying out solid-liquid separation, wherein 850g of solid is obtained in a funnel, the average value of the particle size of the solid is 268 mu m, and the median value is 285 mu m, namely the obtained solid particles through crystallization are large, the entrainment of mother liquor is small, and the loss of lithium is small; pumping the filter flask to obtain 11.15kg of lithium-containing mother liquor; the composition was analyzed as follows: ca2+ 1.49g/L，Li+0.73g/L, the calcium removal rate is 90.79%, and the lithium yield is 98.07%;
(2) nanofiltration, namely introducing the lithium-containing mother liquor obtained in the step (1) into a nanofiltration device (manufacturer: Sanda membrane), introducing the strong brine into a nanofiltration liquid storage tank again through an internal pipeline, and circulating through a nanofiltration membrane for three times to reduce the loss of lithium in the strong brine; passing through three-stage nanofiltration membrane in a nanofiltration device to obtain 10.23kg of lithium-containing filtrate, which comprises the following components: ca2+ 0.01 g/L,Li+0.71g/L, wherein Li+The yield is 89.23%;
(3) and (3) evaporation and concentration: placing the container containing the lithium-containing filtrate obtained in step (2) on an electric hot plate for heating and evaporation at the highest temperature of 105 ℃ for 9.5h to obtain 0.558kg of lithium-rich concentrated solution, wherein Li is contained in the lithium-rich concentrated solution+Has a concentration of 12.12g/L, Li+The yield thereof was found to be 93.12%.
The above-mentioned embodiments are only two specific embodiments of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the technical idea of the present application, several changes and modifications can be made, which are all within the protection scope of the present application.
Claims (10)
1. A method for extracting lithium from a high-calcium lithium-containing raw material is characterized by comprising the following steps:
(1) calcium deposition: adding a calcium-containing lithium-containing raw material into a reaction container, adding a calcium precipitator, stirring to generate calcium sulfate crystals, and performing solid-liquid separation to obtain a decalcified lithium-containing mother solution;
(2) and (4) nanofiltration: nano-filtering the decalcified lithium-containing mother liquor obtained in the step (1) by a nano-filtering system, further decalcifying and removing other ions with valence more than or equal to 2 to obtain lithium-containing filtrate;
(3) and (3) evaporation and concentration: and (3) evaporating and concentrating the lithium-containing filtrate obtained in the step (2) to obtain a lithium-rich concentrated solution.
2. The method of claim 1, wherein in step (1), the lithium-containing calcium-containing material is spodumene leachate, lepidolite leachate, or salt lake brine.
3. The method of claim 1, wherein in step (1), the calcium precipitating agent is thenardite solution, Na2SO4One of the solutions of (1).
4. The method of claim 3, wherein the concentration of sodium sulfate in the solution is saturated.
5. The method for extracting lithium from a high-calcium lithium-containing raw material according to any one of claims 1 to 4, wherein the mass content of sodium sulfate in the calcium precipitator solution is 1.00 to 5.00 times of the mass of calcium contained in the raw material.
6. The method of claim 1 to 5, wherein the ratio of the feeding rates of the high calcium lithium-containing raw material solution and the calcium precipitant solution is such that the flow rate of the high calcium lithium-containing raw material solution is 2 times or more the flow rate of the calcium precipitant solution.
7. The method for extracting lithium from a high-calcium lithium-containing raw material according to any one of claims 1 to 6, wherein in the step (1), the reaction vessel is a crystallization reactor.
8. The method for extracting lithium from a high-calcium lithium-containing raw material according to any one of claims 1 to 7, wherein in the step (1), the separation device is a circulating water type vacuum pump, a thickener or a plate-and-frame filter.
9. The method for extracting lithium from high-calcium lithium-containing raw material according to any one of claims 1 to 8, wherein in the step (2), the nanofiltration system is one or more stages of nanofiltration devices and matched backwashing devices; the nanofiltration membrane used has negatively charged groups.
10. The method for extracting lithium from a high-calcium lithium-containing raw material according to any one of claims 1 to 9, wherein in the step (3), the evaporation and concentration device is an MVR evaporation device.
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| 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 |
| CN111268701A (en) * | 2020-03-23 | 2020-06-12 | 中国科学院青海盐湖研究所 | Method for preparing battery-grade lithium hydroxide by using lepidolite |
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