CN104591232A - Method for extracting lithium carbonate from Yichun tantalum niobium tailings lithium mica and obtaining by-product - Google Patents
Method for extracting lithium carbonate from Yichun tantalum niobium tailings lithium mica and obtaining by-product Download PDFInfo
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Abstract
The invention discloses a method for extracting lithium carbonate from Yichun tantalum niobium tailings lithium mica and obtaining by-product. The method comprises the following steps in sequence: acid leaching, vacuum defluorinating, preparing calcium fluoride, preparing aluminum rubidium sulfate and aluminum cesiumsulfate, preparing alum,depositing iron and aluminum, decoloring and concentrating, and preparing lithium carbonate. According to the invention, the technological operations of the method for extracting lithium carbonate from Yichun tantalum niobium tailings lithium mica and obtaining by-product are characterized by selecting different separation methods in line with diverse physicochemical properties of different compounds by adopting chemical leaching thermodynamics methods and techniques. The invention obtains useful by-products such as calcium fluoride, aluminum rubidium sulfate, aluminum cesiumsulfate and alum while preparing lithium carbonate, so as to reduce preparation cost of lithium carbonate from lithium mica by a large margin and raise utilization rate of resources. Compared with existing lime sintering process, the high-temperature calcination method of the invention has the beneficial effects of energy conservation and environment protection, mild conditions, stable operations, recyclable sewage, usable waste residues and low cost of production.
Description
Technical field
The invention belongs to basic theoretical knowledge and the applied technical field of the subjects such as chemistry, physics, material, specifically relate to and a kind ofly from the Ta Nb tailings lithionite of Yichuan, extract Quilonum Retard and obtain the method for byproduct.
Background technology
China's Yichuan Ta Nb tailings is the albite granite mineral deposit, tantalum niobium lithium ore deposit of current Fia, one of multi-metallic minerals selecting and purchasing mine resources base belonging to Ye Shi China Nonferrous Metals Industry Corporation, Yichuan Ta Nb tailings contains abundant Rare Metals Materials, as tantalum, niobium, lithium, rubidium, caesium, potassium, sodium etc.Lithionite is the byproduct that Ta Nb tailings flotation obtains, and annual production can reach more than 200,000 tons.Its concentrate is containing Li
2o4.4%; Rb
2o1.3%; Cs
2o0.243%; Be the important industrial raw material carrying lithium, rubidium, caesium, it developed and utilized there is very Important Economic value and strategic importance.
Wherein: lithium and its esters are the base mateirals of lithium electricity new forms of energy, are described as " industrial monosodium glutamate, Energy Star " by scientist, are the preferred materials of producing lithium ion battery, be the important meals of development new forms of energy, novel material.In recent years lithium-ion secondary cell with average annual 20% tempo increase.The novel polymer lithium ion battery that the U.S. succeeds in developing recently has little, the safe and reliable feature of volume, and its price is only 1/5 of existing lithium ion battery, will be used for electromobile.
The photoelectric properties of rubidium and caesium uniqueness are used as manufacturing the photoelectric cathode materials that phototube and optical telecommunications increase battalion, are widely used in photoelectric instrument and electron rays instrument, for the production of aspects such as the automatic control of process, radar and telegraphic facsimile technology, laser technologies.The oscillation frequency of caesium radiating capacity has long stability, can be used as the standard of frequency and time.Cesium-beam atomic clock has been widely used in communication, transport, military affairs and aerospace.The photoelectric properties of caesium are used for sighting at night mirror, night vision equipment etc.Studying them at magnetohydrodynamic generator at present, the application in the energy transformation that thermoelectric converter and ion rocket propelling engine etc. are new.
Alum, also known as potassium aluminium alum, arcanite and potassium alum, the potassium sulfate of oil-containing crystal water and Tai-Ace S 150 double salt.Chemical formula KAl (SO
4)
212H
2o, molecular weight 474.31.Colourless octahedral crystal.There is acerbity, density 1.75, fusing point 92 DEG C.Water-soluble hydrolytic action and generate aluminium hydroxide glue precipitation.Alum is mainly used in printing, papermaking, process hides, paint, pharmacy and foodstuffs industry at present in China market, be also used as dye cloth mordant, the stiffening agent of film, fire-fighting foams agent, the catalyzer of synthetic ammonia, sugaring and water clarification agent and ore dressing precipitation agent.Effect of medicinal alum: removing toxic substances desinsection, eliminating dampness are antipruritic, the effect of stop blooding antidiarrheal, heat-clearing dissolving phlegm.
The chemical property of fluorine is the most active, can directly and other non-metallic element core metallic element chemical combination, for the manufacture of macromolecular materials such as various fluorochemical, fluoro-containing plastic and fluorine-containing rubber, fluorine carbon superpolymer.When carrying the metals such as lithium, caesium, rubidium from lepidolite raw material, first to remove the fluorine element in lithionite.Traditional method is removed fluorine and is generally adopted lime sinter process, high temperature roast method, and temperature removes fluorine at about 1000 DEG C.At high temperature except fluorine, not only energy consumption is high, and easily causes some loss of elements, loses and adopts lithionite to be economic worth and the comprehensive development and utilization rate that raw material extracts lithium and byproduct.
The present invention utilizes Yichuan Ta Nb tailings lithionite to prepare in the novel method technique of Quilonum Retard and byproduct thereof, to the difference of different compound physico-chemical property, select different separation methods, while preparing Quilonum Retard, also can obtain aluminum rubidium sulfate, aluminium cesium sulfate, potassium aluminium sulfate, Calcium Fluoride (Fluorspan) and the compound such as calcium sulfate and silica sand, considerably reduce production cost, improve lithionite comprehensive development and utilization rate.
The present invention extracts Quilonum Retard and obtains in the method for byproduct from the Ta Nb tailings lithionite of Yichuan, adopt chemical industry lixiviate thermodynamics method and technology, to the difference of different compound physico-chemical property, select different separation methods, method of the present invention not only significantly improves purity and the yield of battery-level lithium carbonate, but also obtains the useful byproduct such as aluminum rubidium sulfate, aluminium cesium sulfate, potassium aluminium sulfate, Calcium Fluoride (Fluorspan).
Summary of the invention
Technical scheme of the present invention is as follows:
A kind ofly from the Ta Nb tailings lithionite of Yichuan, extract Quilonum Retard and obtain the method for byproduct, it is characterized in that, comprise step successively: acidolysis lixiviate → vacuum concentrate → prepares Quilonum Retard except fluorine → prepare Calcium Fluoride (Fluorspan) → prepare aluminum rubidium sulfate and aluminium cesium sulfate → prepare alum → precipitated iron aluminium → decolouring; Be specially:
Acidolysis lixiviate: by the lithionite do not pulverized directly and concentration be that the ratio of sulphuric acid soln 1:2.5 ~ 6 in mass ratio of 25wt% ~ 60wt% is put in reaction unit;
Vacuum is except fluorine: temperature 60 ~ 220 DEG C, pressure is 0.5 × 10
5pa ~ 1.50 × 10
5under pa condition, vacuum was except fluorine reaction 5 ~ 8 hours, isolated fluorine-containing solution, must contain Li
+vitriol mixing solutions;
Prepare Calcium Fluoride (Fluorspan): in isolated fluorine-containing solution, add calcium hydroxide or pH value is adjusted to 8 ~ 9 by calcium oxide, obtain neutralization reaction mixture, filtering separation, dry filter residue, finally obtained Calcium Fluoride (Fluorspan) sample;
Prepare aluminum rubidium sulfate and aluminium cesium sulfate: will containing Li
+vitriol mixing solutions filtered while hot be separated, filter residue water fully washs, and removing filter residue, to obtain filtrate be mother liquor 1; Then by mother liquor 1 under agitation slow cooling to 40 DEG C ~ 60 DEG C, cooling crystallize out aluminum rubidium sulfate and aluminium cesium sulfate, filtering separation, washing filter residue, filtrate is recovered as mother liquor 2;
Prepare alum: be under agitation cooled by mother liquor 2 to 5 DEG C ~ 30 DEG C, control Al in solution
3+, K
+ionic concn is in saturated or hypersaturated state, and crystallization generates potassium aluminium alum compound precipitation, and filtering separation obtains crystal alum, and filtrate is recovered as mother liquor 3;
Precipitated iron aluminium: be under agitation, is adjusted to 2.81 ~ 8.35 by the pH value of mother liquor 3, then adds a small amount of hydrogen peroxide, Fe
2+be oxidized to Fe
3+, make it be converted into precipitation of hydroxide; Filtering separation, removes filter residue, and reclaiming filtrate is mother liquor 4;
Decolouring is concentrated: mother liquor 4 is under agitation heated to 70 DEG C ~ 90 DEG C, adds a small amount of gac, the silicon-dioxide (SiO of the pigment in adsorbent solution and mucilage binding
2nH
2o), decolour complete, concentrating under reduced pressure to terminal time, control Li in solution
+concentration at 20g/L ~ 40g/L, cross filter impurity, filtrate is mother liquor 5;
Prepare Quilonum Retard: mother liquor 5 is under agitation heated to 96 DEG C ~ 100 DEG C, pass into carbonic acid gas sinker reaction 60 ~ 100 minutes with 2 normal atmosphere, generate white precipitate; React complete, filtration or the white precipitate described in centrifugation, after reusable heat water repetitive scrubbing, dry and obtain Quilonum Retard under 110 DEG C of conditions.
In production process of the present invention, the chemical equation related to is as follows:
Li
2O+H
2SO
4＝Li
2SO
4+H
2O
K
2O+H
2SO
4＝K
2SO
4+H
2O
Na
2O+H
2SO
4＝Na
2SO
4+H
2O
A
2O
3+3H
2SO
4＝Al
2(SO
4)
3+3H
2O
Fe
2O
3+3H
2SO
4＝Fe
2(SO
4)
3+3H
2O
Rb
2O+H
2SO
4＝Rb
2SO
4+H
2O
Cs
2O+H
2SO
4＝Cs
2SO
4+H
2O
2HF+Ca(OH)
2＝CaF
2↓+2H
2O
Rb
2SO
4+Al
2(SO
4)
3＝2RbAl(SO
4)
2
Cs
2SO
4+Al
2(SO
4)
3＝2CsAl(SO
4)
2
K
2SO
4+Al
2(SO
4)
3＝2KAl(SO
4)
2
Fe
2(SO
4)
3+3H
2O
2＝2Fe(OH)
3+3SO
2↑+3O
2↑
Al
2(SO
4)
3+3H
2O
2＝2Al(OH)
3+3SO
2↑+3O
2↑
Li
2SO
4+Ca(OH)
2＝2LiOH+CaSO
4↓
2LiOH+CO
2＝Li
2CO
3+H
2O
Technical scheme of the present invention is achieved like this, utilize in the Ta Nb tailings lithionite of Yichuan and extract Quilonum Retard and obtain in the method technological operation of byproduct, it is characterized in that adopting chemical industry lixiviate thermodynamics method and technology, to the difference of different compound physico-chemical property, select different separation methods.While preparing Quilonum Retard, also can obtain the byproduct that Calcium Fluoride (Fluorspan), aluminum rubidium sulfate, aluminium cesium sulfate rubidium and alum etc. are useful, considerably reduce the production cost utilizing lithionite to prepare Quilonum Retard, improve resource utilization.
The present invention adopts chemical industry lixiviate thermodynamics method and utilisation technology, utilize Feld Spar in Yichun Guimaraesite Mine lithionite to prepare Quilonum Retard and reclaim the method for its byproduct, more existing lime sinter process, high-temperature roasting method has energy-conserving and environment-protective, mild condition, stable operation, waste water are recyclable, the effect that waste residue can utilize, production cost is low.
Embodiment
Explain below in conjunction with embodiment and of the present inventionly a kind ofly from the Ta Nb tailings lithionite of Yichuan, extract Quilonum Retard and obtain the method for byproduct.
The concentration related in embodiment is mass concentration.Be now solvent with dilute sulphuric acid, lithionite is that the technological process that raw material prepares Quilonum Retard and byproduct thereof illustrates the novel method utilizing Yichuan Ta Nb tailings lithionite to prepare Quilonum Retard and byproduct thereof.
The present embodiment selects lithionite to adopt Yichuan Ta Nb tailings lithionite.Its physico-chemical property is: appearance white; Vitreous luster or pearliness; Flakey, relative density is 2.8-2.9.In lithium cloud, the main component of chemical constitution is as follows:
| Li 2O | K 2O | Na 2O | Al 2O 3 | Si 2O | Fe 2O 3 | Rb 2O | Cs 2O | F |
| 4.1％ | 8.2％ | 0.9％ | 23.2％ | 53.7 | 0.2％ | 1.3^ | 0.24％ | 4.1％ |
Embodiment 1
Present invention process step is as follows: a kind ofly from the Ta Nb tailings lithionite of Yichuan, extract Quilonum Retard and obtain the method for byproduct, comprises step successively: acidolysis lixiviate → vacuum concentrate → prepares Quilonum Retard except fluorine → prepare Calcium Fluoride (Fluorspan) → prepare aluminum rubidium sulfate and aluminium cesium sulfate → prepare alum → precipitated iron aluminium → decolouring; Be specially:
Acidolysis lixiviate: by the lithionite do not pulverized directly and concentration be that the ratio of sulphuric acid soln 1:2.5 ~ 6 in mass ratio of 25wt% ~ 60wt% is put in reaction unit;
Vacuum is except fluorine: temperature 60 ~ 220 DEG C, pressure is 0.5 × 10
5pa ~ 1.50 × 10
5under pa condition, vacuum was except fluorine reaction 5 ~ 8 hours, isolated fluorine-containing solution, must contain Li
+vitriol mixing solutions;
Prepare Calcium Fluoride (Fluorspan): in isolated fluorine-containing solution, add calcium hydroxide or pH value is adjusted to 8 ~ 9 by calcium oxide, obtain neutralization reaction mixture, filtering separation, dry filter residue, finally obtained Calcium Fluoride (Fluorspan) sample;
Prepare aluminum rubidium sulfate and aluminium cesium sulfate: will containing Li
+vitriol mixing solutions filtered while hot be separated, filter residue water fully washs, and removing filter residue, to obtain filtrate be mother liquor 1; Then by mother liquor 1 under agitation slow cooling to 40 DEG C ~ 60 DEG C, cooling crystallize out aluminum rubidium sulfate and aluminium cesium sulfate, filtering separation, washing filter residue, filtrate is recovered as mother liquor 2;
Prepare alum: be under agitation cooled by mother liquor 2 to 5 DEG C ~ 30 DEG C, control Al in solution
3+, K
+ionic concn is in saturated or hypersaturated state, and crystallization generates potassium aluminium alum compound precipitation, and filtering separation obtains crystal alum, and filtrate is recovered as mother liquor 3;
Precipitated iron aluminium: be under agitation, is adjusted to 2.81 ~ 8.35 by the pH value of mother liquor 3, then adds a small amount of hydrogen peroxide, Fe
2+be oxidized to Fe
3+, make it be converted into precipitation of hydroxide; Filtering separation, removes filter residue, and reclaiming filtrate is mother liquor 4;
Decolouring is concentrated: mother liquor 4 is under agitation heated to 70 DEG C ~ 90 DEG C, adds a small amount of gac, the silicon-dioxide (SiO of the pigment in adsorbent solution and mucilage binding
2nH
2o), decolour complete, concentrating under reduced pressure to terminal time, control Li in solution
+concentration at 20g/L ~ 40g/L, cross filter impurity, filtrate is mother liquor 5;
Prepare Quilonum Retard: mother liquor 5 is under agitation heated to 96 DEG C ~ 100 DEG C, pass into carbonic acid gas sinker reaction 60 ~ 100 minutes with 2 normal atmosphere, generate white precipitate; React complete, filtration or the white precipitate described in centrifugation, after reusable heat water repetitive scrubbing, dry and obtain Quilonum Retard under 110 DEG C of conditions.
Embodiment 2
The lithionite do not pulverized is taken 200 grams directly and concentration be that the sulphuric acid soln of 45wt% is in quality 1:5 ratio input reaction unit; Temperature be 110 DEG C carry out acidolysis except fluorine react 6 time; React complete, be separated removing hydrofluoric acid, discharging filtered while hot, obtaining filtrate is mother liquor 1; In hydrofluoric acid, add calcium hydroxide or calcium oxide, filter residue water fully washs slagging-off, generates byproduct Calcium Fluoride (Fluorspan); Cooled by mother liquor 1 to 60 DEG C of precipitations, filtering separation obtains aluminum rubidium sulfate and aluminium cesium sulfate, and filtrate is mother liquor 2; Cooling mother liquor 2 to 20 DEG C, filtering separation obtains alum, and filtrate is mother liquor 3; Then by the pH value of mother liquor 3 modulation 3.5, H is used
2o
2fe
2+chlorination becomes Fe
3+, make it change into precipitation of hydroxide, filtering separation, remove filter residue, reclaiming filtrate, is mother liquor 4; Mother liquor 4 is decoloured after concentrating and obtain mother liquor 5; Then mother liquor 5 is heated to 98 DEG C and passes into carbonic acid gas sinker reaction 60-100 minute in 2 normal atmosphere, generate white precipitate.React complete, then filtration or centrifugal, obtains lithium carbonate product.
Embodiment 3
The lithionite do not pulverized is taken 200 grams directly and concentration be that the sulphuric acid soln of 35wt% is in quality 1:3 ratio input reaction unit; Temperature be 110 DEG C carry out acidolysis except fluorine react 6 time; React complete, be separated removing hydrofluoric acid, discharging filtered while hot, obtaining filtrate is mother liquor 1; In hydrofluoric acid, add calcium hydroxide or calcium oxide, filter residue water fully washs slagging-off, generates byproduct Calcium Fluoride (Fluorspan); Cooled by mother liquor 1 to 50 DEG C of precipitations, filtering separation obtains aluminum rubidium sulfate and aluminium cesium sulfate, and filtrate is mother liquor 2; Cooling mother liquor 2 to 5 DEG C, filtering separation obtains alum, and filtrate is mother liquor 3; Then by the pH value of mother liquor 3 modulation 5, H is used
2o
2fe
2+chlorination becomes Fe
3+, make it change into precipitation of hydroxide, filtering separation, remove filter residue, reclaiming filtrate, is mother liquor 4; Mother liquor 4 is decoloured after concentrating and obtain mother liquor 5; Then mother liquor 5 is heated to 98 DEG C and passes into carbonic acid gas sinker reaction 60-100 minute in 2 normal atmosphere, generate white precipitate.React complete, then filtration or centrifugal, obtains lithium carbonate product.
Embodiment 4
Take Yichuan Ta Nb tailings through 2 flotation containing Li
2o is the lithionite 200 grams 3 parts of 4.4%, through 20.4 grams, 20 grams, the finally prepd Quilonum Retard sample of present invention process step and 21.3 grams 3 parts, detect through national authority department, the purity of the key technical indexes Quilonum Retard is respectively 99.59%, 99.63%, and yield is respectively 81.6%, 80.0% and 84%; The crystallized sample 68.2 grams of 12 potassium aluminium sulfates prepared, 65.4 grams and 66.9 grams 3 parts, check through complexometry, the purity of 12 potassium aluminium sulfates is respectively 96%, 96.9% and 96.4%, and their productive rate is 88.32%, 84.69% and 86.64% respectively; The aluminum rubidium sulfate prepared 8.27 grams, 8.31 grams and 8.35 grams, their productive rate is 98%, 98.5% and 99% respectively; The aluminium cesium sulfate prepared 0.93 gram, 0.94 gram and 0.95 gram, their productive rate is 96%, 97% and 98% respectively.
The present invention utilizes in the Ta Nb tailings lithionite of Yichuan and extracts Quilonum Retard and obtain in the method technological operation of byproduct, it is characterized in that adopting chemical industry lixiviate thermodynamics method and technology, to the difference of different compound physico-chemical property, selects different separation methods.While preparing Quilonum Retard, also can obtain the byproduct that Calcium Fluoride (Fluorspan), aluminum rubidium sulfate, aluminium cesium sulfate rubidium and alum etc. are useful, considerably reduce the production cost utilizing lithionite to prepare Quilonum Retard, improve resource utilization, more existing lime sinter process, high-temperature roasting method has energy-conserving and environment-protective, mild condition, and stable operation, waste water are recyclable, the effect that waste residue can utilize, production cost is low.
Claims (9)
1. one kind is extracted Quilonum Retard and obtains the method for byproduct from the Ta Nb tailings lithionite of Yichuan, it is characterized in that, comprise step successively: acidolysis lixiviate → vacuum concentrate → prepares Quilonum Retard except fluorine → prepare Calcium Fluoride (Fluorspan) → prepare aluminum rubidium sulfate and aluminium cesium sulfate → prepare alum → precipitated iron aluminium → decolouring.
2. method according to claim 1, is characterized in that, described acidolysis lixiviate is specially: by the lithionite do not pulverized directly and concentration be that the ratio of sulphuric acid soln 1:2.5 ~ 6 in mass ratio of 25wt% ~ 60wt% is put in reaction unit.
3. method according to claim 1, is characterized in that, described vacuum is removed fluorine and is specially: temperature 60 ~ 220 DEG C, pressure is 0.5 × 10
5pa ~ 1.50 × 10
5under pa condition, vacuum was except fluorine reaction 5 ~ 8 hours, isolated fluorine-containing solution, must contain Li
+vitriol mixing solutions.
4. method according to claim 3, is characterized in that, described Calcium Fluoride (Fluorspan) of preparing is specially: in isolated fluorine-containing solution, add calcium hydroxide or pH value is adjusted to 8 ~ 9 by calcium oxide, obtain neutralization reaction mixture, filtering separation, dries filter residue, finally obtained Calcium Fluoride (Fluorspan) sample.
5. method according to claim 3, is characterized in that, described prepares aluminum rubidium sulfate and aluminium cesium sulfate is specially: will containing Li
+vitriol mixing solutions filtered while hot be separated, filter residue water fully washs, and removing filter residue, to obtain filtrate be mother liquor 1; Then by mother liquor 1 under agitation slow cooling to 40 DEG C ~ 60 DEG C, cooling crystallize out aluminum rubidium sulfate and aluminium cesium sulfate, filtering separation, washing filter residue, filtrate is recovered as mother liquor 2.
6. method according to claim 5, is characterized in that, described alum of preparing is specially: under agitation cooled by mother liquor 2 to 5 DEG C ~ 30 DEG C, controls Al in solution
3+, K
+ionic concn is in saturated or hypersaturated state, and crystallization generates potassium aluminium alum compound precipitation, and filtering separation obtains crystal alum, and filtrate is recovered as mother liquor 3.
7. method according to claim 6, is characterized in that, described precipitated iron aluminium is specially: under agitation, and the pH value of mother liquor 3 is adjusted to 2.81 ~ 8.35, then adds a small amount of hydrogen peroxide, Fe
2+be oxidized to Fe
3+, make it be converted into precipitation of hydroxide; Filtering separation, removes filter residue, and reclaiming filtrate is mother liquor 4.
8. method according to claim 7, is characterized in that, described decolouring is concentrated to be specially: mother liquor 4 is under agitation heated to 70 DEG C ~ 90 DEG C, add a small amount of gac, the pigment in adsorbent solution and the silicon-dioxide of mucilage binding, decolour complete, concentrating under reduced pressure to terminal time, control Li in solution
+concentration at 20g/L ~ 40g/L, cross filter impurity, filtrate is mother liquor 5.
9. method according to claim 8, is characterized in that, described Quilonum Retard of preparing is specially: mother liquor 5 is under agitation heated to 96 DEG C ~ 100 DEG C, passes into carbonic acid gas sinker reaction 60 ~ 100 minutes, generate white precipitate with 2 normal atmosphere; React complete, filtration or the white precipitate described in centrifugation, after reusable heat water repetitive scrubbing, dry and obtain Quilonum Retard under 110 DEG C of conditions.
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| CN105366701B (en) * | 2015-11-06 | 2019-10-01 | 化工部长沙设计研究院 | A kind of technique of continuous production cesium rubidium alum and potassium alum |
| CN110526265A (en) * | 2019-10-10 | 2019-12-03 | 宜春市科远化工有限公司 | A kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite |
| CN114634355A (en) * | 2022-03-11 | 2022-06-17 | 苏州大学 | Treatment method for recycling ferrous lepidolite leaching residues |
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Application publication date: 20150506 |