CN106477609B - Method for producing alumina by coal ash sulfuric acid curing - Google Patents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/26—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with sulfuric acids or sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/24—Alkaline-earth metal silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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Abstract
The invention discloses a method for producing alumina by using sulfuric acid curing of fly ash, belonging to the technical field of comprehensive utilization of fly ash. Mixing a proper amount of concentrated sulfuric acid and fly ash uniformly, curing to obtain sulfated clinker, leaching the clinker by using aluminum sulfate crystallization mother liquor or water to obtain an aluminum sulfate solution and high-silicon slag, evaporating, concentrating, crystallizing, drying and dehydrating the aluminum sulfate solution to obtain aluminum sulfate, rapidly reducing and roasting the aluminum sulfate and a proper amount of reducing agent together to obtain crude alumina, and then treating the crude alumina by adopting a low-temperature Bayer process to produce metallurgical-grade aluminum oxide. The obtained high silicon slag can be leached by sodium hydroxide to produce white carbon black or active calcium silicate. The method has the advantages of high aluminum recovery rate, easy solving of equipment materials, good quality of aluminum oxide products and the like, and residues after aluminum leaching are high-silicon residues with good alkali dissolution activity, so that various high-value-added silicon products can be further produced.
Description
Technical field
The invention belongs to the comprehensive utilizations of flyash, are related to the method for flyash production aluminium oxide, in particular by sulfuric acid
The method that curing process produces aluminium oxide.
Background technology
Coal burning process generates a large amount of flyash, is utilized except small part obtains part for cement building material raw materials for production
Outside, most of flyash stockpiling, does not only take up large amount of land resources, and environmental pollution is serious.There are a large amount of high alumina coals in China,
The a large amount of aluminous fly-ash of combustion power generation process output, aluminium content is more up to 40-60% in flyash, has higher extraction
Aluminium is worth.But since the alumina silica ratio in flyash is very low, traditional process for making alumina is difficult in adapt to treated coal ash, needs
Using the technology of suitable flyash feature, the flyash production aluminium oxide method studied both at home and abroad at present is roughly divided into alkaline process
With two major class of acid system.
Alkaline process includes direct sintering and pre-desiliconizing-sintering process etc..Direct sintering is produced similar to Bauxite Sintering method
Flyash and agstone are mixed in a certain ratio dry sintering after ore grinding, then go out clinker with alkali soluble and carry by alumina technology
Aluminium oxide is taken, leached mud is for producing cement, and due to the siliceous height of flyash, direct sintering needs to be incorporated large quantities of lime mountain flour, burns
High energy consumption is tied, and extracts the meeting after aluminium oxide and generates a large amount of calcium silicate slags, often producing 1 ton of aluminium oxide needs 8~10 tons of calcium silicate slags of output,
How to dissolve dispose these new top of the slag face bigger difficulty.Alkali leaching pre-desiliconizing processing is carried out to flyash can reduce sintered material
Amount leaches the quantity of slag, while the siliceous solution that pre-desiliconizing obtains can produce white carbon, silicon ash so as to reduce sintering energy consumption and reduce
The high level silicon product such as stone.A kind of method that aluminium oxide is extracted from aluminous fly-ash as disclosed in CN101284668A, by high alumina
Flyash carries out pressure leaching with sodium hydroxide solution in autoclave, makes part silicon dissolution, and siliceous leachate is used to give birth to
White carbon is produced, the flyash after pre-desiliconizing is sintered after being mixed with agstone, sodium carbonate liquor, then leaches aluminium.Using pre- de-
Silicon technology can improve the alumina silica ratio of flyash, reduce sintering amount, so as to reduce alumina producing energy consumption, and by-product white carbon,
The silicon product such as wollastonite, but for large-scale total utilization of PCA, the market sale that white carbon, wollastonite product face with
Competitive pressure is very big.In addition, for circulating fluidized bed boiler flyash, since its sulfur-bearing is generally higher, using alkali process
Alkaline consumption higher, and be carbonized or seed precipitation solution in sulfate concentration it is high, desulphurization load is big, of high cost.
Flyash acid system produces aluminium oxide due to not needing to slagging medicament, and the level of residue extracted after aluminium oxide is few, meets and subtracts
The requirement of quantization comprehensive utilization Industrial Solid Waste.But due in flyash aluminium mainly with the low aluminium silicon of mullite or other chemisms
Acid salts exist, and direct acidleach is difficult, need leach or pressurize using the concentrated sulfuric acid high temperature salt Ore Leaching or the leaching of fluoride hydrotropy
Go out, corrosive medium is strong, and equipment material requirement is high, cost is high, and aluminium leaching rate is relatively low, and the energy consumption of aluminium oxide is high, of high cost.
Invention content
The purpose of the invention is to overcome the shortcomings of in existing flyash extraction aluminum oxide technology, a kind of flyash is provided
The method of sulfuric acid curing production aluminium oxide.
For achieving the above object, technical scheme is as follows.
The method of flyash sulfuric acid curing production aluminium oxide, includes the following steps：
(1) sulfuric acid cures：Flyash is cured with the concentrated sulfuric acid after mixing according to a certain ratio obtain sulphation ripe
Material, 100~500 DEG C of the curing temperature of the curing, 1~48h of curing time；
(2) it leaches：The sulphation clinker aluminum sulfate crystals mother liquor and appropriate supplement water that step (1) is obtained are mixed
It is filtered after a period of time, obtains aluminum sulfate solution and high white residue；
(3) condensing crystallizing：The aluminum sulfate solution that step (2) is obtained is concentrated by evaporation, and is then crystallized, is filtered, is crystallized
Aluminum sulfate and crystalline mother solution, crystalline mother solution return to step (2) leach；
(4) drying and dehydrating：The crystalline sulfuric acid aluminium that step (3) obtains is dried and removed the crystallization water, obtains aluminum sulfate；
(5) reduction roasting：The aluminum sulfate that step (4) is obtained restores at a certain temperature together with appropriate reducing agent
Roasting obtains thick aluminium oxide and sulfur-containing smoke gas, and relieving haperacidity return to step (1) recycles after sulfur-containing smoke gas is collected；
(6) low temperature Bayer Process digestion：The thick aluminium oxide that step (5) obtains is carried out with seed precipitation solution and appropriate supplement lye
Low-temperature alkaline soaks, and then solid-liquor separation obtains sodium aluminate solution；
(7) aluminium oxide is prepared：The sodium aluminate solution that step (6) obtains is prepared into aluminium hydroxide through kind point or carbon point, then
Separation of solid and liquid obtains aluminium hydroxide and seed precipitation solution, and mother liquor return to step (6) recycles, and aluminium hydroxide is through calcining production oxidation
Aluminium.
The proportioning of flyash and the concentrated sulfuric acid is by H in the concentrated sulfuric acid in step (1)2SO4With Al in flyash2O3Mole ratio
3:1~5:1 adds in, mass concentration >=85% of the concentrated sulfuric acid.
Curing is using swinging equipment in step (1), and the swinging equipment is rotary kiln, revolving drum, rotating disk, spiral
It puddles one or more in equipment.Temperature divides 1~6 section to be cured from low to high.
Further, the curing temperature in step (1) is 150~350 DEG C, and the curing time is 0.5~4h.
Further, the curing in step (1) is cured using rotary kiln, controls the heating rate of material in rotary kiln
For 0.5~5 DEG C/min, wherein 100~150 DEG C of sections residence time not less than 30min, in the stop of 200~300 DEG C of sections
Between be 0.5~2h.
Further, in step (3), before condensing crystallizing, the sulfuric acid concentration in aluminum sulfate solution is adjusted, until in solution
Al2(SO4)3With H2SO4Mass concentration ratio be 10:1~50:1.
Further, it is concentrated by evaporation in step (3) and is evaporated using MVR evaporators, 60~100 DEG C of evaporating temperature.It crystallizes and is
Crystallisation by cooling, liquid is cooled to 30~50 DEG C and is crystallized after will concentrating.
Reducing agent described in step (5) contains for low values such as coal dust, bastard coal mountain flour, coal gas, natural gas, sulphur or petroleum cokes
It is one or more in carbon fuel, preferably coal gas or natural gas.
Further, the reduction roasting described in step (5) is roasted for fast fluidization, and roaster is roasted for recirculating fluidized bed
Burn one kind in stove, gaseous pollutant control or fluidised form flash roaster.
Further, the reduction roasting temperature in step (5) is 500-900 DEG C, preferably 650-800 DEG C, during reduction roasting
Between 0.1-60min, preferably 0.1-15min.
Low temperature Bayer Process digestion described in step (6), leaching condition are：80-250 DEG C of leaching temperature, alkali concn 100-
250g/L, extraction time 20-80min, ingredients molecular ratio αk0.8-2.0。
Further, the high white residue sodium hydroxide solution that step (2) obtains leaches silicon, and obtained sodium silicate solution is used for
Produce white carbon or active calcium silicate.
The method of the flyash sulfuric acid curing production aluminium oxide of the present invention, available for various types of flyash, Ke Yishi
It is one or more in Circulation fluidized-bed furnace flyash, coal-powder boiler flyash, grate furnace flyash, cyclone furnace flyash, especially
It is suitable for processing cycle fluid bed furnace desulfurization flyash.
The method of the flyash sulfuric acid curing production aluminium oxide of the present invention, --- water logging --- MVR steamings are cured using sulfuric acid
--- --- drying and dehydrating --- reduction roasting --- low temperature Bayer process recycles aluminium oxide to crystallisation by cooling, ripe by sulfuric acid for hair concentration
Change enhances the decomposition of aluminium silicate mineral in flyash and is converted into water-soluble aluminum sulfate, then extracts aluminium oxide by water logging
And adverse effect of the sulphur in flyash to alumina producing Bayer process is eliminated, equipment material easily solves, and aluminium recovery is high；
Condensing crystallizing is carried out using MVR evaporations and crystallisation by cooling, evaporation capacity is few, low energy consumption；Aluminum sulfate is decomposed using reduction roasting, can be dropped
The decomposition temperature of low aluminum sulfate and the alkali soluble activity for improving aluminium oxide in calcining, so as to reduce roasting energy consumption and improve the recycling of aluminium
Rate.
Description of the drawings
Principle flow chart of the attached drawing for the method for the present invention.
Specific embodiment
Further explanation is made to the present invention below in conjunction with attached drawing.
By suitable concentrated sulfuric acid and flyash mix it is uniform after cured to obtain sulphation clinker, then with aluminum sulfate knot
Brilliant mother liquor or water logging go out clinker and obtain aluminum sulfate solution and high white residue, and aluminum sulfate solution is obtained through evaporating, concentrating and crystallizing, drying and dehydrating
To aluminum sulfate, aluminum sulfate is subjected to quick reduction roasting together with appropriate reducing agent and obtains thick aluminium oxide, is then visitd using low temperature
The thick alumina producing metallurgical-grade aluminum oxide of ear method processing.The high white residue of gained produces white carbon or active silicic acid through leaching with sodium hydroxide
Calcium.
The method of the present invention is further described with nonlimiting examples below, to help to understand the present invention's
Content and its advantage, and not as limiting the scope of the present invention, protection scope of the present invention is determined by claims.
Embodiment 1
The concentrated sulfuric acid of cycle fluid-bed boiler fly ash and concentration 93% is cured 2h after mixing to obtain at 200 DEG C
Sulphation clinker, the addition of the concentrated sulfuric acid is by H in sulfuric acid2SO4With Al in flyash2O3Mole ratio 3.5:1 adds in, and uses water logging
Go out clinker, leachate is concentrated by evaporation, crystallizes, drying and dehydrating obtains aluminum sulfate, and aluminum sulfate obtains thick aluminium oxide through reduction roasting, slightly
Aluminium oxide is leached at 95 DEG C using the sodium hydroxide solution of 100g/L and obtains sodium aluminate solution, and sodium aluminate solution divides through kind, forges
Burning obtains metallurgical-grade aluminum oxide.
Embodiment 2
Cycle fluid-bed boiler fly ash and the concentrated sulfuric acid of concentration 93% are cured in rotary kiln after mixing,
The addition of the concentrated sulfuric acid presses H in sulfuric acid2SO4With Al in flyash2O3Mole ratio 3.5:1 adds in, and mixed material is 100~150
The residence time of DEG C temperature section is 1h, obtains sulphation clinker in the residence time 0.5h of 200~250 DEG C of temperature sections, uses water logging
Go out clinker, leachate is concentrated by evaporation, crystallizes, drying and dehydrating obtains aluminum sulfate, and aluminum sulfate obtains thick aluminium oxide through reduction roasting, slightly
Aluminium oxide is leached at 95 DEG C using the sodium hydroxide solution of 100g/L and obtains sodium aluminate solution, and sodium aluminate solution divides through kind, forges
Burning obtains metallurgical-grade aluminum oxide.
Embodiment 3
Cycle fluid-bed boiler fly ash and the concentrated sulfuric acid of concentration 93% are cured in rotary kiln after mixing,
The addition of the concentrated sulfuric acid presses H in sulfuric acid2SO4With Al in flyash2O3Mole ratio 3.5:1 adds in, and mixed material is 100~150
The residence time of DEG C temperature section is 1h, sulphation clinker is obtained in the residence time 0.5h of 200~250 DEG C of temperature sections, with implementation
The aluminum sulfate crystals mother liquor and appropriate supplement water obtained in example 2 leaches clinker together, and leachate is concentrated by evaporation, crystallizes, is dry de-
Water obtains aluminum sulfate, and aluminum sulfate obtains thick aluminium oxide through reduction roasting, thick aluminium oxide using 100g/L sodium hydroxide solution in
It is leached at 95 DEG C and obtains sodium aluminate solution, sodium aluminate solution obtains metallurgical-grade aluminum oxide through kind point, calcining.
Embodiment 4
Cycle fluid-bed boiler fly ash and the concentrated sulfuric acid of concentration 93% are cured in rotary kiln after mixing,
The addition of the concentrated sulfuric acid presses H in sulfuric acid2SO4With Al in flyash2O3Mole ratio 3.5:1 adds in, and mixed material is 100~150
The residence time of DEG C temperature section is 1h, obtains sulphation clinker in the residence time 0.5h of 200~250 DEG C of temperature sections, uses sulfuric acid
Crystalline aluminophosphate mother liquor and appropriate supplement water leach clinker together, and leachate is concentrated by evaporation with MVR evaporation technologies in 90 DEG C, after concentration
Aluminum sulfate solution is cooled to 40 DEG C and is crystallized, and crystal obtains aluminum sulfate through drying and dehydrating, and aluminum sulfate is in gas suspension calcination
Stove carries out reduction roasting with coal smell reducers and obtains thick aluminium oxide, thick aluminium oxide using 150g/L sodium hydroxide solution in
It is leached at 150 DEG C and obtains sodium aluminate solution, sodium aluminate solution obtains metallurgical-grade aluminum oxide through kind point, calcining.
Embodiment 5
Cycle fluid-bed boiler fly ash and the concentrated sulfuric acid of concentration 93% are cured in rotary kiln after mixing,
The addition of the concentrated sulfuric acid presses H in sulfuric acid2SO4With Al in flyash2O3Mole ratio 3.5:1 adds in, and mixed material is 100~150
The residence time of DEG C temperature section is 1h, obtains sulphation clinker in the residence time 0.5h of 200~250 DEG C of temperature sections, uses water logging
Go out clinker, obtain aluminum sulfate solution and high white residue, aluminum sulfate solution is supplemented into Al in moderate amount of sulfuric acid to solution2(SO4)3With H2SO4
Mass concentration ratio be 25:1, then be concentrated by evaporation, crystallize, drying and dehydrating obtain aluminum sulfate, aluminum sulfate is obtained through reduction roasting
Thick aluminium oxide, thick aluminium oxide are leached at 95 DEG C using the sodium hydroxide solution of 100g/L and obtain sodium aluminate solution, sodium aluminate solution
Liquid obtains metallurgical-grade aluminum oxide through kind point, calcining.
Embodiment 6
The sodium hydroxide solution of high white residue 100g/L that embodiment 5 is obtained leaches that obtain sodium metasilicate molten at 100 DEG C
Then liquid prepares white carbon.
Claims (11)
1. the method for flyash sulfuric acid curing production aluminium oxide, which is characterized in that include the following steps：
(1) sulfuric acid cures：Flyash and the concentrated sulfuric acid are cured to obtain sulphation clinker, institute according to a certain ratio after mixing
State 100~500 DEG C of the curing temperature of curing, 1~48h of curing time；Curing equipment is rotary kiln, controls material in rotary kiln
Heating rate is 0.5~5 DEG C/min, and material is not less than 30min in the residence time of 100~150 DEG C of sections, in 200~300 DEG C of sections
Residence time be 0.5~2h；
(2) it leaches：The sulphation clinker aluminum sulfate crystals mother liquor and appropriate supplement water that step (1) is obtained are mixed one section
It is filtered after time, obtains aluminum sulfate solution and high white residue；
(3) condensing crystallizing：Sulfuric acid concentration in the aluminum sulfate solution that regulating step (2) obtains, until Al in solution2(SO4)3With
H2SO4Mass concentration ratio be 10:1~50:1, it is then concentrated by evaporation, then crystallizes, filters, obtain crystalline sulfuric acid aluminium and crystallization
Mother liquor, crystalline mother solution return to step (2) leach；
(4) drying and dehydrating：The crystalline sulfuric acid aluminium that step (3) obtains is dried and removed the crystallization water, obtains aluminum sulfate；
(5) reduction roasting：The aluminum sulfate that step (4) obtains is subjected to reduction roasting, reduction roasting temperature together with appropriate reducing agent
500-900 DEG C, reduction roasting time 0.1-60min of degree, obtains thick aluminium oxide and sulfur-containing smoke gas, after sulfur-containing smoke gas is collected relieving haperacidity return
Step (1) is returned to recycle；
(6) low temperature Bayer Process digestion：The thick aluminium oxide seed precipitation solution that step (5) is obtained carries out low temperature with appropriate supplement lye
Alkali soaks, and then solid-liquor separation obtains sodium aluminate solution；
(7) aluminium oxide is prepared：The sodium aluminate solution that step (6) obtains is prepared into aluminium hydroxide through kind point or carbon point, then solid-liquid
Isolated aluminium hydroxide and seed precipitation solution, mother liquor return to step (6) recycle, and aluminium hydroxide produces aluminium oxide through calcining.
2. according to the method described in claim 1, it is characterized in that, the proportioning of flyash and the concentrated sulfuric acid is by dense in step (1)
H in sulfuric acid2SO4With Al in flyash2O3Mole ratio 3:1~5:1 adds in, mass concentration >=85% of the concentrated sulfuric acid.
3. according to the method described in claim 1, it is characterized in that, described be concentrated by evaporation of step (3) is steamed using MVR evaporators
Hair, 60~100 DEG C of evaporating temperature；The crystallization is cooled to 30~50 DEG C for liquid after concentrating and crystallizes.
4. according to the method described in claim 1, it is characterized in that, reducing agent described in step (5) for coal dust, bastard coal mountain flour,
It is one or more in coal gas, natural gas, sulphur or petroleum coke.
5. according to the method described in claim 4, it is characterized in that, reducing agent described in step (5) is coal gas or natural gas.
6. according to the method described in claim 1, it is characterized in that, 650-800 DEG C of reduction roasting temperature, reduction in step (5)
Roasting time 0.1-15min.
7. according to the method described in claim 1, it is characterized in that, the reduction roasting described in step (5) is fast fluidization
Roasting, roaster are one kind in circulating fluidized bed roasting furnace, gaseous pollutant control or fluidised form flash roaster.
8. according to the method described in claim 1, it is characterized in that, step (6) the low temperature Bayer Process digestion, leaching condition
For：80-200 DEG C of leaching temperature, alkali concn 100-250g/L, extraction time 20-80min, ingredients molecular ratio αk0.8-2.0。
9. according to the method described in claim 1, it is characterized in that, further include step (8), the high white residue that step (2) is obtained
Silicon is leached with sodium hydroxide solution, obtained sodium silicate solution further produces white carbon or active calcium silicate.
10. according to the method described in claim 1, it is characterized in that, step (1) described flyash is Circulation fluidized-bed furnace fine coal
It is one or more in ash, coal-powder boiler flyash, grate furnace flyash, cyclone furnace flyash.
11. according to the method described in claim 10, it is characterized in that, step (1) described flyash is Circulation fluidized-bed furnace powder
Coal ash.
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| CN108130432B (en) * | 2017-12-21 | 2020-08-25 | 武汉理工大学 | Method for dissolving out aluminum by low-temperature activation of kaolin |
| CN108455638A (en) * | 2018-01-25 | 2018-08-28 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | A method of producing aluminum and coproducing 4A zeolite molecular sieves |
| CN109455746A (en) * | 2018-10-25 | 2019-03-12 | 昆明理工大学 | A kind of method of alkali metal salt catalysis aluminum sulfate carbon thermal reduction |
| CN109336147B (en) * | 2018-10-25 | 2021-01-12 | 昆明理工大学 | Method for producing alumina by using industrial solid waste rich in alumina |
| CN109835930A (en) * | 2019-02-19 | 2019-06-04 | 昆明理工大学 | A kind of production method of aluminium oxide |
| EP3825426A1 (en) | 2019-11-22 | 2021-05-26 | Befesa Aluminio, S.L. | Process for transforming secondary aluminium oxide into alternative raw material and uses thereof |
| CN113044865B (en) * | 2019-12-26 | 2022-03-22 | 国家能源投资集团有限责任公司 | Method for preparing aluminum oxide |
| CN111252774A (en) * | 2020-01-19 | 2020-06-09 | 刘文治 | Method for producing silica sol by using desulfurized gypsum and fly ash through treating waste with waste |
| CN112919512B (en) * | 2021-03-01 | 2023-06-30 | 贵州遵义金山磨料有限公司 | Method for preparing aluminum oxide and potassium sulfate by using brown corundum dust-removing ash |
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