CN102502735A - Method for producing alumina by using pulverized fuel ash - Google Patents
Method for producing alumina by using pulverized fuel ash Download PDFInfo
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- CN102502735A CN102502735A CN2011103426286A CN201110342628A CN102502735A CN 102502735 A CN102502735 A CN 102502735A CN 2011103426286 A CN2011103426286 A CN 2011103426286A CN 201110342628 A CN201110342628 A CN 201110342628A CN 102502735 A CN102502735 A CN 102502735A
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Abstract
The invention relates to a method for preparing alumina by using pulverized fuel ash. The method comprises the following steps of: (1) preparing raw meal; (2) baking clinker; (3) recovering ammonia gas; (4) dissolving the clinker out; (5) separating and washing high-silicon residues; (6) preparing alumina with an obtained aluminum sulfate solution; and (7) evaporating an ammonia sulfate solution. The method has the advantages and effects that: no aid is added, so that alumina in pulverized fuel ash can be extracted effectively, and the extraction ratio of alumina can be over 85 percent. In the process flow of the method, circulation of ammonia sulfate is realized, so that alumina can be extracted from pulverized fuel ash in batches by circulating; no waste gas or waste liquid is discharged in an entire process; and a major component in residues left by extraction of alumina from pulverized fuel ash is carbon dioxide which is easy to utilize. A reaction system is a weakly acid system, equipment is easy to handle, and industrialization is facilitated.
Description
Technical field
The present invention relates to a kind of industrial solid castoff production method of alumina of utilizing, 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.China's flyash annual emissions in 2010 is up to 3.5 hundred million tons, and total volume of cargo in storage of China's flyash has more than 50 hundred million 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 constituted the dual destruction to ecological and environment.Therefore the comprehensive utilization of carrying out flyash has great realistic meaning and long-range strategic importance.Equally, China is the not rich country of a bauxite resource, and by the rate of growth and the bauxite recovery rate of present aluminum oxide output, even consider prospective reserves, the time limit of the bauxite of China also is difficult to reach 30 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 staple of flyash, and its massfraction is generally 10% ~ 40%, reaches as high as 58%.So, carry out from flyash the pollution that the research work of extracting aluminum 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, employing be exactly improved soda-lime sintering process.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 facility investment of sintering process processing flyash is big, and energy consumption is high, and cost is high.
Because the alumina silica ratio of flyash is very low, generally all less than 1, so adopt acidic process flyash more reasonable in principle.Aluminum oxide in acid or acidic cpd and the flyash reacts the aluminium salt that generates, and aluminium salt dissolving back gets into solution, and silicon does not react with acid or acidic cpd, 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 alumina extraction ratio 85%) in the slag, so more helps its utilization.It is feasible on principle that acid system (comprising sulfuric acid process and salt acid system) is handled flyash production aluminum oxide, but because acid has severe corrosive, equipment and its large-scale application of Corrosion of Pipeline problem restriction.
Adopt the ammonium sulfate sintering process to handle flyash and extract the direction that aluminum oxide has become vast researcher research; Adopting ammonium sulfate is that circulatory mediator does not add extra increment material; Silicon-dioxide meeting enrichment in the same slag with acid system; But do not have strong corrosive material in the whole technological process, be easy to industrialization promotion.
Summary of the invention
For solving the problems of the technologies described above the present invention a kind of fly-ash Preparation method of alumina of utilizing is provided, does not add any auxiliary agent, alumina extraction ratio is high in the flyash, and the ammonium sulfate cycle efficiency is high.
For realizing a kind of fly-ash Preparation method of alumina of utilizing of above-mentioned purpose the present invention; It comprises the steps: the preparation of (1) raw material: flyash and ammonium sulfate are mixed and made into raw material, and wherein the weight ratio of the aluminum oxide in ammonium sulfate and the flyash is 4.5～8:1; (2) grog burns till: raw material are heated to 350 ~ 700 ℃, and firing time is controlled at 0.5 ~ 5h, processes the grog and the ammonia of sulfur acid aluminium, and ammonia is used to prepare ammoniacal liquor or feeds the Tai-Ace S 150 decomposition process; (3) ammonia reclaims: adopt water or washing lotion to absorb the ammonia of grog sintering process generation and the CO that decomposition produces with alum liquor that grog burns till generation
2, form ammonium salt; (4) grog stripping: grog is used the hot water stripping, dissolution time 0.1 ~ 2h, and aluminium gets into solution with the form of Tai-Ace S 150, and silicon is stayed and is formed high white residue in the residue; (5) high white residue separating, washing: the slurries after the stripping carry out solid-liquid separation and countercurrent washing, and solution is alum liquor, and washing the back slag is high white residue; (6) alum liquor that obtains prepares aluminum oxide; (7) ammoniumsulphate soln evaporation: separate the ammoniumsulphate soln that obtains and evaporate, obtain being fit to the ammoniumsulphate soln or the ammonia sulfate crystal of batching.
The described alum liquor that obtains prepares aluminum oxide: add the ammonium salt that the ammonia recovery process obtains to alum liquor, obtain white lake, ironic hydroxide, ammoniumsulphate soln and CO
2Gas, solid are the many thick white lake of foreign matter content; Thick white lake carries out the low temperature Bayer process with the circulation alkaline solution to be handled, and removes wherein iron, calcium impurities, obtains aluminum oxide and high scum.
The described alum liquor that obtains prepares aluminum oxide: add ammonium salt adjusting pH value fractional precipitation ironic hydroxide and the white lake that the ammonia recovery process obtains to alum liquor; The pH value is 1.5 ~ 3.5 deposition ironic hydroxides; After isolating high scum, continue in solution, to add ammonium salt and obtain white lake, ammoniumsulphate soln and CO
2Gas, white lake obtains the finished product aluminum oxide 900 ~ 1300 ℃ of following roastings.
The described alum liquor that obtains prepares aluminum oxide: alum liquor is through the multi-stage counter current extraction deironing, and the alum liquor after deironing adds the ammonium salt that the ammonia recovery process obtains, and obtains white lake, ammoniumsulphate soln and CO
2Gas, white lake obtains the finished product aluminum oxide 900 ~ 1300 ℃ of following roastings.
The described alum liquor that obtains prepares aluminum oxide: alum liquor is through the ion exchange resin deironing, and the alum liquor after deironing adds the ammonium salt that the ammonia recovery process obtains, and obtains white lake, ammoniumsulphate soln and CO
2Gas, white lake obtains the finished product aluminum oxide 900 ~ 1300 ℃ of following roastings.
The preparation of described raw material is to adopt a kind of in dry method batch mixing or the material by wet type mixing; The staple of described high white residue is a silicon-dioxide, is used to prepare silicon series product or high silicon fillers such as WHITE CARBON BLACK.
Described employing Bayer process is handled thick white lake for producing the full bayer process flow process of aluminum oxide, comprises raw pulp allotment, low temperature stripping, red mud separating, washing, sodium aluminate solution decomposition, white lake separating, washing and Aluminium hydroxide roasting operation.
The extraction agent that described alum liquor extraction deironing is adopted is a kind of in lipid acid, primary amine or the tertiary amine;
Anionite-exchange resin that described ion exchange resin deironing is adopted or Zeo-karb a kind of;
Described high scum or ironic hydroxide can be used as iron-smelting raw material.
Advantageous effect of the present invention: the present invention does not add any auxiliary agent, can effectively extract aluminum oxide in the flyash, and the extraction yield of aluminum oxide can reach more than 85%.Realized the ammonium sulfate circulation in the technical process of the present invention, through circulation can be many batches of extraction flyash in aluminum oxide, whole process does not have the discharge of waste gas, waste liquid, the residue staple that flyash extracts behind the aluminum oxide is a silicon-dioxide, is easy to utilize.Reaction system of the present invention is a weak acid system, and equipment solves easily, is beneficial to industrialization.
Description of drawings
Fig. 1 ~ Fig. 4 is a process flow sheet of the present invention.
Embodiment
Embodiment 1
The raw material powder coal ash consists of: Al
2O
3: SiO 41%,
2: Fe 48%,
2O
3: 3.3%, CaO:3.3%, TiO
2: MgO:0.2% 1.3%.The composition of raw material powder coal ash also can adopt other moity, and this can not be used to limit protection scope of the present invention.
Get the flyash of the above-mentioned composition of 1000g, flyash is obtained raw material with ammoniumsulphate soln mixing wet-milling, wherein the weight ratio of the aluminum oxide in ammonium sulfate and the flyash is 5:1; Raw material are heated to 450 ℃, and insulation 1h processes grog, and water absorbs ammonia, the CO that discharges
2Decompose the CO that produces with alum liquor
2Process ammonium salt, be used for Tai-Ace S 150 and decompose; Grog is stripping 0.5h in hot water, and aluminium gets into solution with the form of Tai-Ace S 150, and silicon is stayed and formed high white residue in the residue; The stripping rear slurry is through solid-liquid separation and countercurrent washing, and liquid is alum liquor, and solid is high white residue; In alum liquor, add ammonia and reclaim the ammonium salt that obtains, make aluminium, iron deposition in the solution become rough white lake, liquid is ammoniumsulphate soln, and gas is CO
2Rough aluminum hydroxide slurry separating, washing obtains rough white lake solid and ammoniumsulphate soln; Ammoniumsulphate soln returns the raw material preparation after evaporation, recycle; Roughly carry out the low temperature Bayer process with the circulation alkaline solution and handle, remove wherein impurity such as iron, calcium, obtain aluminum oxide and high scum.Bayer process is handled thick white lake for producing the full bayer process flow process of aluminum oxide, comprises raw pulp allotment, low temperature stripping, red mud separating, washing, sodium aluminate solution decomposition, white lake separating, washing and Aluminium hydroxide roasting operation.
Embodiment 2
Get the raw material powder coal ash of forming among the 1000g embodiment 1, raw material powder coal ash and ammonium sulfate circulation fluid material by wet type mixing are obtained raw material, wherein the weight ratio of the aluminum oxide in ammonium sulfate and the flyash is 6:1; Raw material are heated to 500 ℃, and insulation 3h processes grog, and water absorbs ammonia, the CO that discharges
2Decompose the CO that produces with alum liquor
2Process ammonium salt, be used for Tai-Ace S 150 and decompose; Grog is stripping 1h in hot water, and aluminium gets into solution with the form of Tai-Ace S 150, and silicon is stayed and formed high white residue in the residue; The stripping rear slurry is through solid-liquid separation and countercurrent washing, and liquid is alum liquor, and solid is high white residue; In alum liquor, add ammonia and reclaim the ammonium salt that obtains, regulate pH value to 2.5 deposition ironic hydroxide, isolate high scum after, continue that the adding ammonium salt obtains white lake, ammoniumsulphate soln and CO in alum liquor
2, ammoniumsulphate soln returns the raw material preparation after evaporation, recycle; White lake obtains the finished product aluminum oxide 1150 ℃ of following roastings.
Embodiment 3
Get the raw material powder coal ash of forming among the 1000g embodiment 1, raw material powder coal ash and ammonium sulfate circulation fluid material by wet type mixing are obtained raw material, wherein the weight ratio of the aluminum oxide in ammonium sulfate and the flyash is 7:1; Raw material are heated to 350 ℃, and insulation 5h processes grog, absorbs ammonia, the CO that discharges with washing lotion
2Decompose the CO that produces with alum liquor
2Process ammonium salt, be used for Tai-Ace S 150 and decompose; Grog is stripping 2h in hot water, and aluminium gets into solution with the form of Tai-Ace S 150, and silicon is stayed and formed high white residue in the residue; The stripping rear slurry is through solid-liquid separation and countercurrent washing, and liquid is alum liquor, and solid is high white residue; Alum liquor adopts lipid acid extraction deironing through multi-stage countercurrent, and the alum liquor after deironing adds the ammonium salt that the ammonia recovery process obtains, and obtains white lake, ammoniumsulphate soln and CO
2, ammoniumsulphate soln returns the raw material preparation after evaporation, recycle; White lake obtains the finished product aluminum oxide 1200 ℃ of following roastings.
Embodiment 4
Alum liquor extraction iron removal employing primary amine is an extraction agent among the embodiment 3, and other is identical with embodiment 4.
Embodiment 5
Alum liquor extraction iron removal employing tertiary amine is an extraction agent among the embodiment 3, and white lake obtains the finished product aluminum oxide 900 ℃ of following roastings, and other is identical with embodiment 4.
Embodiment 6
Get the raw material powder coal ash of forming among the 1000g embodiment 1, raw material powder coal ash and ammonium sulfate circulation fluid material by wet type mixing are obtained raw material, wherein the weight ratio of the aluminum oxide in ammonium sulfate and the flyash is 8:1; Raw material are heated to 700 ℃, and insulation 0.5h processes grog, and water absorbs ammonia, the CO that discharges
2Decompose the CO that produces with Tai-Ace S 150
2Process ammonium salt, be used for Tai-Ace S 150 and decompose; Grog is stripping 0.1h in hot water, and aluminium gets into solution with the form of Tai-Ace S 150, and silicon is stayed and formed high white residue in the residue; The stripping rear slurry is through solid-liquid separation and countercurrent washing, and liquid is alum liquor, and solid is high white residue; Alum liquor is through the Zeo-karb deironing, and the alum liquor after deironing adds the ammonium salt that the ammonia recovery process obtains, and obtains white lake, ammoniumsulphate soln and CO
2, ammoniumsulphate soln returns the raw material preparation after evaporation, recycle; White lake obtains the finished product aluminum oxide 1200 ℃ of following roastings.
Embodiment 7
Absorb ammonia, the CO that discharges with high white residue washing lotion among the embodiment 6
2Decompose the CO that produces with alum liquor
2Process ammonium salt; Alum liquor adopts the anionite-exchange resin deironing, and other is identical with embodiment 6.
Embodiment 8
The ammonium sulfate among the embodiment 2 and the weight ratio of the aluminum oxide in the flyash are 4.5:1; In alum liquor, add ammonia and reclaim the ammonium salt that obtains, regulate pH value to 1.5 deposition ironic hydroxide, white lake obtains the finished product aluminum oxide 1300 ℃ of following roastings, and other is with embodiment 2.
Embodiment 9
The ammonia that in alum liquor, adds among the embodiment 2 reclaims the ammonium salt that obtains, and regulates pH value to 3.5 deposition ironic hydroxide, and other is with embodiment 2.
Claims (10)
1. utilize flyash production method of alumina, it is characterized in that comprising the steps:
(1) raw material preparation: flyash and ammonium sulfate are mixed and made into raw material, and wherein the weight ratio of the aluminum oxide in ammonium sulfate and the flyash is 4.5～8:1;
(2) grog burns till: raw material are heated to 350 ~ 700 ℃, and firing time is controlled at 0.5 ~ 5h, processes the grog and the ammonia of sulfur acid aluminium, and ammonia is used to prepare ammoniacal liquor or feeds the Tai-Ace S 150 decomposition process;
(3) ammonia reclaims: adopt water or washing lotion to absorb the ammonia of grog sintering process generation and the CO that decomposition produces with alum liquor that grog burns till generation
2, form ammonium salt;
(4) grog stripping: grog is used the hot water stripping, dissolution time 0.1 ~ 2h, and aluminium gets into solution with the form of Tai-Ace S 150, and silicon is stayed and is formed high white residue in the residue;
(5) high white residue separating, washing: the slurries after the stripping carry out solid-liquid separation and countercurrent washing, and solution is alum liquor, and washing the back slag is high white residue;
(6) alum liquor that obtains prepares aluminum oxide;
(7) ammoniumsulphate soln evaporation: separate the ammoniumsulphate soln that obtains and evaporate, obtain being fit to the ammoniumsulphate soln or the ammonia sulfate crystal of batching.
2. the flyash production method of alumina of utilizing according to claim 1; It is characterized in that the described alum liquor that obtains prepares aluminum oxide and is: add the ammonium salt that the ammonia recovery process obtains to alum liquor, obtain white lake, ironic hydroxide, ammoniumsulphate soln and CO
2Gas, solid are the many thick white lake of foreign matter content; Thick white lake carries out the low temperature Bayer process with the circulation alkaline solution to be handled, and removes wherein iron, calcium impurities, obtains aluminum oxide and high scum.
3. the flyash production method of alumina of utilizing according to claim 1; It is characterized in that the described alum liquor that obtains prepares aluminum oxide and is: add ammonium salt adjusting pH value fractional precipitation ironic hydroxide and the white lake that the ammonia recovery process obtains to alum liquor; The pH value is 1.5 ~ 3.5 deposition ironic hydroxides; After isolating high scum, continue in solution, to add ammonium salt and obtain white lake, ammoniumsulphate soln and CO
2Gas, white lake obtains the finished product aluminum oxide 900 ~ 1300 ℃ of following roastings.
4. the flyash production method of alumina of utilizing according to claim 1; It is characterized in that the described alum liquor that obtains prepares aluminum oxide and is: alum liquor is through the multi-stage counter current extraction deironing; Alum liquor after deironing adds the ammonium salt that the ammonia recovery process obtains, and obtains white lake, ammoniumsulphate soln and CO
2Gas, white lake obtains the finished product aluminum oxide 900 ~ 1300 ℃ of following roastings.
5. the flyash production method of alumina of utilizing according to claim 1; It is characterized in that the described alum liquor that obtains prepares aluminum oxide and is: alum liquor is through the ion exchange resin deironing; Alum liquor after deironing adds the ammonium salt that the ammonia recovery process obtains, and obtains white lake, ammoniumsulphate soln and CO
2Gas, white lake obtains the finished product aluminum oxide 900 ~ 1300 ℃ of following roastings.
6. the flyash production method of alumina of utilizing according to claim 1 is characterized in that the preparation of described raw material is to adopt a kind of in dry method batch mixing or the material by wet type mixing; The staple of described high white residue is a silicon-dioxide, is used to prepare silicon series product or high silicon fillers such as WHITE CARBON BLACK.
7. the flyash production method of alumina of utilizing according to claim 2; It is characterized in that it is the full bayer process flow process of producing aluminum oxide that described employing Bayer process is handled thick white lake, comprises raw pulp allotment, low temperature stripping, red mud separating, washing, sodium aluminate solution decomposition, white lake separating, washing and Aluminium hydroxide roasting operation.
8. the flyash production method of alumina of utilizing according to claim 4 is characterized in that extraction agent that described alum liquor extraction deironing is adopted is a kind of in lipid acid, primary amine or the tertiary amine.
9. the flyash production method of alumina of utilizing according to claim 5 is characterized in that a kind of of anionite-exchange resin that described ion exchange resin deironing is adopted or Zeo-karb.
10. according to claim 2 or the 3 described fly-ash Preparation method of alumina of utilizing, it is characterized in that the iron-smelting raw material that can be used as of described high scum or ironic hydroxide.
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| WO2013040862A1 (en) * | 2011-09-24 | 2013-03-28 | 中铝国际工程股份有限公司 | Method for producing aluminium oxide by processing fly ash with ammonia process |
| CN103342376A (en) * | 2013-07-11 | 2013-10-09 | 中北大学 | Process for extracting valuable metal from coal gangues |
| CN103848447A (en) * | 2012-11-28 | 2014-06-11 | 沈阳铝镁设计研究院有限公司 | Fly ash raw material pellet production method |
| CN103936048A (en) * | 2013-01-18 | 2014-07-23 | 新疆大学 | Method for recovering and utilizing sewage generated during technology process of acid method for extracting aluminum oxide from fly ash |
| CN104030329A (en) * | 2013-07-04 | 2014-09-10 | 沈阳工业大学 | Method for comprehensively using aluminum-containing resource |
| CN104098116A (en) * | 2013-04-12 | 2014-10-15 | 沈阳铝镁设计研究院有限公司 | Roasting clinker dissolve-out method in fly ash and ammonium sulfate mixed roasting technology |
| CN104609451A (en) * | 2015-01-30 | 2015-05-13 | 魏子贺 | Process for preparing aluminum oxide by virtue of dry-sintering method |
| CN105753026A (en) * | 2016-04-11 | 2016-07-13 | 北京世纪地和控股有限公司 | Method for recycling aluminum oxide from coal ash |
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| CN104609451A (en) * | 2015-01-30 | 2015-05-13 | 魏子贺 | Process for preparing aluminum oxide by virtue of dry-sintering method |
| CN105753026A (en) * | 2016-04-11 | 2016-07-13 | 北京世纪地和控股有限公司 | Method for recycling aluminum oxide from coal ash |
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