CN101974678A - Method for extracting lithium and other alkali metal elements from lepidolite mineral - Google Patents
Method for extracting lithium and other alkali metal elements from lepidolite mineral Download PDFInfo
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Abstract
The invention discloses a high-temperature mineral phase reconstruction method for extracting lithium and other alkali metal elements from lepidolite mineral, comprising the following steps: mixing raw materials, pelletizing, calcining at high temperature, water quenching, ball milling, dissolving out, producing compounds and the like. The invention teaks raw mineral component composition to design target reconstruction mineral and composition to obtain the purpose of optimizing processes, lowering energy consumption and cost of treatment process and efficiently extracting lithium, potassium, rubidium, caesium and the like. Silicon and aluminum in lepidolite can enter anorthite type mineral phase (CaO.Al2O3.2SiO2, (Ca, Na)O. (Al, Si)2O3.2SiO2) and calcium ash quarry phase (CaO.SiO2) after mineral phase reconstruction, and do not dissolve in water and aqueous solution. After mineral phase reconstruction reaction, fluorine in lepidolite enters calcium fluoride mineral phase and does not dissolve in water and aqueous solution. Lithium and other alkali metal elements in lepidolite enter salt (chloride, sulfate) or alkali (hydroxide) phase of lithium and other alkali metal elements after mineral phase reconstruction reaction and can be dissolved in water and aqueous solution.
Description
Technical field
The invention belongs to the basic metal metallurgy method in the nonferrous metallurgy field, be specifically related to a kind of method of from the lithionite ore deposit, extracting lithium and other alkali metal.
Background technology
" lithium is the energy source element of 21 century ", lithium and lithium salts are widely used in fields such as high energy green battery, aerospace, nucleosynthesis generating, and its demand increases day by day; " 21 century is the century of lithium ", the lithium industrial expansion is generally paid attention in countries in the world.There are abundant lithionite resource, its Li in China
2O content is generally about 4%; Exploitation lithionite resource tool has very important significance.
At present, the metallurgical method of extraction lithium mainly contains the lime-roasting method, presses cooking method, sulfuric acid process, chlorinating roasting etc. from the lithionite ore deposit.
(1) lime-roasting method: lime method is handled lithionite and is produced lithium salts, be exactly with Wingdale through after the fragmentation with lithionite by 3: 1 part by weight in ball mill ball milling, mix; Through 1150～1200 ℃ of high-temperature roasting ripe materials; Grog is through shrend, fine grinding, leaching, thus the extraction lithium.
(2) press cooking method: with the lithionite concentrate after feeding the steam roasting defluorinate under 870～930 ℃ of temperature, by roasting material: calcium oxide: the weight ratio of yellow soda ash (or sodium hydroxide) is 10: (3～10): (1～6), liquid-solid ratio are 4～6, compound is ground size mixing that to be placed on temperature be that 120～150 ℃, pressure are (2～5) * 10
5Carry out the stripping lithium in the autoclave of handkerchief.
(3) sulfuric acid process.Handle the lithionite defluorinate with high-temperature vapor, adopt sulfuric acid process to handle lithionite then; By lithionite: the vitriolate of tartar weight ratio is 1: (0.6～1.0) batching, through batch mixing, make ball, at 950～1100 ℃ of roasting temperatures, dilute sulphuric acid leaches lithium.
(4) chlorinating roasting.Roasting lithium ore under the chlorizating agent effect makes lithium in the ore and other valuable element potassium, rubidium, caesium etc. change muriate into and is comprehensively extracted.Yu Baoyu etc. are to lithionite and NaCl and NaCl-CaCl
2Interaction study, experimental result shows that temperature of reaction is 800 ℃, alkali ratio in ore deposit is that 1: 1 o'clock lithium, rubidium, the caesium rate of decomposition in the lithionite ore deposit all reaches 80%.
Lime-roasting method production process adopts lime, the treatment temp height of high adapted amount, and inventory is big, energy consumption is high and production efficiency is low, production cost height when handling low-grade lithionite ore deposit.Press cooking method and sulfuric acid process to need in advance lithionite is carried out roasting transition, high-temperature vapor defluorinate, pyroreaction generates hydrogen fluoride gas, thereby brings environmental pollution and to the equipment corrosion problem; Press cooking method to adopt high-voltage high-temperature equipment and operation, investment and running cost height simultaneously; Sulfuric acid process adopts materials such as vitriolate of tartar, sulfuric acid, and process cost is increased.The temperature control requirement height of chlorinating roasting: maturing temperature is low excessively, fully chlorination of lithium concentrate, and the lithium rate of recovery is low; Temperature is too high, grog fusing bonding, and in rotary kiln ring formation, make operational difficulty.
Therefore, how economic, development and utilization lithionite ore efficiently, significant to China's lithium industry.
Summary of the invention
Because the existing problem in existing development and use lithionite ore deposit, make the technician press for to find one for large-scale development lithionite resource, be extracted in the compound of metallic elements such as the lithium that accounts for critical role in the global economy, potassium, rubidium, caesium, the method for a kind of economy, efficient development and utilization lithionite ore resource is provided.
The contriver can adopt the ore phase reconstruction method to handle lithionite by discovering, and the purpose of ore phase reconstruction, be to re-construct by handling the mineral structure that former mineral pair wherein contains the valency composition, make valuable constituent be in separable state, thereby effectively separate valuable constituent, promptly at the composition and the mineral structure of lithionite, design ore phase reconstruction target, realize that lithium, potassium, rubidium and caesium etc. become Yi Rong (in water) compound in the lithionite ore deposit, reach with gangue contents such as silicon, aluminium by dissolving and separate.
The structural formula of lithionite is
K{Li
2-xAl
1+x[Al
2xSi
4-2xO
10][F
1-y(OH)
y]
2}(x：0～0.50)
The x value that has practicality to carry the lithionite of lithium value mostly is 0.2～0.5.The lithium position can be replaced by sodium, potassium, rubidium and caesium in the formula; Be to realize separating and extraction of lithium, rubidium, caesium and potassium, must destroy and recombinate the lithionite structure, make lithium, rubidium, caesium and potassium be in can with aluminium, siliceous isolating state.Compositing characteristic (silica alumina ratio) according to the lithionite ore deposit can be reconstructed into lime feldspar CaOAl with gangue contents such as silicon, aluminium
2O
32SiO
2With wollastonite CaOSiO
2Deng material; In the ore phase reconstruction process, meeting produces silicon based on lime feldspar and moves into the aluminium position, the silicon-aluminium mixing on the aluminium position occurs, is balancing charge Sodium mixing on the sodium position that occurs sodium replacement calcium on the molybdenum position simultaneously, the lime feldspar type of generation aluminium position and the mixing of calcium position ((Na, Ca)
2O (Si, Al)
2O
32SiO
2) the ore deposit phase.Therefore, with producing ore phase reconstruction composition (as: CaO and Na
2O) alkali metal compound and alkaline earth metal compound all can be used as the ore phase reconstruction agent of lithionite; But must be molten altogether in ore phase reconstruction temperature and flux (low melting component), so that infiltration, diffusion and the phase reaction of generation solid-liquid effectively realize the reconstruct of solid phase ore deposit phase.
Owing to contain fluorine in the lithionite, the present invention is fixed on fluorine in the solid phase composition, prevents that the volatilization of fluorochemical gas phase from influencing environment.Alkaline-earth metal (calcium, strontium and barium) compound is fixing fluorine all, so adopts the compound of alkaline-earth metal (calcium, strontium and barium) among the present invention, in the ore phase reconstruction process fluorine is fixed up with alkaline-earth metal fluoride.
As when selecting for use calcium chloride, sodium-chlor to be ore phase reconstruction agent, fluorine fixing material and flux, under 900 ℃, lithionite discharges alkali metal compound, the ore phase reconstruction reaction takes place:
K{Li
2-xAl
1+x[Al
2xSi
4-2xO
10][F
1-y(OH)
y]
2}+CaCl
2+NaCl——LiCl+KCl+CaO·Al
2O
3·2SiO
2+(Ca，Na)O·(Al，Si)
2O
3·2SiO
2+CaO·SiO
2+CaF
2+H
2O
By method of the present invention, can consist of the basis by former mineral, only need to add and determine required ore phase reconstruction auxiliary agent of reconstruct mineral structure and restructuring procedure condition, just can reach economic, efficient development and utilization lithionite ore resource.
The high temperature ore phase reconstruction method of extracting lithium and other alkali metal element from the lithionite ore deposit mainly may further comprise the steps: the material mixing material, make ball, high-temperature roasting, shrend ball milling, stripping and compound production etc.
Technical scheme of the present invention may further comprise the steps:
1) material mixing material: lithionite ore deposit and ore phase reconstruction auxiliary agent are mixed; The ore phase reconstruction auxiliary agent is the mixture of ore phase reconstruction agent and flux; Described ore phase reconstruction agent is that lithionite generates the alkali earth metal in the ore phase reconstruction composition set and the compound of alkali metal; Described flux is selected from and is the simplification compound or the mixture of molten state under the ore phase reconstruction temperature of reaction; The add-on of ore phase reconstruction agent is at least ore phase reconstruction reaction aequum takes place, and it is poor to deduct the amount of the corresponding composition that exists in the lithionite ore deposit, to guarantee the generation of reconstruct ore deposit phase;
2) make ball: with compacting or group's system mode with 1) mix material in the step and make the rawore pelletizing;
3) roasting: above-mentioned rawore pellet roasting is carried out the ore phase reconstruction reaction, generate the ripe ore deposit of the ore phase reconstruction pelletizing that contains valuable constituent compound soluble in water; Maturing temperature be controlled at the fusing point of flux above, below the pelletizing softening temperature of ore deposit;
4) quenching, ball milling and stripping valuable constituent.
The alkali metal salt soln circulation of water or last quenching operation output is carried out quenching to ripe ore deposit pelletizing.By wet ball-milling, stripping, make compound dissolutions such as valuable constituent such as lithium, potassium, sodium, rubidium, caesium enter solution.The stripping temperature is normal temperature～70 ℃.
The present invention is preferably with Li
2O content is that lithionite ore deposit and the ore phase reconstruction auxiliary agent of 3-6% is 1 by mass ratio: (0.7～1.2) batching mixes.
The reaction of described ore phase reconstruction, generate lime feldspar type ore deposit that the reconstruct ore deposit of containing valuable constituent compound soluble in water is meant that mutually silicon and aluminium in the lithionite ore deposit can enter water insoluble and the aqueous solution after the ore phase reconstruction reaction mutually with the grey stone ore of calcium mutually; In the lithionite ore deposit lithium and other alkali metal after the ore phase reconstruction reaction, enter its salt of the water soluble or the aqueous solution or alkali mutually in.
The Calcium Fluoride (Fluorspan) ore deposit phase that fluorine enters water insoluble and the aqueous solution in the lithionite ore deposit after the ore phase reconstruction reaction.
Operation steps of the present invention is:
Material mixing material: with Li
2O content is that lithionite ore deposit and the ore phase reconstruction auxiliary agent of 3-6% is 1 by mass ratio: (0.7～1.2) batching mixes; The ore phase reconstruction auxiliary agent is the mixture of ore phase reconstruction agent and flux.
The ore phase reconstruction agent is for generating the ore phase reconstruction composition (as CaO, SrO, BaO and Na
2O etc.) alkaline earth metal compound and sodium compound, wherein the compound of alkali earth metal comprises a kind of in the muriate, vitriol, carbonate, oxyhydroxide of calcium, strontium, barium or two or more mixture, and the compound of alkali metal comprises a kind of in sodium-chlor, sodium sulfate and the sodium hydroxide or two or more mixture.Material as flux is low melting component promptly is melt into liquid phase in the roasting restructuring procedure a compound, comprises a kind of in alkaline earth metal chloride, an alkali metal salt and the alkali or two or more mixture; Wherein alkaline earth metal chloride is calcium chloride, strontium chloride and bariumchloride, and an alkali metal salt is vitriol, the muriate of potassium, sodium, and alkali is oxyhydroxide.
Make ball: with compacting or group's system method mixture is made the rawore pelletizing, the size of ball or group is decided by the type and the processing power of conversion unit.
High-temperature roasting: above-mentioned rawore pelletizing in 850～950 ℃ of following roasting 10～50min, is finished the ore phase reconstruction of mineral, the ripe ore deposit of output pelletizing.Temperature be controlled at the fusing point of flux above, below the ball softening temperature of ore deposit.
Quenching, ball milling and stripping: the alkali metal salt soln of water or this operation output carries out quenching, wet ball-milling, stripping to ripe ore deposit pelletizing, makes compound dissolutions such as lithium, potassium, sodium, rubidium, caesium enter solution.The stripping temperature is normal temperature～70 ℃.
Handle leach liquor and extract alkali metal compound: adopt ordinary method to handle leach liquor, carry out lithium, potassium, sodium, rubidium, caesium separation and production respective compound.
The present invention preferentially selects for use can congruent melting, aboundresources, cheap calcium, sodium compound; With calcium cpd as the ore phase reconstruction agent, and fluorine fixing material; Sodium compound is as ore phase reconstruction agent and flux.
Calcium cpd is preferentially selected calcium chloride (CaCl for use
2), lime carbonate (CaCO
3) and calcium sulfate (CaSO
4); Sodium compound is preferentially selected sodium sulfate (Na for use
2SO
4), sodium-chlor (NaCl) and sodium hydroxide (NaOH).
The ore phase reconstruction auxiliary agent is the mixture of calcium cpd and sodium compound, CaO/Na
2The O molar ratio is 0.6～1.5.
The present invention has following advantage and positively effect:
(1) the present invention becomes to be grouped into design objective reconstruct mineral and formation with raw ore, reaches the purpose of optimizing process, reduction treating processes energy consumption and cost, high efficiency extraction lithium, potassium, rubidium and caesium etc.Silicon can enter lime feldspar type ore deposit (CaOAl mutually with aluminium in the lithionite after the ore phase reconstruction reaction
2O
32SiO
2, (Ca, Na) O (Al, Si)
2O
32SiO
2) with calcium ash stone ore (CaOSiO mutually
2), the water insoluble and aqueous solution.Fluorine enters Calcium Fluoride (Fluorspan) ore deposit phase, the water insoluble and aqueous solution in the lithionite after the ore phase reconstruction reaction.In the lithionite lithium and other alkali metal element after the ore phase reconstruction reaction, enter its salt (muriate, vitriol) or alkali (oxyhydroxide) mutually in, the water soluble or the aqueous solution.
(2) compound with alkali earth metal is ore phase reconstruction agent or flux, simultaneously can be in treating processes the fixing fluorine in the raw ore, do not need to carry out mineral processing by the defluorinate process, reduced the mica treatment process, shortened treatment scheme; Eliminated simultaneously the influence of the gas phase volatilization of fluorine effectively to environment.
(3) with the low melting component be flux, make it in the lithionite treating processes, become liquid phase with ore phase reconstruction agent congruent melting, react by infiltration and diffusion, the liquid-solid phase of liquid phase the solid hole, fast, fully carry out the ore phase reconstruction process, avoid solid-temperature required height of solid state reaction reconstruct, time length and incomplete shortcoming.
(4) reaction system is limited in by in the liquid phase agglutinating pelletizing, liquid phase when carrying the ore phase reconstruction agent, the compound of lithium, potassium, rubidium and caesium that dissolution process produces, reduce product activity, increase the completeness of restructuring procedure speed and reconstruct.
(5), avoid because the material that the flux fusion produces hardens by mixture being made ball or agglomerating processing; By making ball or agglomerating, the contact between the reactant is tight, helps reaction and carries out; Simultaneously since in treating processes an amount of melt increase the ore deposit pellet strength, prevent the excessive and pelletizing bonding of melt in the infiltration and the capillary force that diffusion produces of solid hole.
In sum, the present invention adopts high temperature ore phase reconstruction method to handle the lithionite ore deposit to separate and extract valuable metal element compounds such as lithium and potassium, rubidium, caesium.The lithionite ore deposit through the material mixing material, make processing steps such as ball, high temperature ore phase reconstruction, shrend ball milling, stripping filtration, compound production, with ore phase reconstruction in the mineral aggregate, fixedly process such as fluorine and alkaline-earth metal chlorination is carried out synchronously; Resulting valuable metal extraction yield height can effectively be realized the economy of valuable metals such as lithium and potassium, rubidium, caesium, efficient stripping and extraction; Lithionite resource utilization height; Treating processes flow process weak point, chemical materials and energy consumption are few.
Description of drawings
Fig. 1 is the high temperature ore phase reconstruction schematic flow sheet that extracts lithium and other alkali metal element from the lithionite ore deposit.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.Providing of these embodiment limits the present invention anything but.
Embodiment 1
Lithionite ore deposit main component and content (%) are: Li
2O 3.6; (K, Na)
2O 8.5; (Rb, Cs)
2O 1.4; Al
2O
322.5; SiO
258.0; F 4.5.
Is mixing in 1.00: 0.28: 0.42 with lithionite ore deposit, calcium chloride, sodium-chlor by mass ratio, manufactures～25mm rawore pelletizing; In 850 ℃ of following roasting 50min, furnace gas is through cooling, collection flue dust and purifying treatment with above-mentioned rawore pelletizing; Roasting after-ripening ore deposit pelletizing aqueous solution quenching, back wet ball-milling goes out lithium, potassium, rubidium and caesium etc. with the aqueous solution in dissolved with flue dust, obtains containing the mixed chloride aqueous solution of lithium, potassium, sodium, rubidium and caesium.In the molten slag silicon, aluminium mainly with (Ca, Na) O (Al, Si)
2O
32SiO
2And CaOSiO
2Exist, fluorine is fixed to CaF
2
The stripping yield (%) of each main component is respectively: Li 91.2; K 93.3; Rb+Cs 87.1;
The fixed rate of fluorine in slag is 92.2%.
Embodiment 2
Lithionite ore deposit main component and content (%) are: Li
2O 4.5; (K, Na)
2O 9.2; (Rb, Cs)
2O 1.6; Al
2O
328.2; SiO
247.0; F 5.2
Is mixing in 1.00: 0.72: 0.48 with lithionite ore deposit, calcium sulfate, sodium sulfate by mass ratio, manufactures～25mm rawore pelletizing; In 950 ℃ of following roasting 30min, furnace gas is through cooling, collection flue dust and purifying treatment with above-mentioned rawore pelletizing; Roasting after-ripening ore deposit pelletizing aqueous solution quenching, back wet ball-milling uses the aqueous solution in 70 ℃ of following stripping lithiums, potassium, rubidium and caesiums etc. with flue dust, obtains containing the mixed sulfate aqueous solution of lithium, potassium, sodium, rubidium and caesium.In the molten slag silicon, aluminium mainly with (Ca, Na) O (Al, Si)
2O
32SiO
2Exist, fluorine is fixed to CaF2.
The stripping yield (%) of each main component is respectively: Li 93.1; K 94.4; Rb+Cs 88.7;
The fixed rate of fluorine in slag is 95.3%.
Embodiment 3
Lithionite ore deposit main component and content (%) are: Li
2O 5.4; (K, Na)
2O 8.1; (Rb, Cs)
2O 1.7; Al
2O
324.6; SiO
250.2; F 6.4
Is mixing in 1.00: 0.55: 0.45 with lithionite ore deposit, lime carbonate, sodium hydroxide by mass ratio, manufactures～25mm rawore pelletizing; In 900 ℃ of following roasting 20min, furnace gas is through cooling, collection flue dust and purifying treatment with above-mentioned rawore pelletizing; Roasting after-ripening ore deposit pelletizing aqueous solution quenching, back wet ball-milling uses the aqueous solution in 50 ℃ of following stripping lithiums, potassium, rubidium and caesiums etc. with flue dust, obtains containing the mixed hydroxides aqueous solution of lithium, potassium, sodium, rubidium and caesium.Silicon, the main aluminium of aluminium are mainly with CaOAl in the molten slag
2O
32SiO
2, (Ca, Na) O (Al, Si)
2O
32SiO
2And CaOSiO
2Exist, fluorine is fixed to CaF
2
The stripping yield (%) of each main component is respectively: Li 92.4; K 93.8; Rb+Cs 85.7;
The fixed rate of fluorine in slag is 93.3%.
Embodiment 4
Lithionite ore deposit main component and content (%) are: Li
2O 5.4; (K, Na)
2O 8.1; (Rb, Cs)
2O 1.7; Al
2O
324.6; SiO
250.2; F 6.4
Is 1.00: 0.40: 0.15 with lithionite ore deposit, calcium chloride, lime carbonate, sodium-chlor, sodium sulfate by mass ratio: mix, manufacture～25mm rawore pelletizing at 0.15: 0.30; In 900 ℃ of following roasting 20min, furnace gas is through cooling, collection flue dust and purifying treatment with above-mentioned rawore pelletizing; Roasting after-ripening ore deposit pelletizing aqueous solution quenching, back wet ball-milling uses the aqueous solution in 60 ℃ of following stripping lithiums, potassium, rubidium and caesiums etc. with flue dust, obtains containing mixed chloride, the sulfate solution of lithium, potassium, sodium, rubidium and caesium.Silicon, the main aluminium of aluminium are mainly with CaOAl in the molten slag
2O
32SiO
2, (Ca, Na) O (Al, Si)
2O
32SiO
2And CaOSiO
2Exist, fluorine is fixed to CaF
2
The stripping yield (%) of each main component is respectively: Li 94.1; K 95.3; Rb+Cs 87.4; The fixed rate of fluorine in slag is 94.1%.
Claims (9)
1. method of extracting lithium and other alkali metal from the lithionite ore deposit may further comprise the steps:
1) material mixing material: lithionite ore deposit and ore phase reconstruction auxiliary agent are mixed; The ore phase reconstruction auxiliary agent is the mixture of ore phase reconstruction agent and flux; Described ore phase reconstruction agent is that lithionite generates the alkali earth metal in the ore phase reconstruction composition set and the compound of alkali metal; Described flux is selected from and is the simplification compound or the mixture of fused state under the ore phase reconstruction temperature of reaction; The add-on of ore phase reconstruction agent is at least ore phase reconstruction reaction aequum takes place, and it is poor to deduct the amount of the corresponding composition that exists in the lithionite ore deposit, to guarantee the generation of reconstruct ore deposit phase;
2) make ball: with compacting or group's system mode with 1) mix material in the step and make the rawore pelletizing;
3) roasting: above-mentioned rawore pellet roasting is carried out the ore phase reconstruction reaction, generate the ripe ore deposit pelletizing that contains valuable constituent compound soluble in water; Temperature be controlled at the fusing point of flux above, below the pelletizing softening temperature of ore deposit;
4) quenching, ball milling and stripping valuable constituent.
2. method according to claim 1 is with Li
2O content is that lithionite ore deposit and the ore phase reconstruction auxiliary agent of 3-6% is 1 by mass ratio: (0.7～1.2) adds batching, mixes.
3. method according to claim 1 and 2, the compound of described alkali earth metal comprises a kind of in the muriate, vitriol, carbonate, oxyhydroxide of calcium, strontium, barium, or two or more mixture, the compound of alkali metal comprises a kind of in sodium-chlor, sodium sulfate and the sodium hydroxide or two kinds or two kinds of mixtures; Material as flux is alkaline earth metal chloride, an alkali metal salt or the alkali that is melt into liquid phase in the roasting restructuring procedure.
4. method according to claim 3, described alkaline earth metal chloride are calcium chloride, strontium chloride and bariumchloride, and described an alkali metal salt is vitriol, the muriate of potassium, sodium, and described alkali is oxyhydroxide; Flux is a kind of in above-mentioned these compounds or two or more mixture.
5. method according to claim 3, ore phase reconstruction agent are calcium cpd and sodium compound, constitute the ore phase reconstruction auxiliary agent thereby flux is sodium compound.
6. method according to claim 5, described calcium cpd are selected in calcium chloride, lime carbonate and the calcium sulfate one or more for use; Sodium compound is selected in sodium sulfate, sodium-chlor and the sodium hydroxide one or more for use.
7. method according to claim 5, ore phase reconstruction auxiliary agent are the mixture of calcium cpd and sodium compound, CaO/Na
2The O molar ratio is 0.6～1.5.
8. according to each described method of claim 1-7, described ore phase reconstruction reaction, generation contains the reconstruct ore deposit phase of valuable constituent compound soluble in water, be meant lithium and other alkali metal in the lithionite ore deposit after the ore phase reconstruction reaction, enter its salt of the water soluble or the aqueous solution or alkali mutually in; And the lime feldspar type ore deposit that silicon and aluminium can enter water insoluble and the aqueous solution in the lithionite ore deposit after the ore phase reconstruction reaction mutually with the grey stone ore of calcium mutually.
9. method according to claim 8, the Calcium Fluoride (Fluorspan) ore deposit phase that fluorine enters water insoluble and the aqueous solution in the lithionite ore deposit after the ore phase reconstruction reaction.
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