CN102923742A - Method for comprehensively extracting aluminum and lithium from coal ash - Google Patents
Method for comprehensively extracting aluminum and lithium from coal ash Download PDFInfo
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Abstract
The invention provides a method for comprehensively extracting aluminum and lithium from coal ash. The method is characterized by comprising the following technological steps which are carried out in sequence: (A) desiliconizing and magnetically separating; (B) roasting; (C) primary dipping by alkali; (D) secondary dipping by alkali; (E) carbonizing, and precipitating aluminum; (F) purifying lithium mother liquor; and (G) evaporating, concentrating and precipitating lithium. The method has the advantages that silicon, iron, aluminum and lithium are sequentially extracted from the industrial coal ash, so that the waste is turned into treasure, the cost of the raw materials is reduced, the technological operation is simple and convenient, and the comprehensive extracting rate of aluminum lithium resources can be maximized; and the method is an ideal method for comprehensively extracting aluminum and lithium from the coal ash.
Description
Technical field
The present invention relates to a kind of method of from flyash, comprehensively extracting aluminium and lithium.
Background technology
At present, bauxite resource production both domestic and external is mainly derived from the smelting of bauxite; In China; because a large amount of productions of aluminum oxide cause the sharply shortage of high-quality, higher-grade bauxite resource; along with increasingly stringent and the bauxite resource shortage crisis aggravation of national environmental protection policy, from high alumina coal gangue, aluminous fly-ash and high waste slag of aluminum, extract the major subjects that bauxite resource becomes numerous Chinese scholars researchs for the moment.And the processing method of extracting aluminum oxide or aluminium hydroxide or aluminium salt from flyash mainly contains alkaline process sintering and pickling process two classes, and wherein, the alkaline process sintered coal ash therefrom extracts the processing method of aluminium, mainly contains calcium salt sintering adjuvant method and sodium salt sintering adjuvant method two large classes.At present, extract lithium and lithium salts method thereof both at home and abroad and mainly be from the liquid mineral such as the solid mineral such as granite pegmatite lithium deposite and salt lake brine lithium deposite, seawater lithium deposite and extract, also not about from flyash, extracting the report of lithium.
In addition, at home and abroad there is no at present comprehensive correlation technique research of extracting aluminium and lithium from flyash, although it is existing a lot of to extract the technique of aluminium from flyash, want the comprehensive extraction rate reached of aluminium in the flyash and lithium resource is arrived maximum, but still be in the exploratory stage.
Summary of the invention
The objective of the invention is: a kind of method of comprehensively extracting aluminium and lithium from flyash is provided, the method can effectively utilize industrial waste flyash to extract aluminium and lithium, reduced raw materials cost, technological operation is easy, and can make the comprehensive extraction rate reached of aluminium and lithium resource arrive maximum.
Purpose of the present invention can realize by following technical proposals:
This is the comprehensive method of extracting aluminium and lithium from flyash, it is characterized in that comprising in sequence following processing step:
(A) desiliconization, magnetic separation: after the flyash desiliconization, grind, cross 200 mesh sieves, then iron removal by magnetic separation;
(B) roasting: the flyash after the step of learning from else's experience (A) desiliconization, the magnetic separation and agglutinant are that the ratio of 1:0.5～1:3 is mixed, stirred according to mass ratio, place nickel crucible, then use retort furnace under 650～950 ℃ of temperature, add thermal bake-out 30～90min, carry out afterwards grog from efflorescence;
(C) alkali soaks: the grog that step (B) is roasting imports in the Erlenmeyer flask, and to add massfraction according to liquid and solid volume than the ratio for 1:10～1:300 be 10%～30% sodium carbonate solution, then place on the hot plate under 90～200 ℃ of temperature, heating 30～120min, finish once leaching, filter, obtain leached mud and leach liquor I;
(D) secondary alkali soaks: be 10%～30% sodium carbonate solution again with massfraction with the leached mud of step (C) gained, wash in the Erlenmeyer flask for the ratio of 1:10～1:300 according to liquid and solid volume ratio, then place on the hot plate under 90～200 ℃ of temperature, heating 30～60min, finish the secondary leaching, again filter, obtain the leach liquor II, the leach liquor II is mixed with the leach liquor I of step (C) gained, be and contain aluminium, lithium solution;
(E) the heavy aluminium of carbonization: contain aluminium with what step (D) obtained, lithium solution carries out carbonating to be processed, in solution, pass into carbon dioxide, the starting temperature of solution is 60-80 ℃ during the control ventilation, final temperature is 40 ℃, the carbonic acid gas draft speed is 2.5-3.5L/min, when the pH=7-9 of solution, stop ventilation, obtain impure aluminum hydroxide precipitation, then be that 40% sodium hydroxide solution dissolves with formed impure aluminum hydroxide precipitation massfraction, the carbonating of again carrying out under above-mentioned the same terms is processed, obtain pure aluminium hydroxide, pure aluminium hydroxide is through washing, bake and further obtain the aluminium product;
(F) purify the lithium mother liquor: after step (E) operation is finished, obtain simultaneously containing the lithium mother liquor, to contain the lithium mother liquor and under 50～100 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor stirred and be cooled to room temperature, filter, subsequently filtrate is carried out-5～5 ℃ of deepfreezes, separate out a large amount of crystal, this crystal can be used as the agglutinant of step (B);
(G) evaporation concentration sinker: the operation of above-mentioned steps (F) is carried out repeatedly, until after the concentration of Lithium Oxide 98min reaches 40-54g/L in the solution, with concentrated solution evaporate to dryness or the precipitation lithium of resulting lithium, thereby obtain the lithium solid phase prod.
The present invention is in step (B), and described agglutinant is yellow soda ash, perhaps the mixture of unslaked lime and yellow soda ash, the perhaps mixture of Wingdale and yellow soda ash.
The present invention carries out grog and from the operating process of efflorescence is in step (B): after naturally being cooled to 450～750 ℃, constant temperature keeps 20min to finish from efflorescence.
The present invention is in step (B), and the mass ratio of flyash and agglutinant is 1:0.5, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 950 ℃, and the heating roasting time is 60min, grog from the operating process of efflorescence is: naturally be cooled to 750 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 90 ℃, and be 120min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 90 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
The present invention is in step (B), and the mass ratio of flyash and agglutinant is 1:1.5, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 850 ℃, and the heating roasting time is 90min, grog from the operating process of efflorescence is: naturally be cooled to 650 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 150 ℃, and be 90min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 150 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
The present invention is in step (B), and the mass ratio of flyash and agglutinant is 1:3, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 650 ℃, and the heating roasting time is 90min, grog from the operating process of efflorescence is: naturally be cooled to 450 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 200 ℃, and be 120min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 200 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
Advantage of the present invention is: the method takes full advantage of industrial waste flyash and extracts successively silicon-iron-aluminium-lithium, turn waste into wealth, reduced raw materials cost, technological operation is easy, and can make the comprehensive extraction rate reached of aluminium and lithium resource to maximum, be a kind of desirable comprehensive method of extracting aluminium and lithium from flyash.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
As shown in Figure 1, this is the comprehensive method of extracting aluminium and lithium from flyash, it is characterized in that comprising in sequence following processing step:
(A) desiliconization, magnetic separation: after the flyash desiliconization, grind, cross 200 mesh sieves, then iron removal by magnetic separation;
(B) roasting: the flyash after the step of learning from else's experience (A) desiliconization, the magnetic separation and agglutinant are that the ratio of 1:0.5～1:3 is mixed, stirred according to mass ratio, place nickel crucible, then use retort furnace under 650～950 ℃ of temperature, add thermal bake-out 30～90min, carry out afterwards grog from efflorescence;
(C) alkali soaks: the grog that step (B) is roasting imports in the Erlenmeyer flask, and to add massfraction according to liquid and solid volume than the ratio for 1:10～1:300 be 10%～30% sodium carbonate solution, then place on the hot plate under 90～200 ℃ of temperature, heating 30～120min, finish once leaching, filter, obtain leached mud and leach liquor I;
(D) secondary alkali soaks: be 10%～30% sodium carbonate solution again with massfraction with the leached mud of step (C) gained, wash in the Erlenmeyer flask for the ratio of 1:10～1:300 according to liquid and solid volume ratio, then place on the hot plate under 90～200 ℃ of temperature, heating 30～60min, finish the secondary leaching, again filter, obtain the leach liquor II, the leach liquor II is mixed with the leach liquor I of step (C) gained, be and contain aluminium, lithium solution;
(E) the heavy aluminium of carbonization: contain aluminium with what step (D) obtained, lithium solution carries out carbonating to be processed, in solution, pass into carbon dioxide, the starting temperature of solution is 60-80 ℃ during the control ventilation, final temperature is 40 ℃, the carbonic acid gas draft speed is 2.5-3.5L/min, when the pH=7-9 of solution, stop ventilation, obtain impure aluminum hydroxide precipitation, then be that 40% sodium hydroxide solution dissolves with formed impure aluminum hydroxide precipitation massfraction, the carbonating of again carrying out under above-mentioned the same terms is processed, obtain pure aluminium hydroxide, pure aluminium hydroxide is through washing, bake and further obtain the aluminium product;
(F) purify the lithium mother liquor: after step (E) operation is finished, obtain simultaneously containing the lithium mother liquor, to contain the lithium mother liquor and under 50～100 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor stirred and be cooled to room temperature, filter, subsequently filtrate is carried out-5～5 ℃ of deepfreezes, separate out a large amount of crystal, this crystal can be used as the agglutinant of step (B);
(G) evaporation concentration sinker: the operation of above-mentioned steps (F) is carried out repeatedly, until after the concentration of Lithium Oxide 98min reaches 40-54g/L in the solution, with concentrated solution evaporate to dryness or the precipitation lithium of resulting lithium, thereby obtain the lithium solid phase prod.
In step (B), described agglutinant is yellow soda ash, perhaps the mixture of unslaked lime and yellow soda ash, the perhaps mixture of Wingdale and yellow soda ash.
In step (B), carry out grog and from the operating process of efflorescence be: after naturally being cooled to 450～750 ℃, constant temperature keeps 20min to finish from efflorescence.
The below is several embodiment of material content of the present invention and operational condition:
Embodiment 1:
In step (B), the mass ratio of flyash and agglutinant is 1:0.5, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 950 ℃, and the heating roasting time is 60min, grog from the operating process of efflorescence is: naturally be cooled to 750 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 90 ℃, and be 120min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 90 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
After adopting embodiment 1, the result measures: the leaching rate of aluminium and lithium all reaches more than 90%, soaks removal of impurities, step (E) carbonization by step (C) and twice alkali of step (D) and sinks behind the aluminium, and about 80% of lithium total amount still exists in solution.
Embodiment 2:
In step (B), the mass ratio of flyash and agglutinant is 1:1.5, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 850 ℃, and the heating roasting time is 90min, grog from the operating process of efflorescence is: naturally be cooled to 650 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 150 ℃, and be 90min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 150 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
After adopting embodiment 2, the result measures: the leaching rate of aluminium and lithium all reaches more than 85%, soaks removal of impurities, step (E) carbonization by step (C) and twice alkali of step (D) and sinks behind the aluminium, and about 80% of lithium total amount still exists in solution.
Embodiment 3:
In step (B), the mass ratio of flyash and agglutinant is 1:3, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 650 ℃, and the heating roasting time is 90min, grog from the operating process of efflorescence is: naturally be cooled to 450 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 200 ℃, and be 120min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 200 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
After adopting embodiment 3, the result measures: the leaching rate of aluminium and lithium all reaches about 50%.
Claims (6)
1. comprehensive method of extracting aluminium and lithium from flyash is characterized in that comprising in sequence following processing step:
(A) desiliconization, magnetic separation: after the flyash desiliconization, grind, cross 200 mesh sieves, then iron removal by magnetic separation;
(B) roasting: the flyash after the step of learning from else's experience (A) desiliconization, the magnetic separation and agglutinant are that the ratio of 1:0.5～1:3 is mixed, stirred according to mass ratio, place nickel crucible, then use retort furnace under 650～950 ℃ of temperature, add thermal bake-out 30～90min, carry out afterwards grog from efflorescence;
(C) alkali soaks: the grog that step (B) is roasting imports in the Erlenmeyer flask, and to add massfraction according to liquid and solid volume than the ratio for 1:10～1:300 be 10%～30% sodium carbonate solution, then place on the hot plate under 90～200 ℃ of temperature, heating 30～120min, finish once leaching, filter, obtain leached mud and leach liquor I;
(D) secondary alkali soaks: be 10%～30% sodium carbonate solution again with massfraction with the leached mud of step (C) gained, wash in the Erlenmeyer flask for the ratio of 1:10～1:300 according to liquid and solid volume ratio, then place on the hot plate under 90～200 ℃ of temperature, heating 30～60min, finish the secondary leaching, again filter, obtain the leach liquor II, the leach liquor II is mixed with the leach liquor I of step (C) gained, be and contain aluminium, lithium solution;
(E) the heavy aluminium of carbonization: contain aluminium with what step (D) obtained, lithium solution carries out carbonating to be processed, in solution, pass into carbon dioxide, the starting temperature of solution is 60-80 ℃ during the control ventilation, final temperature is 40 ℃, the carbonic acid gas draft speed is 2.5-3.5L/min, when the pH=7-9 of solution, stop ventilation, obtain impure aluminum hydroxide precipitation, then be that 40% sodium hydroxide solution dissolves with formed impure aluminum hydroxide precipitation massfraction, the carbonating of again carrying out under above-mentioned the same terms is processed, obtain pure aluminium hydroxide, pure aluminium hydroxide is through washing, bake and further obtain the aluminium product;
(F) purify the lithium mother liquor: after step (E) operation is finished, obtain simultaneously containing the lithium mother liquor, to contain the lithium mother liquor and under 50～100 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor stirred and be cooled to room temperature, filter, subsequently filtrate is carried out-5～5 ℃ of deepfreezes, separate out a large amount of crystal, this crystal can be used as the agglutinant of step (B);
(G) evaporation concentration sinker: the operation of above-mentioned steps (F) is carried out repeatedly, until after the concentration of Lithium Oxide 98min reaches 40-54g/L in the solution, with concentrated solution evaporate to dryness or the precipitation lithium of resulting lithium, thereby obtain the lithium solid phase prod.
According to claim 1 a kind of from flyash the comprehensive method of extracting aluminium and lithium, it is characterized in that: in step (B), described agglutinant is yellow soda ash, perhaps the mixture of unslaked lime and yellow soda ash, the perhaps mixture of Wingdale and yellow soda ash.
According to claim 1 and 2 a kind of from flyash the comprehensive method of extracting aluminium and lithium, it is characterized in that: in step (B), carrying out grog from the operating process of efflorescence is: after naturally being cooled to 450～750 ℃, constant temperature keeps 20min to finish from efflorescence.
According to claim 3 a kind of from flyash the comprehensive method of extracting aluminium and lithium, it is characterized in that: in step (B), the mass ratio of flyash and agglutinant is 1:0.5, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 950 ℃, and the heating roasting time is 60min, grog from the operating process of efflorescence is: naturally be cooled to 750 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 90 ℃, and be 120min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 90 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
According to claim 3 a kind of from flyash the comprehensive method of extracting aluminium and lithium, it is characterized in that: in step (B), the mass ratio of flyash and agglutinant is 1:1.5, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 850 ℃, and the heating roasting time is 90min, grog from the operating process of efflorescence is: naturally be cooled to 650 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 150 ℃, and be 90min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 150 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
According to claim 3 a kind of from flyash the comprehensive method of extracting aluminium and lithium, it is characterized in that: in step (B), the mass ratio of flyash and agglutinant is 1:3, wherein, agglutinant is selected yellow soda ash, and the temperature of retort furnace is 650 ℃, and the heating roasting time is 90min, grog from the operating process of efflorescence is: naturally be cooled to 450 ℃, constant temperature keeps 20min to finish from efflorescence; In step (C), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 200 ℃, and be 120min heat-up time; In step (D), liquid and solid volume are than being 1:50, and the massfraction of sodium carbonate solution is 10%, and the temperature of hot plate is 200 ℃, and be 60min heat-up time; In step (E), in solution, pass into carbon dioxide, when the pH=7 of solution, stop ventilation; In step (F), to contain the lithium mother liquor and under 65 ℃ of temperature, carry out evaporation concentration, until when having crystal to begin to separate out, mother liquor is stirred and be cooled to room temperature, filter, subsequently filtrate is carried out 2 ℃ of deepfreezes, separate out a large amount of crystals of sodium carbonate, this crystals of sodium carbonate can be used as the agglutinant of step (B).
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