CN101397146A - Method for preparing alumina by using fly ash - Google Patents
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- CN101397146A CN101397146A CN 200710012997 CN200710012997A CN101397146A CN 101397146 A CN101397146 A CN 101397146A CN 200710012997 CN200710012997 CN 200710012997 CN 200710012997 A CN200710012997 A CN 200710012997A CN 101397146 A CN101397146 A CN 101397146A
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Abstract
The invention discloses a method for producing alumina by disposing and utilizing industrial solid wastes, in particular to a method for preparing alumina by fly ash, comprising the steps as follows: the fly ash is mechanically activated; the activated fly ash, water and concentrated sulfuric acid react in a reaction kettle under the conditions of heating and pressurizing; the solid is separated from the liquid after the temperature of the reaction is reduced so as to gain aluminium sulfate liquid; the aluminium sulfate liquid is evaporated, concentrated and cooled so as to precipitate aluminium sulphate crystals; the aluminium sulphate crystals are dehydrated and decomposed to gain gama-Al2O3 and SO3; coarse gama-Al2O3 is dissolved in alkaline solution; after the solid is separated from the liquid, the pure sodium aluminate solution is gained; aluminum hydroxide crystal seed is added to the sodium aluminate solution so as to precipitate the aluminum hydroxide; the coarse gama-Al2O3 can be prepared by circularly dissolving the seed-precipitated alkaline solution after vaporization-concentration; the metallurgical alumina can be gained by baking the prepared aluminum hydroxide. The method adds no additive, can lead the alumina in the fly ash to be effectively leached out with the leaching rate more than 90% and saves the energy resource.
Description
Technical field
The present invention relates to a kind of industrial solid castoff processing and utilizing production method of alumina, relate in particular to a kind of fly-ash Preparation method of alumina of utilizing.
Background technology
Flyash is the solid waste that the coal-burning power plant discharges.At present, the more than one hundred million tons of China's flyash annual emissions, total volume of cargo in storage of China's flyash has tens00000000 tons.A large amount of soils are are not only occupied in the discharging of a large amount of flyash, and serious environment pollution, have consisted of the dual destruction to ecosystem environment.Therefore the comprehensive utilization of carrying out flyash has Great significance and long-range strategic importance.Equally, China is the rich country of a bauxite resource, and document announcement the has been arranged assurance degree of 45 kinds of main mineral products of China to demand in 2010 have 10 kinds of mineral products to belong to and can not guarantee, comprising bauxite.According to the waste during the rate of growth and the bauxite of aluminum oxide output are exploited, utilized at present, even consider prospective reserves, the time limit of the bauxite of China also is difficult to reach 50 years.So the method that solves this crisis of resource has two kinds: the one, rationally utilize existing bauxite resource; The 2nd, actively look for and utilize other to contain bauxite resource.And aluminum oxide is one of main component of flyash, and its massfraction is generally 15%～40%, reaches as high as 58%.So, carry out from flyash the pollution that the research work of extracting aluminium oxide can solve flyash, turn waste into wealth.
At present, from flyash, extract aluminum oxide the research comparative maturity limestone sintering method and soda-lime sintering process arranged, both are commonly referred to as alkaline process for this.In December, 2004, Inner Mongolia Autonomous Region Science and Technology Department held " flyash extracts the aluminum and coproducing cement industrialization technology " the project appraisal of scientific and technological achievements meeting of covering the research and development of western new and high technology Group Co.,Ltd, what adopt is exactly improved soda-lime sintering process, this group has independently finished nearly 5000 tonnes pilot scale, and obtains multinomial patent.Also there are some problems in aluminum oxide in the flyash but alkaline process extracts, it mainly is the 1. silico-calcium slag that produces of sintering process, can only be used as cement raw material, the aluminum oxide that every production is 1 ton will produce the silico-calcium slag that is several times as much as flyash, and cement has its corresponding radius of selling, if local do not have large-scale Cement industry support will cause secondary pollution; 2. sintering process has only been extracted the aluminum oxide in the flyash, and the utility value of its silicon-dioxide is low.3. the equipment investment of sintering process treated coal ash is big, energy consumption height, cost height.
Because the alumina silica ratio of flyash is very low, generally all less than 1, so adopt acidic process flyash more reasonable in principle.Acid system leaches the aluminium oxide in the flyash, can make the aluminium salt of generation enter solution, silicon not with acid reaction, fully in the solid phase slag.Acidic process flyash can overcome the deficiency of sintering process, can not produce solid waste more than the raw material powder coal ash, and after extracting aluminum oxide, silicon-dioxide meeting enrichment, its content can reach 80～90% (by leaching rate of alumina 85%) in the slag, so more helps its utilization.Because flyash is that so glassy phase accounts for significant proportion, its chemism is very low through rapidly cooling behind the high-temp combustion.The recovery rate that therefore, improve aluminium oxide in the flyash will be started with from the chemism that improves flyash.The method of document announcement is to add the fluorochemical hydrotropy in acid-leaching reaction at present, silicon is combined with fluorine, reach and discharge the wherein purpose of aluminum oxide, but in the process of hydrotropy, may produce obnoxious flavoures such as HF, in the process of removing the fluorine purifying, can discharge fluorine-containing waste liquid and waste residue again, not only pollute the environment, and can cause potential safety hazard operator.
Summary of the invention
The invention provides a kind of fly-ash Preparation method of alumina of utilizing for solving the problems of the technologies described above, purpose is not added any auxiliary agent, makes alumina extraction ratio height in the flyash, saves the energy.
A kind of coal ash for manufacturing that utilizes of the present invention is for the method for aluminium oxide for achieving the above object, and it comprises the steps: the flyash mechanical activation; Flyash behind the mechanical activation is mixed according to 1:0.5～2.5 with water, add weight ratio and be 1～3.5 the concentrated sulfuric acid in reaction kettle for reaction, be heated to 120 ℃～250 ℃, pressure is 0.11MPa～0.5MPa, reaction time 1h～8h; Separation of Solid and Liquid after the reaction cooling obtains aluminum sulfate liquid, cools off after the evaporation and concentration, separates out the aluminum sulfate crystal; The dehydration of aluminum sulfate crystal obtains dry type aluminum sulfate; The decomposition of dry type aluminum sulfate obtains γ-Al
2O
3And SO
3With thick γ-Al
2O
3In aqueous slkali, dissolve, obtain pure sodium aluminate solution after the Separation of Solid and Liquid; Add aluminium hydroxide crystal seed in the sodium aluminate solution and separate out aluminium hydroxide, plant thick γ-Al that the alkali lye dissolving capable of circulation after inspissation after dividing makes
2O
3The aluminium hydroxide calcining of preparation obtains metallurgical-grade aluminum oxide.
Described mechanical activation is a kind of grinding of adopting in vibration mill, vertical mill, planetary mills or the high-energy ball milling, is ground to the 100-800 order.
The liner of described reactor is a kind of in acid-proof ceramic tile, enamel, glass, fluoroplastics, the tetrafluoroethylene.
Behind described flyash and the acid reaction, the Separation of Solid and Liquid of aluminum sulfate solution and slag adopts a kind of in flocculating setting, pressure filtration or the filtration under diminished pressure.
Described liquid aluminium sulfate evaporation concentration adopts normal pressure or reduction vaporization.
Described Tai-Ace S 150 crystal dehydration is to obtain dry type Tai-Ace S 150 200 ℃ of-400 ℃ of calcinings.
Described dry type aluminum sulfate adds 60%～90% air under 500-900 ℃ temperature, calcining obtains γ-Al
2O
3And SO
3
Described SO
3Absorb preparation sulfuric acid with the vitriol oil.
Described γ-Al
2O
3Contain impurity, with thick γ-Al
2O
3Under 120 ℃～260 ℃, use Na
2The aqueous slkali dissolved under pressure of O150g/L～200g/L, aluminium enter liquid phase and form sodium aluminate solution, in impurity existence and the solid phase, obtain pure sodium aluminate solution after the Separation of Solid and Liquid.
The described aluminium hydroxide crystal seed that adds in sodium aluminate solution is pressed bayer process condition decomposition of crystal seed, obtains aluminium hydroxide.
Described aluminium hydroxide obtains metallurgical-grade aluminum oxide 1000 ℃～1200 ℃ calcinings down.
The sulfuric acid concentration of the described vitriol oil in reactor reduced to 20%-75%.
Described flyash and water add in the reactor, and the concentrated sulfuric acid joins in the pressure vessel that reactor connects, and the concentrated sulfuric acid is flowed in flyash and the reactor that water mixes.
Advantageous effect of the present invention: the present invention adopts new flyash activating technology, does not add any auxiliary agent, can make that aluminium oxide effectively leaches in the flyash, and the leaching rate of aluminium oxide can reach more than 90%.The present invention utilizes diluting concentrated sulfuric acid heat, and reactor temperature is raise, and forms high pressure, strengthens the leaching of aluminium oxide in the flyash, energy savings.Realized the circulation of sour circulation and alkali in the technological process of the present invention, whole process does not have the discharge of waste gas, waste liquid, waste residue.Reaction conditions of the present invention is a sulfuric acid concentration 20%～75%, 120 ℃～250 ℃ of temperature, and equipment solves easily under this condition, is beneficial to industrialization.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1
The raw meal coal ash consists of: Al
2O
3: 41%, SiO
2: 48%, Fe
2O
3: 3.3%, CaO:3.3%, TiO
2: 1.3%, MgO:0.2%.The composition of raw meal coal ash also can adopt other constituent and concrete consumption, and the flyash of any routine is all passable, and this can not be used for limiting protection scope of the present invention.
With the flyash mechanical activation, be ground to 200 orders with vibromill, mix according to 1: 1 with water and to place acidproof autoclave, be that 1.5 the concentrated sulfuric acid places in another pressure vessel that is connected with reactor with weight ratio, the concentrated sulfuric acid is flowed in flyash and the reactor that water mixes, reactor is that liner is acid-proof ceramic tile, be heated to 180 ℃, pressure is 0.29MPa, reaction time 2h, Separation of Solid and Liquid after the reaction cooling, obtain aluminum sulfate liquid, the solid-liquid separating equipment of aluminum sulfate solution and slag adopts flocculating setting, cools off after the evaporation and concentration, separates out the aluminum sulfate crystal, the liquid aluminium sulfate evaporation and concentration adopts atmospheric evaporation, the evaporation equipment liner is organic material, gets the rear wash heat of part leaching and washs to neutrality, analyzes wherein Al
2O
3And SiO
2Content, the leaching rate of calculating aluminium oxide in the flyash reaches 88.2%, and the aluminum sulfate crystal obtains dry type aluminum sulfate at 400 ℃ of lower dehydration 3h, allocates 80% air into, and at 850 ℃ of lower calcining 3h, dry type aluminum sulfate decomposes fully, obtains γ-Al
2O
3And SO
3, SO
3The method for preparing sulfuric acid in industry absorbs with the concentrated sulfuric acid, realizes the recycling of sulfuric acid.
Thick γ-Al that calcining obtains
2O
3Under 200 ℃, use Na
2The aqueous slkali dissolved under pressure of O180g/L obtains pure sodium aluminate solution after the Separation of Solid and Liquid.Add aluminium hydroxide crystal seed in sodium aluminate solution, decompose 75 ℃ of initial temperature, 54 ℃ of temperature eventually, seed is than 2.5, caustic sodium concentration 150gl
-1, resolving time 48h separates out thick γ-Al that the alkali lye dissolving capable of circulation after evaporation concentration behind the aluminium hydroxide makes
2O
3, realize the recycle of alkali, the aluminium hydroxide of preparation obtains standard compliant metallurgical-grade aluminum oxide 1150 ℃ of calcinings.
Embodiment 2
With the raw meal coal ash mechanical activation among the embodiment 1, in vertical mill, be ground to 300 orders, mix according to 1:1.5 with water and to place acidproof autoclave, be that 2 the concentrated sulfuric acid places in another pressure vessel that is connected with reactor with weight ratio, the concentrated sulfuric acid is flowed in flyash and the reactor that water mixes, the liner of reactor is acid-proof enamel, be heated to 205 ℃, pressure is 0.35MPa, reaction time 1.5h, Separation of Solid and Liquid after the reaction cooling, obtain aluminum sulfate liquid, the solid-liquid separating equipment of aluminum sulfate solution and slag adopts pressure filtration, cools off after the evaporation and concentration, separates out the aluminum sulfate crystal, the liquid aluminium sulfate evaporation and concentration adopts reduction vaporization, the evaporation equipment liner is organic material, gets the rear wash heat of part leaching and washs to neutrality, analyzes wherein Al
2O
3And SiO
2Content, the leaching rate of calculating aluminium oxide in the flyash reaches 91.6%; The aluminum sulfate crystal obtains dry type aluminum sulfate at 400 ℃ of lower dehydration 3h.Allocate 90% air into, at 820 ℃ of lower calcining 5h, dry type aluminum sulfate decomposes fully, obtains γ-Al
2O
3And SO
3SO
3Absorb with the vitriol oil in industrial preparation vitriolic method, realize the vitriolic recycle.
Thick γ-Al that calcining obtains
2O
3Under 220 ℃, use Na
2The aqueous slkali dissolved under pressure of O150g/L obtains pure sodium aluminate solution after the Separation of Solid and Liquid.Add aluminium hydroxide crystal seed in sodium aluminate solution, decompose 80 ℃ of initial temperature, 48 ℃ of temperature eventually, seed is than 2.5, caustic sodium concentration 150gl
-1, resolving time 60h separates out thick γ-Al that the alkali lye dissolving capable of circulation after inspissation behind the aluminium hydroxide makes
2O
3, realize the recycle of alkali.The aluminium hydroxide of preparation obtains standard compliant metallurgical-grade aluminum oxide 1100 ℃ of calcinings.
Embodiment 3
With the raw material among the embodiment 1 with the flyash mechanical activation, be milled to 150 orders at the planet barreling, mix according to 1:0.5 with water and to place acidproof autoclave, with weight ratio is that 1 the vitriol oil places in another pressure vessel that is connected with reactor, after the high-pressure system sealing vitriol oil is flowed in flyash and the water blended reactor, the liner of reactor is an acid-resistant glass, is heated to 120 ℃, pressure is 0.11MPa, at insulation 8h.Reaction cooling back solid-liquid separation obtains Tai-Ace S 150 liquid, the solid-liquid separating equipment filtration under diminished pressure of alum liquor and slag, and the evaporation concentration postcooling is separated out the Tai-Ace S 150 crystal, and the liquid aluminium sulfate evaporation concentration adopts atmospheric evaporation, and the evaporation equipment liner is an organic materials.Wash heat is washed to neutrality after getting the part leaching, analyzes wherein Al
2O
3And SiO
2Content, the leaching rate of calculating aluminium oxide in the flyash reaches 85.6%.
The Tai-Ace S 150 crystal obtains dry type Tai-Ace S 150 at 400 ℃ of 2.5h that dewater down.Allocate 60% air into, at 800 ℃ of lower calcining 6h, dry type aluminum sulfate decomposes fully, obtains γ-Al
2O
3And SO
3SO
3Absorb with the vitriol oil in industrial preparation vitriolic method, realize the vitriolic recycle.
Thick γ-Al that calcining obtains
2O
3Under 120 ℃, use Na
2The aqueous slkali dissolved under pressure of O200g/L obtains pure sodium aluminate solution after the Separation of Solid and Liquid.Add aluminium hydroxide crystal seed in sodium aluminate solution, decompose 75 ℃ of initial temperature, 54 ℃ of temperature eventually, seed is than 2.5, caustic sodium concentration 150gl
-1, resolving time 48h separates out thick γ-Al that the alkali lye dissolving capable of circulation after inspissation behind the aluminium hydroxide makes
2O
3, realize the recycle of alkali.The aluminium hydroxide of preparation obtains standard compliant metallurgical-grade aluminum oxide 1000 ℃ of calcinings.
Embodiment 4
With the raw material powder coal ash mechanical activation among the embodiment 1, be ground to 500 orders at high-energy ball milling, mix according to 1:2.5 with water and to place acidproof autoclave, with weight ratio is that 3.5 the vitriol oil places in another pressure vessel that is connected with reactor, after the high-pressure system sealing vitriol oil is flowed in flyash and the water blended reactor, the liner of reactor is acidproof fluoroplastics, is heated to 250 ℃, pressure is 0.5MPa, at insulation 1h.Reaction cooling back solid-liquid separation obtains Tai-Ace S 150 liquid, and the solid-liquid separating equipment of alum liquor and slag adopts flocculating settling, the evaporation concentration postcooling, separate out the Tai-Ace S 150 crystal, the liquid aluminium sulfate evaporation concentration adopts atmospheric evaporation, and the evaporation equipment liner is an organic materials.Wash heat is washed to neutrality after getting the part leaching, analyzes wherein Al
2O
3And SiO
2Content, the leaching rate of calculating aluminium oxide in the flyash reaches 93.5%.
The Tai-Ace S 150 crystal obtains dry type Tai-Ace S 150 at 400 ℃ of 2.5h that dewater down.Allocate 90% air into, at 800 ℃ of lower calcining 6h, dry type aluminum sulfate decomposes fully, obtains γ-Al
2O
3And SO
3SO
3Absorb with the vitriol oil in industrial preparation vitriolic method, realize the vitriolic recycle.
Thick γ-Al that calcining obtains
2O
3Under 200 ℃, use Na
2The aqueous slkali dissolved under pressure of O180g/L obtains pure sodium aluminate solution after the Separation of Solid and Liquid.Add aluminium hydroxide crystal seed in sodium aluminate solution, decompose 75 ℃ of initial temperature, 54 ℃ of temperature eventually, seed is than 2.5, caustic sodium concentration 150gl
-1, resolving time 48h separates out thick γ-Al that the alkali lye dissolving capable of circulation after inspissation behind the aluminium hydroxide makes
2O
3, realize the recycle of alkali.The aluminium hydroxide of preparation obtains standard compliant metallurgical-grade aluminum oxide 1200 ℃ of calcinings.
Embodiment 5
The liner of the reactor among the embodiment 1 is acidproof tetrafluoroethylene, and other is with embodiment 1.
Claims (13)
1, a kind of fly-ash Preparation method of alumina of utilizing is characterized in that comprising the steps:
With the flyash mechanical activation;
Flyash behind the mechanical activation is mixed according to 1:0.5～2.5 with water, add weight ratio and be 1～3.5 the vitriol oil in reaction kettle for reaction, be heated to 120 ℃～250 ℃, pressure is 0.11MPa～0.5MPa, reaction times 1h～8h;
Reaction cooling back solid-liquid separation obtains Tai-Ace S 150 liquid, and the evaporation concentration postcooling is separated out the Tai-Ace S 150 crystal;
The dehydration of Tai-Ace S 150 crystal obtains dry type Tai-Ace S 150;
The decomposition of dry type aluminum sulfate obtains γ-Al
2O
3And SO
3
With thick γ-Al
2O
3In aqueous slkali, dissolve, obtain pure sodium aluminate solution after the Separation of Solid and Liquid;
Add aluminium hydroxide crystal seed in the sodium aluminate solution and separate out aluminium hydroxide, plant thick γ-Al that the alkali lye dissolving capable of circulation after inspissation after dividing makes
2O
3
The aluminium hydroxide calcining of preparation obtains metallurgical-grade aluminum oxide.
2, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1 is characterized in that described mechanical activation is a kind of grinding of adopting in vibration mill, vertical mill, planetary mills or the high-energy ball milling, is ground to the 100-800 order.
3, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1, the liner that it is characterized in that described reactor are a kind of in acid-proof ceramic tile, enamel, glass, fluoroplastics, the tetrafluoroethylene.
4, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1, it is characterized in that described flyash and acid-respons after, the solid-liquid separation of alum liquor and slag adopts a kind of in flocculating settling, pressure filtration or the filtration under diminished pressure.
5, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1 is characterized in that described liquid aluminium sulfate evaporation concentration adopts normal pressure or reduction vaporization.
6, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1 is characterized in that described Tai-Ace S 150 crystal dehydration is to obtain dry type Tai-Ace S 150 200 ℃ of-400 ℃ of calcinings.
7, a kind of method of utilizing the standby aluminium oxide of coal ash for manufacturing according to claim 6 is characterized in that described dry type aluminum sulfate under 500-900 ℃ of temperature, adds 60%～90% air, and calcining obtains γ-Al
2O
3And SO
3
8, according to claim 1 or 7 described a kind of methods of utilizing the standby aluminium oxide of coal ash for manufacturing, it is characterized in that described SO
3Absorb preparation sulfuric acid with the concentrated sulfuric acid.
9, according to claim 1 or 7 described a kind of methods of utilizing the standby aluminium oxide of coal ash for manufacturing, it is characterized in that described γ-Al
2O
3Contain impurity, with thick γ-Al
2O
3Under 120 ℃～260 ℃, use Na
2The aqueous slkali dissolved under pressure of O150g/L～200g/L, aluminium enter liquid phase and form sodium aluminate solution, in impurity existence and the solid phase, obtain pure sodium aluminate solution after the Separation of Solid and Liquid.
10, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1 is characterized in that the described aluminium hydroxide crystal seed that adds in sodium aluminate solution, presses bayer process condition decomposition of crystal seed, obtains aluminium hydroxide.
11, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1 is characterized in that described aluminium hydroxide 1000 ℃～1200 ℃ calcinings down, obtains metallurgical-grade aluminum oxide.
12, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1 is characterized in that the sulfuric acid concentration of the described vitriol oil in reactor reduce to 20%-75%.
13, a kind of fly-ash Preparation method of alumina of utilizing according to claim 1, it is characterized in that described flyash and water add in the reactor, the vitriol oil joins in the pressure vessel of reactor connection, after the high-pressure system sealing vitriol oil is flowed in flyash and the water blended reactor.
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| CN102020299A (en) * | 2010-12-23 | 2011-04-20 | 南京航空航天大学 | Method for producing industrial activated aluminum oxide from pulverized fuel ash |
| CN102398913A (en) * | 2010-09-14 | 2012-04-04 | 贵阳铝镁设计研究院有限公司 | Process for extracting metallurgical grade alumina through treatment of high alumina fly ash by using sulfuric acid method |
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| CN102515227A (en) * | 2011-12-23 | 2012-06-27 | 西安航天科技工业公司 | Method for extracting alumina from fly ash based on grinding and acid leaching technology |
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| CN103936040A (en) * | 2013-01-18 | 2014-07-23 | 新疆大学 | Ultrasonic wave acid method for extracting aluminum oxide from fly ash |
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| CN104787789B (en) * | 2015-01-15 | 2016-03-30 | 北京矿冶研究总院 | Method for producing alumina by using coal-based solid waste |
| CN107055582A (en) * | 2016-12-15 | 2017-08-18 | 中国恩菲工程技术有限公司 | The system of Aluminum from flyash |
| CN107055582B (en) * | 2016-12-15 | 2021-10-22 | 中国恩菲工程技术有限公司 | System for dissolve out aluminium from fly ash |
| CN107385224A (en) * | 2017-08-04 | 2017-11-24 | 攀钢集团研究院有限公司 | It is a kind of that the method that aluminium is reclaimed in corundum slag is smelted from vanadium iron |
| CN107385224B (en) * | 2017-08-04 | 2019-04-26 | 攀钢集团研究院有限公司 | A method of it is smelted from vanadium iron and recycles aluminium in corundum slag |
| CN108950603A (en) * | 2018-08-31 | 2018-12-07 | 营口忠旺铝业有限公司 | A kind of method for electrolyzing aluminum improving electrolyte dissolution degree |
| CN115591517A (en) * | 2022-09-19 | 2023-01-13 | 山东科技大学（Cn） | Rice hull ash/fly ash-based adsorbent, preparation method and application thereof |
| CN115591517B (en) * | 2022-09-19 | 2024-02-02 | 山东科技大学 | Rice hull ash/fly ash-based adsorbent, preparation method and application thereof |
| CN117205908A (en) * | 2023-11-09 | 2023-12-12 | 上海银锅环保科技有限公司 | Alumina and calcium silicate composite catalyst and preparation method and application thereof |
| CN117205908B (en) * | 2023-11-09 | 2024-02-27 | 上海银锅环保科技有限公司 | Alumina and calcium silicate composite catalyst and preparation method and application thereof |
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