CN113104868A - Method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene - Google Patents
Method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene Download PDFInfo
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Abstract
The invention aims to provide a method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene. The method has simple process, can fully utilize low-grade or weathered spodumene raw ore, realizes changing waste into valuable, and has great economic benefit and environmental protection benefit.
Description
Technical Field
The invention belongs to the technical field of mineral processing, and particularly relates to a method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene.
Background
Lithium and lithium compounds have unique and excellent physical properties and chemical properties, and are widely applied to the fields of high-energy batteries, synthetic rubbers, alloys, air conditioners, medicines, welding and the like, so that the lithium and lithium compounds become new strategic resources gradually. For lithium-containing ores, the great difference of ore properties and the difference of lithium content are caused by the diversity of lithium-containing minerals, and simultaneously, the complex reaction and the product diversity of the lithium-containing ores in the forming process become important reasons of the complex sorting process of the lithium ores.
Low grade spodumene (also known as spodumene) is often a product of spodumene alteration, Li2The content of O is low, the selectivity is poor, and the factors make the situation that the enrichment is difficult and the selective recovery of the recovered lithium element more unfavorable. The existing spodumene raw ore dressing method mainly comprises the following stepsThe flotation method has large environmental protection pressure, high requirement on the grade of spodumene raw ore and high Li requirement2Low grade ore with O content below 1.0% can only be discarded.
The weathered spodumene is loose, crisp and soft after being leached by weathering, and is difficult to be selected by the traditional mineral separation method and difficult to be treated.
How to reasonably apply the low-grade or weathered spodumene, improve the economic value of the spodumene and realize the change of waste into valuable is a technical problem to be solved urgently at present.
Disclosure of Invention
The invention aims to provide a method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene, which has a simple process, can fully utilize low-grade or weathered spodumene raw ore, realizes changing waste into valuable, and has great economic benefit and environmental protection benefit.
The invention aims to realize the technical scheme that the method for preparing the battery-grade lithium carbonate from the low-grade or weathered spodumene comprises the following steps:
s1, crushing, namely crushing the low-grade or weathered spodumene raw ore into blocks with the diameter of less than 5 cm;
s2, preheating, namely preheating the crushed massive ore S1 to the temperature of 200-500 ℃;
s3, sintering, namely transferring the preheated massive ore in the step S2 to a sintering furnace, heating to 1000-1100 ℃, and sintering for 0.5 h;
s4, cooling and screening, namely naturally cooling the powder sintered in the step S3 to normal temperature, and then screening, wherein the powder with the fineness of more than 100 meshes is the selected lithium concentrate powder;
s5, mixing acid, namely mixing the lithium concentrate powder obtained in the step S4 and 98% sulfuric acid according to the mass ratio of 1: 0.22-0.24, and uniformly mixing in a double-helix mixer;
s6, roasting, transferring the mixed material obtained in the step S5 to an acidification roasting kiln, and roasting for 1h at the temperature of 280-300 ℃;
s7, curing, namely stacking the roasted material obtained in the step S6 for 12 hours for curing;
s8, leaching, namely adding water into the cured material obtained in the step S7, pulping, and adjusting the pH value to 5.5-6 by using calcium carbonate; adjusting pH to 7.5-8 with calcium hydroxide;
s9, filtering, namely filtering the mixture obtained in the step S8, wherein the filtrate is lithium sulfate;
s10, removing impurities, namely, further filtering the filtrate obtained in the step S9 by using a precision filter, and removing the impurities;
s11, detecting the content, namely detecting the content of lithium sulfate in the filtrate obtained in the step S10;
s12, reacting the saturated solution of sodium carbonate with lithium sulfate according to the content of lithium sulfate detected in the step S11, and adding CO according to the ratio of Li to CO3 2-The molar ratio is 2: 1.1, preparing a saturated sodium carbonate solution, filtering the saturated sodium carbonate solution, heating to 95-100 ℃, adding the lithium sulfate obtained in the step S10 into the saturated sodium carbonate solution at a constant speed, and stirring uniformly;
s13, hot filtering, namely hot filtering the mixture obtained in the step S12 to obtain a solid lithium carbonate crude product and liquid sodium sulfate;
s14, stirring and washing, namely stirring and washing the solid lithium carbonate crude product obtained in the step S13 at high temperature;
s15, filtering and leaching, namely, hot filtering the mixture obtained in the step S14 and then leaching with hot water;
and S16, drying, namely drying the material washed in the step S14 at 200 ℃ for 2-3h to obtain the battery-grade lithium carbonate.
Further, in step S1, the lithium oxide content of the low grade or weathered spodumene is 1.0%.
Further, the content of lithium oxide in the lithium concentrate ore powder in the step S4 reaches 4.0-4.8%; the lithium oxide yield reaches more than 85 percent.
Further, the stirring speed of the double-helix mixer in the step S5 is 80-120 r/min, and the mixing time is 20-30 min.
Further, the solid-liquid mass ratio after the size mixing in the step S8 is 30% to 40%.
Further, the stirring speed of step S12 is 100-200 rpm, and the stirring time is 0.5 h.
Further, the stirring temperature of step S14 is 95-100 ℃, the stirring speed is 100-.
The method for preparing the battery-grade lithium carbonate from the low-grade or weathered spodumene has a simple process, can fully utilize the low-grade or weathered spodumene raw ore, realizes changing waste into valuable, and has great economic benefit and environmental protection benefit.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A method for preparing battery-grade lithium carbonate from low-grade spodumene comprises the following steps:
s1, crushing, namely crushing 1000kg of low-grade spodumene raw ore with the lithium oxide content of 1.0% into blocks with the diameter of less than 5 cm;
s2, preheating, namely preheating the crushed massive ore S1 by blowing hot air to ensure that the temperature of the crushed massive ore reaches 300 ℃;
s3, sintering, namely transferring the preheated massive ore obtained in the step S2 to a sintering furnace, heating to 1050 ℃, and sintering for 50 min;
s4, cooling and screening, namely naturally cooling the powder sintered in the step S3 to normal temperature, and then screening, wherein the powder with the fineness of more than 100 meshes is the selected lithium concentrate powder; the lithium oxide content of the lithium concentrate powder is 4.0 percent;
s5, mixing acid, namely mixing the lithium concentrate powder obtained in the step S4 and 98% sulfuric acid according to the mass ratio of 1: 0.22, uniformly mixing in a double-helix mixer, wherein the stirring speed of the double-helix mixer is 80 revolutions per minute, and the mixing time is 30 minutes;
s6, roasting, namely transferring the mixed material obtained in the step S5 to an acidification roasting kiln, and roasting for 1h at 280 ℃;
s7, curing, namely stacking the roasted material obtained in the step S6 for 12 hours for curing;
s8, leaching, namely adding water into the cured material obtained in the step S7, mixing the slurry, wherein the solid-liquid mass ratio after mixing is 30%, and the pH value is adjusted to 5.5 by using calcium carbonate; then adjusting the pH value to 7.5 by using calcium hydroxide;
s9, filtering, namely filtering the mixture obtained in the step S8, wherein the filtrate is lithium sulfate;
s10, removing impurities, namely, further filtering the filtrate obtained in the step S9 by using a precision filter, and removing the impurities;
s11, detecting the content, namely detecting the content of lithium sulfate in the filtrate obtained in the step S10;
s12, according to the content of lithium sulfate detected in the step S11, according to Li to CO3 2-The molar ratio is 2: 1.1, preparing a saturated sodium carbonate solution, filtering the saturated sodium carbonate solution, heating to 95 ℃, adding the lithium sulfate obtained in the step S10 into the saturated sodium carbonate solution, and stirring uniformly at a stirring speed of 100 revolutions per minute for 0.5 h;
s13, hot filtering, namely hot filtering the mixture obtained in the step S12 to obtain a solid lithium carbonate crude product and liquid sodium sulfate;
s14, stirring and washing, namely stirring and washing the solid lithium carbonate crude product obtained in the step S13 at a high temperature, wherein the stirring and washing temperature is 95 ℃, the stirring speed is 100 r/min, and the stirring time is 0.5 h;
s15, filtering and leaching, namely, hot filtering the mixture obtained in the step S14 and then leaching with hot water;
and S16, drying, namely drying the material washed in the step S14 at 200 ℃ for 2h to obtain 20.01kg of battery-grade lithium carbonate.
Example 2
A method for preparing battery-grade lithium carbonate from weathered spodumene comprises the following steps:
s1, crushing, namely crushing 1000kg of weathered spodumene raw ore with the lithium oxide content of 1.0% into blocks with the diameter of less than 5 cm;
s2, preheating, namely preheating the crushed massive ore S1 by blowing hot air to ensure that the temperature of the crushed massive ore reaches 200 ℃;
s3, sintering, namely transferring the preheated massive ore in the step S2 to a sintering furnace, heating to 1100 ℃, and sintering for 0.5 h;
s4, cooling and screening, namely naturally cooling the powder sintered in the step S3 to normal temperature, and then screening, wherein the powder with the fineness of more than 100 meshes is the selected lithium concentrate powder; the lithium oxide content of the lithium concentrate powder is 4.4%;
s5, mixing acid, namely mixing the lithium concentrate powder obtained in the step S4 and 98% sulfuric acid according to the mass ratio of 1: 0.24, uniformly mixing in a double-helix mixer, wherein the stirring speed of the double-helix mixer is 120 revolutions per minute, and the mixing time is 20 minutes;
s6, roasting, namely transferring the mixed material obtained in the step S5 to an acidification roasting kiln, and roasting for 1h at 300 ℃;
s7, curing, namely stacking the roasted material obtained in the step S6 for 12 hours for curing;
s8, leaching, namely adding water into the cured material obtained in the step S7, mixing the slurry, wherein the solid-liquid mass ratio after mixing is 35%, and adjusting the pH value to 6 by using calcium carbonate; then adjusting the pH value to 8 by using calcium hydroxide;
s9, filtering, namely filtering the mixture obtained in the step S8, wherein the filtrate is lithium sulfate;
s10, removing impurities, namely, further filtering the filtrate obtained in the step S9 by using a precision filter, and removing the impurities;
s11, detecting the content, namely detecting the content of lithium sulfate in the filtrate obtained in the step S10;
s12, according to the content of lithium sulfate detected in the step S11, according to Li to CO3 2-The molar ratio is 2: 1.1, preparing a saturated sodium carbonate solution, filtering the saturated sodium carbonate solution, heating to 100 ℃, adding the lithium sulfate obtained in the step S10 into the saturated sodium carbonate solution, and stirring uniformly at a stirring speed of 200 revolutions per minute for 0.5 h;
s13, hot filtering, namely hot filtering the mixture obtained in the step S12 to obtain a solid lithium carbonate crude product and liquid sodium sulfate;
s14, stirring and washing, namely stirring and washing the solid lithium carbonate crude product obtained in the step S13 at a high temperature, wherein the stirring and washing temperature is 100 ℃, the stirring speed is 130 r/min, and the stirring time is 0.5 h;
s15, filtering and leaching, namely, hot filtering the mixture obtained in the step S14 and then leaching with hot water;
and S16, drying, namely drying the material washed in the step S14 at 200 ℃ for 3 hours to obtain 19.98kg of battery-grade lithium carbonate.
Example 3
A method for preparing battery-grade lithium carbonate from low-grade spodumene comprises the following steps:
s1, crushing, namely crushing 1000kg of low-grade spodumene raw ore with the lithium oxide content of 0.98% into blocks with the diameter of less than 5 cm;
s2, preheating, namely preheating the crushed massive ore S1 by blowing hot air to ensure that the temperature of the crushed massive ore reaches 400 ℃;
s3, sintering, namely transferring the preheated massive ore obtained in the step S2 to a sintering furnace, heating to 1050 ℃, and sintering for 0.5 h;
s4, cooling and screening, namely naturally cooling the powder sintered in the step S3 to normal temperature, and then screening, wherein the powder with the fineness of more than 100 meshes is the selected lithium concentrate powder; the lithium oxide content of the lithium concentrate powder is 4.6%;
s5, mixing acid, namely mixing the lithium concentrate powder obtained in the step S4 and 98% sulfuric acid according to the mass ratio of 1: 0.23, uniformly mixing in a double-helix mixer, wherein the stirring speed of the double-helix mixer is 110 r/min, and the mixing time is 25 min;
s6, roasting, namely transferring the mixed material obtained in the step S5 to an acidification roasting kiln, and roasting for 1h at 290 ℃;
s7, curing, namely stacking the roasted material obtained in the step S6 for 12 hours for curing;
s8, leaching, namely adding water into the cured material obtained in the step S7, mixing the slurry, wherein the solid-liquid mass ratio after mixing is 40%, and the pH value is adjusted to 5.6 by using calcium carbonate; then adjusting the pH value to 7.8 by using calcium hydroxide;
s9, filtering, namely filtering the mixture obtained in the step S8, wherein the filtrate is lithium sulfate;
s10, removing impurities, namely, further filtering the filtrate obtained in the step S9 by using a precision filter, and removing the impurities;
s11, detecting the content, namely detecting the content of lithium sulfate in the filtrate obtained in the step S10;
s12, according to the content of lithium sulfate detected in the step S11, according to Li to CO3 2-The molar ratio is 2: 1.1, preparing a saturated sodium carbonate solution, filtering the saturated sodium carbonate solution, heating to 98 ℃, adding the lithium sulfate obtained in the step S10 into the saturated sodium carbonate solution, and stirring uniformly at a stirring speed of 150 revolutions per minute for 0.5 h;
s13, hot filtering, namely hot filtering the mixture obtained in the step S12 to obtain a solid lithium carbonate crude product and liquid sodium sulfate;
s14, leaching, namely stirring and washing the solid lithium carbonate crude product obtained in the step S13 at a high temperature of 100 ℃, wherein the stirring speed is 110 r/min, and the stirring time is 0.5 h;
s15, filtering and leaching, namely, hot filtering the mixture obtained in the step S14 and then leaching with hot water;
and S16, drying, namely drying the material washed in the step S14 at 200 ℃ for 2.5 hours to obtain 19.04kg of battery-grade lithium carbonate.
Example 4
A method for preparing battery-grade lithium carbonate from weathered spodumene comprises the following steps:
s1, crushing, namely crushing 1000kg of weathered spodumene raw ore with the lithium oxide content of 0.95% into blocks with the diameter of less than 5 cm;
s2, preheating, namely preheating the crushed massive ore S1 by blowing hot air to ensure that the temperature of the crushed massive ore reaches 500 ℃;
s3, sintering, namely transferring the preheated massive ore in the step S2 to a sintering furnace, heating to 1020 ℃, and sintering for 0.5 h;
s4, cooling and screening, namely naturally cooling the powder sintered in the step S3 to normal temperature, and then screening, wherein the powder with the fineness of more than 100 meshes is the selected lithium concentrate powder; the lithium oxide content of the lithium concentrate powder is 4.8%;
s5, mixing acid, namely mixing the lithium concentrate powder obtained in the step S4 and 98% sulfuric acid according to the mass ratio of 1: 0.22, uniformly mixing in a double-helix mixer, wherein the stirring speed of the double-helix mixer is 100 revolutions per minute, and the mixing time is 30 minutes;
s6, roasting, namely transferring the mixed material obtained in the step S5 to an acidification roasting kiln, and roasting for 1h at 285 ℃;
s7, curing, namely stacking the roasted material obtained in the step S6 for 12 hours for curing;
s8, leaching, namely adding water into the cured material obtained in the step S7, mixing the slurry, wherein the solid-liquid mass ratio after mixing is 36%, and the pH value is adjusted to 5.8 by calcium carbonate; then adjusting the pH value to 7.6 by using calcium hydroxide;
s9, filtering, namely filtering the mixture obtained in the step S8, wherein the filtrate is lithium sulfate;
s10, removing impurities, namely, further filtering the filtrate obtained in the step S9 by using a precision filter, and removing the impurities;
s11, detecting the content, namely detecting the content of lithium sulfate in the filtrate obtained in the step S10;
s12, according to the content of lithium sulfate detected in the step S11, according to Li to CO3 2-The molar ratio is 2: 1.1, preparing a saturated sodium carbonate solution, filtering the saturated sodium carbonate solution, heating to 96 ℃, uniformly stirring the lithium sulfate obtained in the step S10 into the saturated sodium carbonate solution at a stirring speed of 120 revolutions per minute for 0.5 h;
s13, hot filtering, namely hot filtering the mixture obtained in the step S12 to obtain a solid lithium carbonate crude product and liquid sodium sulfate;
s14, leaching, namely stirring and washing the solid lithium carbonate crude product obtained in the step S13 at a high temperature of 98 ℃, wherein the stirring speed is 120 r/min, and the stirring time is 0.5 h;
s15, filtering and leaching, namely, hot filtering the mixture obtained in the step S14 and then leaching with hot water;
and S16, drying, namely drying the material washed in the step S14 at 200 ℃ for 2.2h to obtain 19.48kg of battery-grade lithium carbonate.
The lithium carbonates prepared in examples 1 to 4 were tested, and the test results were as follows:
| item | Example 1 | Example 2 | Example 3 | Example 4 |
| Li2CO3 content (%) | 99.65 | 99.72 | 99.73 | 99.69 |
| Na(％) | 0.022 | 0.024 | 0.022 | 0.023 |
| Mg(％) | 0.0071 | 0.0075 | 0.0067 | 0.0072 |
| Ca(％) | 0.0045 | 0.0041 | 0.0035 | 0.0042 |
| K(％) | 0.00076 | 0.00091 | 0.00087 | 0.00083 |
| Fe(％) | 0.00082 | 0.00084 | 0.00083 | 0.00082 |
| Zn(％) | <0.0001 | <0.0001 | <0.0001 | <0.0001 |
| Cu(％) | <0.0001 | <0.0001 | <0.0001 | <0.0001 |
| Pb(％) | <0.0001 | <0.0001 | <0.0001 | <0.0001 |
| Si(％) | 0.0022 | 0.0025 | 0.0022 | 0.0024 |
| Al(％) | 0.00082 | 0.00085 | 0.00087 | 0.00084 |
| Mn(％) | <0.0001 | <0.0001 | <0.0001 | <0.0001 |
| Ni(％) | 0.00062 | 0.00074 | 0.00063 | 0.00062 |
| SO4 2-(％) | 0.065 | 0.066 | 0.071 | 0.068 |
| Cl-(％) | 0.0022 | 0.0026 | 0.0024 | 0.0022 |
| Moisture (%) | 0.10 | 0.12 | 0.11 | 0.10 |
Therefore, the method for preparing the battery-grade lithium carbonate from the low-grade or weathered spodumene has a simple process, can prepare the battery-grade lithium carbonate from the low-grade or weathered spodumene raw ore, changes waste into valuable, and has great economic benefit and environmental protection benefit.
It should be understood that the examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that any changes and modifications to the present invention may occur to those skilled in the art after reading the present teachings, and such equivalents are also intended to be limited by the appended claims.
Claims (7)
1. A method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene, which is characterized in that the method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene comprises the following steps:
s1, crushing, namely crushing the low-grade or weathered spodumene raw ore into blocks with the diameter of less than 5 cm;
s2, preheating, namely preheating the crushed massive ore S1 to the temperature of 200-500 ℃;
s3, sintering, namely transferring the preheated massive ore in the step S2 to a sintering furnace, heating to 1000-1100 ℃, and sintering for 0.5 h;
s4, cooling and screening, namely naturally cooling the powder sintered in the step S3 to normal temperature, and then screening, wherein the powder with the fineness of more than 100 meshes is the selected lithium concentrate powder;
s5, mixing acid, namely mixing the lithium concentrate powder obtained in the step S4 and 98% sulfuric acid according to the mass ratio of 1: 0.22-0.24, and uniformly mixing in a double-helix mixer;
s6, roasting, transferring the mixed material obtained in the step S5 to an acidification roasting kiln, and roasting for 1h at the temperature of 280-300 ℃;
s7, curing, namely stacking the roasted material obtained in the step S6 for 12 hours for curing;
s8, leaching, namely adding water into the cured material obtained in the step S7, pulping, and adjusting the pH value to 5.5-6 by using calcium carbonate; adjusting pH to 7.5-8 with calcium hydroxide;
s9, filtering, namely filtering the mixture obtained in the step S8, wherein the filtrate is lithium sulfate;
s10, removing impurities, namely, further filtering the filtrate obtained in the step S9 by using a precision filter, and removing the impurities;
s11, detecting the content, namely detecting the content of lithium sulfate in the filtrate obtained in the step S10;
s12, reacting the saturated solution of sodium carbonate with lithium sulfate according to the content of lithium sulfate detected in the step S11, and adding CO according to the ratio of Li to CO3 2-The molar ratio is 2: 1.1, preparing a saturated sodium carbonate solution, filtering the saturated sodium carbonate solution, and heatingWhen the temperature is 95-100 ℃, adding the lithium sulfate obtained in the step S10 into the saturated solution of sodium carbonate at a constant speed, and stirring uniformly;
s13, hot filtering, namely hot filtering the mixture obtained in the step S12 to obtain a solid lithium carbonate crude product and liquid sodium sulfate;
s14, stirring and washing, namely stirring and washing the solid lithium carbonate crude product obtained in the step S13 at high temperature;
s15, filtering and leaching, namely, hot filtering the mixture obtained in the step S14 and then leaching with hot water;
and S16, drying, namely drying the material washed in the step S14 at 200 ℃ for 2-3h to obtain the battery-grade lithium carbonate.
2. The method for preparing battery grade lithium carbonate from low grade or weathered spodumene of claim 1, wherein said low grade or weathered spodumene has a lithium oxide content of 1.0% in step S1.
3. The method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene according to claim 1, wherein the lithium oxide content of the spodumene powder in step S4 is 4.0-4.8%; the lithium oxide yield reaches more than 85 percent.
4. The method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene according to claim 1, wherein the stirring speed of the double-helix blender in the step S5 is 80-120 r/min, and the mixing time is 20-30 min.
5. The method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene according to claim 1, wherein the solid-liquid mass ratio after size mixing in the step S8 is 30-40%.
6. The method for preparing battery-grade lithium carbonate from low-grade or weathered spodumene as claimed in claim 1, wherein the stirring speed of step S12 is 100-200 rpm, and the stirring time is 0.5 h.
7. The method for preparing battery grade lithium carbonate from low-grade or weathered spodumene according to any one of claims 1 to 6, wherein the agitation temperature of step S14 is 95-100 ℃, the agitation speed is 100-.
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Application publication date: 20210713 |