CN101284668B - Process for abstracting earth silicon, oxide of alumina and gallium oxide from high-alumina flying ash - Google Patents
Process for abstracting earth silicon, oxide of alumina and gallium oxide from high-alumina flying ash Download PDFInfo
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Abstract
A method for extracting silicon dioxide, alumina and gallium oxide from high-alumina fly ash relates to the technology fields of environmental mineralogy and material, chemical industry and metallurgy. The method comprises the main steps as follows: causing the high-alumina fly ash to react with a sodium hydroxide solution; filtering the solution; introducing CO2 to the filtrate for full gelation; cleaning, purifying, drying, grinding and calcining the silica gel after gel filtration to obtain finished white carbon black; adding limestone and a sodium carbonate solution into the filter mass after the reaction and the filtration of the high-alumina fly ash and the sodium hydroxide solution; ball-grinding the mixture into raw slurry; dissolving out the clinker obtained by baking the raw slurry; deep-desiliconizing the filtrate to obtain a sodium aluminate extraction liquid; filtrating the sodium aluminate extraction liquid after subjecting the sodium aluminate extraction liquid to carbon dioxide decomposition; baking the aluminum hydroxide after washing the filter mass to form the aluminum hydroxide product; and extracting the gallium oxide from the carbon dioxide decomposition mother solution and desiliconized solution. The method has the advantages of cheap raw materials, simple operating procedures, low investment, low production cost, low energy consumption and less slag.
Description
Technical field
The present invention relates to environmental mineral and material, chemical industry and metallurgical technology field, particularly a kind of method of from aluminous fly-ash, extracting silicon-dioxide, aluminum oxide and gallium oxide.
Background technology
Along with the continuous increase of country to the metallurgical-grade aluminum oxide demand, and the minimizing day by day of China's bauxite reserves, the aluminum-containing mineral resource such as flyash, the coal gangue etc. that utilize mankind's activity to produce, replace natural bauxite to produce Industrial products such as aluminum oxide, and the recycling economy industrial chain of formation coal-electric power-metallurgy, paid more and more attention.Chinese patent of the prior art, " a kind of method of utilizing fly-ash Preparation aluminum and coproducing cement grog " of the patent No. 03131079.6 and two patents of invention of " utilizing the method for flyash and Wingdale combination producing aluminum oxide and cement " of the patent No. 200410090949.1 all relate to from flyash to be produced aluminum oxide and produces cement.The flyash of these two technology adds materials and is Wingdale, because the addition of Wingdale is bigger, cause energy consumption and become the quantity of slag higher, and other resource in the aluminous fly-ash does not make full use of.
White carbon black, i.e. hydrated SiO 2, a kind of white powder amorphous hydrated silica as a kind of important fine inorganic Chemicals, has extensive use in every field such as rubber, plastics, agricultural chemicals, paint, pharmacy, papermaking, household chemicalss.Chinese patent of the prior art, the patent No. is that the raw material that 93111642.2 patent of invention " is utilized coal ash to produce the method for carbon black and white carbon black " to adopt also is a flyash, but flyash need pass through flotation, drying, classification, levigate, homogenizing is handled the back and prepared white carbon black.Complex manufacturing, and material consumption is bigger, and production cost is also higher.
The purposes of gallium is very extensive, is mainly used in electronic industry, and the demand of the annual gallium in the whole world is 100 tons, and 80 tons of actual output less thaies, so the extraction of gallium also has good marketable value.Still find no at present the patented technology of from flyash, extracting gallium oxide.
Summary of the invention
In order to overcome the deficiency that above-mentioned prior art exists, purpose of the present invention provides a kind of method of extracting silicon-dioxide, aluminum oxide and gallium oxide from aluminous fly-ash.The cost of material that this method is used is cheap, operation steps simple, less investment, production cost is low, energy consumption is low, the quantity of slag is few.
In order to reach above-mentioned goal of the invention, technical scheme of the present invention realizes as follows:
A kind of method of from aluminous fly-ash, extracting silicon-dioxide, aluminum oxide and gallium oxide, its key step is:
A) aluminous fly-ash and sodium hydroxide solution generate the filtrate and the desiliconization flyash filter cake of preparation white carbon black at autoclave internal reaction after-filtration.With the part silicon-dioxide in the sodium hydroxide solution extraction aluminous fly-ash, the concentration of sodium hydroxide solution is 15-30%, and the mass ratio of sodium hydroxide and aluminous fly-ash is 0.3-0.8: 1, and temperature of reaction is 90-150 ℃, reaction times is 2-4 hour, SiO in the desiliconization filtrate
2Concentration be 50-80g/l, Si/Al is 40-50.
B) in filtrate, feed CO
2Gas reacts, and when the pH value drops to 13, stops ventilation, and filtrate leaving standstill removed post precipitation, continues to feed in filtrate CO under equality of temperature
2Up to the abundant gel of filtrate.
C) to gel solution hybrid filtering, the sodium carbonate solution after the filtration is desiliconization mother liquor and silica gel, by with the desiliconization mother liquor in Na
2O is that 1: 1 mol ratio adds milk of lime and carries out causticization, replenishes solid caustic soda after the NaOH solution concentration that causticization forms and returns step a) and recycle as sodium hydroxide solution.
D) add dilute hydrochloric acid in silica gel, with reacting liquid filtering, and water cleans silica gel behind the stirring reaction, with clean silica gel after the removal of impurities dry, grind, calcine the finished product white carbon black.
E) in filter cake, add thin Wingdale and, mixture is ground into charge pulp at the ball mill endosphere through spissated sodium carbonate solution.
F) charge pulp is sent into rotary kiln baking, reclaim the CO that roasting produces with solvent method
2, CO
2Be used to prepare the refine carbon branch of liquid of white carbon black and sodium aluminate after concentrating.
G) the grog water stripping of charge pulp roasting generation, filtrate is crude liquor of sodium aluminate, filter cake is the silico-calcium slag.
H) with two sections desiliconization methods to the crude liquor of sodium aluminate deep desilication, obtain the sodium aluminate liquid of refining.
I) sodium aluminate is refined liquid divides carbon branch in the tower group at carbon.
J) carbon divides after-filtration, is aluminium hydroxide after the filter cake washing, forms alumina product through roasting, and washings is joined step I) carbon mother liquid in mix, concentrate and additional solid sodium carbonate returns step e) and recycles.
K) carbon mother liquid and desiliconization Recycling Mother Solution become rich Ga solution after using repeatedly, adopt carbon fractional precipitation-dissolution of sodium hydroxide method to make the further enrichment of gallium oxide.The method of enrichment is: carbon branch temperature is 70 ℃ for the first time, and endpoint pH is controlled at 10.5-11; Carry out the carbon branch second time after filtering out aluminum hydroxide precipitation, carbon branch temperature is 50-60 ℃, and endpoint pH is controlled at 8, solution is separated out post precipitation and liquid phase separation, with NaOH solution precipitation is carried out stripping, 80-90 ℃ of stripping temperature, NaOH concentration is 15-20%, and dissolution time is 1-3 hour; Dissolution fluid carries out carbon branch for the third time, and carbon divides condition with for the second time identical, treats after precipitation is separated out precipitated phase to be separated and dissolve once more with NaOH.Adopt resin adsorption method therefrom to extract gallium oxide then.
In aforesaid method, the described CO that in filtrate, feeds
2The temperature of reaction of carrying out gel is 40-70 ℃, and the pH value of impurity A l precipitate and separate is controlled at 13, and except that the Si/Al in the solution behind the Al is 70-80, the pH value of final gel is 10-12.
In aforesaid method, behind the described hi-sil, the dilute hydrochloric acid concentration when with dilute hydrochloric acid the yellow soda ash that is mingled with in the silica gel being removed and washing with water is 15-20%, and the volume of dilute hydrochloric acid and the weight ratio of aluminous fly-ash are 0.02-0.08m
3: 1 ton, temperature of reaction is 50-75 ℃, and the reaction times is 1-2 hour.
In aforesaid method, the bake out temperature after the described silica gel removal of impurities is 80-105 ℃, and calcining temperature is 450-750 ℃, and calcination time is 1-3 hour.
In aforesaid method, the aluminous fly-ash after the described desiliconization, the Wingdale after pulverizing, the charge pulp water ratio that sodium carbonate solution mixes with water and ball milling is made is 30-40%, and Al/Si is than being 2.0-2.5, and the calcium saturation ratio is 0.75-1, and the sodium saturation ratio is 0.90-1.4.
In aforesaid method, described charge pulp is 950-1150 ℃ in the temperature range of revolution roasting in kilns, and the grog index is: Al/Si is than 2.0-2.4, and the calcium saturation ratio is 0.70-1, and the sodium saturation ratio is 0.85-1.35.
In aforesaid method, the leaching condition of the grog that described stripping sinters is: water/clinker quality is than being 1.7-2.5: 1, and the stripping temperature range is 55-75 ℃, the time is 5-30 minute; After stripping finishes, enter separation system and carry out solid-liquid separation, the crude liquor of sodium aluminate after the separation enters the carbon operation break-down, and solid-state silico-calcium slag is produced cement and other building material made with desulfurized gesso of flue gas after washing.
In aforesaid method, the index of described stripping crude liquor of sodium aluminate is: Al
2O
3Concentration is 100-150g/l, and causticity is than being 1.05-1.25; Al/Si is 90-120.
In aforesaid method, describedly the sodium aluminate coarsening solution is carried out deep desilication carry out in two stages in reactor, fs adds the Bayer process red mud of 15-20g/l 150-170 ℃ of desiliconization 2-4 hour of pressurizeing down, subordinate phase is carried out degree of depth silica removal for the sodium aluminate after the first desiliconization is added milk of lime, the add-on of CaO is the 4-6 gram in every liter of sodium aluminate solution, 90-95 ℃ of silica removal temperature, reaction times 1.5-2 hour, the Al/Si that sodium aluminate is refined in the liquid behind the degree of depth silica removal surpassed 1000.
In aforesaid method, feed CO described the branch at carbon in sodium aluminate is refined liquid in the tower group
2The temperature that carbon divides is 75 ℃, and it is 10.5 that carbon divides the pH value of terminal point control.
Compare with existing limestone sintering method, characteristics of the present invention are:
1,1 ton of aluminum oxide of every production needs the overburnt material total mass for the treatment of of preparation to reduce more than 1/3.
2, under the constant condition of soaking time, the maturing temperature of raw material reduces about 250 ℃.
3, the one-tenth quantity of slag of aluminum oxide per ton reduces 70-80%.
4, sodium aluminate is easy to stripping in the grog, and leaching condition is spacious, Al in the dissolution fluid
2O
3Concentration bring up to 120-140g/l by the 20-30g/l of limestone sintering method, and causticity is than being reduced to 1.1-1.2 by 1.7, this just makes the easier deep desilication that carries out of this solution handle.
5, Al
2O
3Extraction yield can improve about 5%.
6, for the flyash that is rich in gallium oxide, from recycle to a certain degree carbon mother liquid and sodium hydroxide solution extract gallium oxide.
7, in whole process of production, CO in the conversion between sodium hydroxide and the yellow soda ash, the kiln gas
2Recycling organic and reasonably combine, both reduced the circulation of material, saved cost, also simplified production link, reduced the shared space of material.
Use the inventive method can make the alumina product that meets standard GB 8178-87 and People's Republic of China's non-ferrous metal industry aluminum oxide standard (YS/T 274-1998), and the white carbon black product that meets standard GB 10517-89, can produce building material product and extract the silico-calcium slag that aluminum oxide produced, demonstrate fully the Scientific Outlook on Development of making the best use of everything.
The present invention will be further described below in conjunction with accompanying drawing.
Description of drawings
Accompanying drawing is technological process of production figure of the present invention.
Embodiment
Referring to accompanying drawing, the method steps when the present invention uses is:
A) with 15% sodium hydroxide solution and aluminous fly-ash under 120 ℃ at 3 hours after-filtration of autoclave internal reaction, filtrate is as the raw material of preparation white carbon black, and filter cake is desiliconization flyash.
B) under 70 ℃ condition, in filtrate, feed CO
2React, when the pH value drops to 13, stop ventilation.After filtrate is left standstill 30 minutes, the precipitation that produces is removed, under equality of temperature, continue logical CO in filtrate
2Up to the abundant gel of solution.
C) mixed system of gel and solution is filtered, the sodium carbonate solution after the filtration is the desiliconization mother liquor, by with the desiliconization mother liquor in Na
2O is that 1: 1 mol ratio adds milk of lime 95 ℃ of following causticizations.Replenishing the small amount of solid caustic soda after the NaOH solution concentration that causticization forms returns step a) and recycles.
D) filter cake is the silica gel that contains a small amount of yellow soda ash, and the ratio of joining 60 kilograms of dilute hydrochloric acid in aluminous fly-ash per ton adds 20% dilute hydrochloric acid in silica gel, reacting liquid filtering is fallen after 1 hour at 60 ℃ of following stirring reactions, and water fully cleans silica gel.Silica gel after the removal of impurities is in 105 ℃ of oven dry down, pulverizing, and calcining was exactly the finished product white carbon black in two hours under 550 ℃.
E) with the aluminous fly-ash after the desiliconization, levigated Wingdale, preceding batch carbon mother liquid sodium carbonate solution and water are mixed in proportion, flyash: Wingdale: the mass ratio of yellow soda ash is 1: 0.55: 0.61, the water ratio of mixed system is 35%, and mixed system abundant ball milling in ball mill is made charge pulp.
F) charge pulp is pressed into rotary kiln baking, roasting condition is: be incubated 1 hour down at 980 ℃.And reclaim the CO that roasting produces with industrial sophisticated solvent method
2, be used to prepare the refine carbon branch of liquid of white carbon black and sodium aluminate after concentrating.
G) after grog burnt till, water was to the stripping of roasting grog, and leaching condition is: 65 ℃ of temperature, and 25 minutes time, the mass ratio of water and grog is 2: 1; Filtrate is crude liquor of sodium aluminate, and filter cake is the silico-calcium slag.
H) with two sections desiliconization methods crude liquor of sodium aluminate is carried out deep desilication, obtain the sodium aluminate liquid of refining, the desiliconization condition is: first desiliconization, and every liter of crude liquor of sodium aluminate adds sodium white residue 15 grams, 150 ℃ of desiliconization temperature, desiliconization time 3 hours, with sodium white residue precipitate and separate, add milk of lime then and carry out the desiliconization second time after the first desiliconization, the desiliconization condition is that the CaO addition of every liter of solution is 6 grams, the desiliconization temperature is 95 ℃, 2 hours reaction times.
I) liquid of refining of the sodium aluminate after the desiliconization divides carbon branch in the tower group at carbon, and carbon branch condition is; Carbon branch temperature is 80 ℃, and endpoint pH is 10.
J) carbon filters after dividing end, filter cake carries out roasting through the aluminium hydroxide after the washing by industrial sophisticated scheme and forms alumina product, washing lotion joins in the carbon mother liquid, it is concentrated to concentration about 25% after, replenish a spot of solid sodium carbonate and return step e) and recycle.
K) carbon mother liquid and desiliconization Recycling Mother Solution use after certain number of times, become rich Ga solution, can adopt three carbon fractional precipitation-dissolution of sodium hydroxide methods to make the further enrichment of gallium oxide in succession, adopt resin adsorption method therefrom to extract gallium oxide then.Carbon branch temperature is 70 ℃ for the first time, endpoint pH is controlled at 11, carry out the carbon branch second time after filtering out aluminum hydroxide precipitation, carbon branch temperature is 60 ℃, and endpoint pH is controlled at 8, solution is separated out after the precipitation, with liquid phase separation, with NaOH solution precipitation is carried out stripping then, 90 ℃ of stripping temperature, NaOH concentration is 10%, and dissolution time is 2 hours.Dissolution fluid is carried out carbon branch for the third time, and carbon divides condition with for the second time identical, treats after precipitation is separated out precipitated phase to be separated and dissolve once more with NaOH, adopts industrial resin adsorption method commonly used to extract gallium oxide in the solution then.
Claims (10)
1. method of from aluminous fly-ash, extracting silicon-dioxide, aluminum oxide and gallium oxide, its key step is:
A) aluminous fly-ash and sodium hydroxide solution generate the filtrate and the desiliconization flyash filter cake of preparation white carbon black at autoclave internal reaction after-filtration; With the part silicon-dioxide in the sodium hydroxide solution extraction aluminous fly-ash, the concentration of sodium hydroxide solution is 15-30%, and the mass ratio of sodium hydroxide and aluminous fly-ash is 0.3-0.8: 1, and temperature of reaction is 90-150 ℃, reaction times is 2-4 hour, SiO in the desiliconization filtrate
2Concentration be 50-80g/l, Si/Al is 40-50;
B) in filtrate, feed CO
2Gas reacts, and when the pH value drops to 13, stops ventilation, and filtrate leaving standstill removed post precipitation, continues to feed in filtrate CO under equality of temperature
2Up to the abundant gel of filtrate;
C) to gel solution hybrid filtering, the sodium carbonate solution after the filtration is desiliconization mother liquor and silica gel, by with the desiliconization mother liquor in Na
2O is that 1: 1 mol ratio adds milk of lime and carries out causticization, replenishes solid caustic soda after the NaOH solution concentration that causticization forms and returns step a) and recycle as sodium hydroxide solution;
D) add dilute hydrochloric acid in silica gel, with reacting liquid filtering, and water cleans silica gel behind the stirring reaction, with clean silica gel after the removal of impurities dry, grind, calcine the finished product white carbon black;
E) in filter cake, add thin Wingdale and, mixture is ground into charge pulp at the ball mill endosphere through spissated sodium carbonate solution;
F) charge pulp is sent into rotary kiln baking, reclaim the CO that roasting produces with solvent method
2, CO
2Be used to prepare the refine carbon branch of liquid of white carbon black and sodium aluminate after concentrating;
G) the grog water stripping of charge pulp roasting generation, filtrate is crude liquor of sodium aluminate, filter cake is the silico-calcium slag;
H) with two sections desiliconization methods to the crude liquor of sodium aluminate deep desilication, obtain the sodium aluminate liquid of refining;
I) sodium aluminate is refined liquid divides carbon branch in the tower group at carbon;
J) carbon divides after-filtration, is aluminium hydroxide after the filter cake washing, forms alumina product through roasting, and washings is joined step I) carbon mother liquid in mix, concentrate and additional solid sodium carbonate returns step e) and recycles;
K) carbon mother liquid and desiliconization Recycling Mother Solution become rich Ga solution after using repeatedly, adopt carbon fractional precipitation-dissolution of sodium hydroxide method to make the further enrichment of gallium oxide, and the method for enrichment is: carbon branch temperature is 70 ℃ for the first time, and endpoint pH is controlled at 10.5-11; Carry out the carbon branch second time after filtering out aluminum hydroxide precipitation, carbon branch temperature is 50-60 ℃, and endpoint pH is controlled at 8, solution is separated out post precipitation and liquid phase separation, with NaOH solution precipitation is carried out stripping, 80-90 ℃ of stripping temperature, NaOH concentration is 15-20%, and dissolution time is 1-3 hour; Dissolution fluid carries out carbon branch for the third time, and carbon divides condition with for the second time identical, treats after precipitation is separated out precipitated phase to be separated and dissolve once more with NaOH; Adopt resin adsorption method therefrom to extract gallium oxide then.
2. method according to claim 1 is characterized in that, the described CO that feeds in filtrate
2The temperature of reaction of carrying out gel is 40-70 ℃, and the pH value of impurity A l precipitate and separate is controlled at 13, and except that the Si/Al in the solution behind the Al is 70-80, the pH value of final gel is 10-12.
3. method according to claim 1 and 2, it is characterized in that, behind the described hi-sil, the dilute hydrochloric acid concentration when with dilute hydrochloric acid the yellow soda ash that is mingled with in the silica gel being removed and washing with water is 15-20%, and the volume of dilute hydrochloric acid and the weight ratio of aluminous fly-ash are 0.02-0.08m
3: 1 ton, temperature of reaction is 50-75 ℃, and the reaction times is 1-2 hour.
4. method according to claim 3 is characterized in that, the bake out temperature after the described silica gel removal of impurities is 80-105 ℃, and calcining temperature is 450-750 ℃, and calcination time is 1-3 hour.
5. method according to claim 1, it is characterized in that, aluminous fly-ash after the described desiliconization, Wingdale after pulverizing, the charge pulp water ratio that sodium carbonate solution mixes with water and ball milling is made is 30-40%, Al/Si is than being 2.0-2.5, and the calcium saturation ratio is 0.75-1, and the sodium saturation ratio is 0.90-1.4.
6. method according to claim 5 is characterized in that, described charge pulp is 950-1150 ℃ in the temperature range of revolution roasting in kilns, and the grog index is: Al/Si is than 2.0-2.4, and the calcium saturation ratio is 0.70-1, and the sodium saturation ratio is 0.85-1.35.
7. method according to claim 6 is characterized in that, the leaching condition of the grog that described stripping sinters is: water/clinker quality is than being 1.7-2.5: 1, and the stripping temperature range is 55-75 ℃, the time is 5-30 minute; After stripping finishes, enter separation system and carry out solid-liquid separation, the crude liquor of sodium aluminate after the separation enters the carbon operation break-down, and solid-state silico-calcium slag is produced cement and other building material made with desulfurized gesso of flue gas after washing.
8. method according to claim 7 is characterized in that the index of described stripping crude liquor of sodium aluminate is: Al
2O
3Concentration is 100-150g/l, and causticity is than being 1.05-1.25; Al/Si is 90-120.
9. method according to claim 8, it is characterized in that, describedly the sodium aluminate coarsening solution is carried out deep desilication carry out in two stages in reactor, fs adds the Bayer process red mud of 15-20g/l 150-170 ℃ of desiliconization 2-4 hour of pressurizeing down, subordinate phase is carried out degree of depth silica removal for the sodium aluminate after the first desiliconization is added milk of lime, the add-on of CaO is the 4-6 gram in every liter of sodium aluminate solution, 90-95 ℃ of silica removal temperature, reaction times 1.5-2 hour, the Al/Si that sodium aluminate is refined in the liquid behind the degree of depth silica removal surpassed 1000.
10. method according to claim 9 is characterized in that, feed CO described the branch at carbon in sodium aluminate is refined liquid in the tower group
2The temperature that carbon divides is 75 ℃, and it is 10.5 that carbon divides the pH value of terminal point control.
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| CN1868884A (en) * | 2006-06-02 | 2006-11-29 | 李禹� | Method of extracting aluminium oxide from fly ash and simultaneously producing white carbon black |
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