CN103086412A - Method for extracting alumina through coal ash - Google Patents
Method for extracting alumina through coal ash Download PDFInfo
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- CN103086412A CN103086412A CN2013100629220A CN201310062922A CN103086412A CN 103086412 A CN103086412 A CN 103086412A CN 2013100629220 A CN2013100629220 A CN 2013100629220A CN 201310062922 A CN201310062922 A CN 201310062922A CN 103086412 A CN103086412 A CN 103086412A
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- ammonium sulfate
- flyash
- roasting
- coal ash
- temperature
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Abstract
The invention particularly discloses a method for extracting alumina through coal ash. The method comprises the following steps of: (1) respectively finely grinding and activating the coal ash and finely grinding ammonium sulfate in order to increase the superficial area; (2) carrying out solid-to-solid mixing on the finely ground coal ash and the ammonium sulfate (on the basis of Al2O3: (NH4)2SO4=1: 3 to 6 (molar ratio) in the coal ash) until reaching the consistency; (3) adding a certain rate of water to the mixed and consistent raw materials in the step (2), which is a mixture of the coal ash and the ammonium sulfate, and granulating; (4) placing the particles in the step (3) into roasting equipment to roast, wherein a two-section temperature control method is carried out in the roasting process; (5) adding the roasted clinker to the water to dissolve into solution; (6) filtering the solution prepared in the step (5), and respectively collecting the filter residue and the filtrate; (7) adding ammonia water to the filtrate in the step (6) to obtain Al(OH3) sediment; and (8) roasting Al(OH3)3 to obtain the Al2O3 product.
Description
Technical field
The invention belongs to the total utilization of PCA field, particularly a kind of method of making the raw material production aluminum oxide of flyash.
Background technology
The a large amount of flyash of the annual generation of China's thermal power generation, sub-fraction wherein is used for building and cement industry, and remaining flyash need to be piled up with the ash field, take a large amount of soils, and contaminate environment.Contain Al on the composition of flyash
2O
320%～50%, SiO
220%～60%, all the other also have a small amount of Fe
2O
3, MgO, Na
2O, K
2The compounds such as O.Meanwhile, along with the development of China's economic society, a large amount of bauxite of annual import is to make up the deficiency of domestic bauxite.Therefore, aluminum oxide is extracted in research from flyash, and is all significant with the comprehensive utilization value that improves flyash to the Sustainable development of national alumina industry.
At present, the method for extraction aluminum oxide mainly contains four kinds, alkali solution technique, acid pasting, using acid and alkali combination method and ammonium sulfate method from flyash.Wherein alkali solution technique is not suitable for high silicon powder-containing coal ash, and another alkali solution technique, acid pasting and using acid and alkali combination method all need soda acid, have increased on the one hand the burden of subsequent disposal, on the other hand easy contaminate environment.The ammonium sulfate method adopts the aluminum oxide in ammonium sulfate and flyash calcination activation flyash, and then stripping exsiccated ammonium alum and Tai-Ace S 150, drip alkaline solution and generate Al (OH)
3Precipitation, last roasting Al (OH)
3Get Al
2O
3The shortcoming of existing ammonium sulfate method is that roasting time is long, exsiccated ammonium alum recrystallization energy consumption is large, process in leaching needs acid adding etc.
A kind of method of extracting aluminum oxide from flyash is disclosed in patent [CN201110208699.7], but direct roasting technique after the method adopts ammonium sulfate to mix with flyash, intrinsic heat character due to ammonium sulfate, melting phenomenon can occur between 260 ℃ to 450 ℃, bring thus ammonium sulfate and mixture of fly ash to adhesion, the bonding of reactor wall, thereby the larger temperature field of formation gradient in reactor, the mixture on wall does not heat up difficult, result is that alumina extraction ratio reduces or the reaction times extends, and affects production efficiency.
A kind of method of aluminum oxide of extracting from flyash based on ammonium sulfate activation process is disclosed in patent [CN201210060558.X], the method is taked after flyash and ammonium sulfate granulation two-stage roasting technique in fluidized-bed, although this patent is claimed technical problems such as having solved material melting sticking wall, caking and ring formation, but consider according to the fluidization principle, flyash and ammonium sulfate particle that mixture is made can be emitted H always in the fluosolids roasting process
2O, NH
3, SO
2And SO
3Deng gas, form, the density of particle change, and can cause the fluidization quality variation, even particle collision occurs and are bonded together, and phenomenon that can't fluidisation can make production process normally carry out in practice.This method adopts dilute sulphuric acid stripping grog in addition, and environment protection is had certain influence.
Summary of the invention
The defective that exists in order to overcome prior art the invention provides a kind of method of being extracted aluminum oxide by flyash.
The technical solution used in the present invention is as follows:
A kind of flyash extracts the method for aluminum oxide, comprises the following steps:
Step (1) is with the levigate activation of flyash, ammonium sulfate is levigate, to increase the surface-area of flyash and ammonium sulfate;
Step (2) is with the flyash after levigate and ammonium sulfate, in molar ratio with Al in flyash
2O
3: (NH
4)
2SO
4=1:3～6 are mixed to homogeneous admittedly;
Step (3) namely adds entry, granulation in flyash and ammonium sulfate mixture in the raw material that mixes homogeneous;
Step (4) is placed in the roasting apparatus roasting with particle described in step (3), calcination procedure adopts two sections method of temperature-control by, described two sections method of temperature-control by comprise respectively low-temperature zone roasting and high temperature section roasting, acting as of low-temperature zone roasting makes ammonium sulfate and the sclerosis of mixture of fly ash particle surface, control particle shape, the low-temperature zone maturing temperature is selected 350 ℃～390 ℃; The high temperature section roasting act as the increase chemical reaction rate, reduce the reaction times, the high temperature section maturing temperature is selected 390 ℃～450 ℃;
Step (5) is put into water with roasting who knows and is dissolved into solution;
The solution that step (6) filtration step (5) is made is collected respectively filter residue and filtrate;
Step (7) adds ammoniacal liquor in the middle filtrate of collecting of step (6), obtain Al (OH)
3Precipitation;
Step (8) is to Al (OH)
3Calcining obtains Al
2O
3Product.
In aforesaid method, the flyash of described step (1) and the levigate granularity of ammonium sulfate are 100 orders～200 orders.
In aforesaid method, the water that adds in described step (3) is tap water or pure water, and the quality that adds entry accounts for 5～15% of flyash and ammonium sulfate mixture quality.
In aforesaid method, in step (5), dissolving adds entry when who knows amount is to who knows 2～6 times of quality, and solvent temperature is 80～100 ℃, and dissolution time is 20min～90min.
In aforesaid method, in step (7), the amount that adds ammoniacal liquor is 3～6 times of aluminum ion mole number.
Be rotary kiln or revolving drum at the described roasting apparatus of step (4), be the chemical industry rotary kiln.
The invention has the beneficial effects as follows:
Granulation step in the present invention can promote the close contact between flyash and ammonium sulfate, and enhance heat transfer, response capacity can also partly solve to improve the yield of aluminum oxide in grog the adhesivity that material produces in reaction process.The part moisture that adds in the particle that causes is separated out in the low-temperature zone of reaction, and granule interior and surface can form tiny duct, and what be conducive to resultant in reaction process separates out to improve yield that who knows middle aluminum oxide.Two sections method of temperature-control by comprise that the reactant particle keeps certain hour in low-temperature zone, partly react so that the moisture in particle is separated out fast with ammonium sulfate, and the silicon-dioxide in flyash is bonded together, and make material particles keep definite shape; In high temperature section, the aluminum oxide generation solid-solid reaction in ammonium sulfate and flyash, high temperature are conducive to reaction and accelerate, Reaction time shorten.The present invention has solved with practice material adhesivity, long reaction time, reaction control and the engineering scale-up problem that ammonium sulfate method extract powder coal ash, aluminum oxide runs on principle.Description of drawings
Fig. 1 is the schematic flow sheet of embodiments of the invention.
Embodiment
Describe embodiments of the invention in detail below in conjunction with accompanying drawing:
Method of the present invention comprises the following steps:
Step (1) is levigate to increase this surface-area with the levigate activation of flyash and ammonium sulfate respectively;
Step (2) (is pressed Al in flyash with the flyash after levigate and ammonium sulfate
2O
3: (NH
4)
2SO
4=1:3～6 (mol ratio)) admittedly be mixed to homogeneous;
Step (3) namely adds entry, granulation in flyash and ammonium sulfate mixture in the raw material that mixes homogeneous;
Step (4) is placed in the roasting apparatus roasting with particle described in step (3);
Step (5) is put into water with roasting who knows and is dissolved into solution;
The solution that step (6) filtration step (5) is made is collected respectively filter residue and filtrate;
Step (7) adds ammoniacal liquor to the filtrate in step (6), can get Al (OH)
3Precipitation;
Step (8) is to Al (OH)
3Calcining can get Al
2O
3Product.
In aforesaid method, the flyash of described step (1) and the levigate granularity of ammonium sulfate are 100 orders～200 orders.
In aforesaid method, the water that adds in described step (3) is tap water or pure water, and the quality that adds accounts for 5～15% of flyash and ammonium sulfate mixture quality.
In aforesaid method, in step (4), the preferred two sections method of temperature-control by of calcination procedure, be respectively low-temperature zone roasting and high temperature section roasting, acting as of low-temperature zone roasting makes ammonium sulfate and the sclerosis of mixture of fly ash particle surface, controls particle shape, 350 ℃～390 ℃ of low-temperature zone maturing temperatures; The high temperature section roasting act as the increase chemical reaction rate, reduce the reaction times, 390 ℃～450 ℃ of high temperature section maturing temperatures.
In aforesaid method, in step (5), dissolving adds entry when who knows amount is to who knows 2～6 times of quality, and solvent temperature is 80～100 ℃, and dissolution time is 20min～90min.
In aforesaid method, in step (7), the amount that adds ammoniacal liquor is 3～6 times of aluminum ion mole number.
Be rotary kiln or revolving drum at the described roasting apparatus of step (4), be the chemical industry rotary kiln.
Be described in detail below in conjunction with several specific embodiments:
Embodiment 1
Flyash salic 21%, silicon-dioxide 62% is levigate to 100 orders, mix after mol ratio 4:1 batching by the aluminum oxide in ammonium sulfate and flyash, add 5% tap water in the material that mixes, then granulation, grain diameter is 5mm, particle enters in rotary kiln, 360 ℃ of roasting 1h, 410 ℃ of roasting 1h.Who knows of burning till adds 3 times of quality to the deionized water that who knows, at 80 ℃ of lower stripping 1.5h, filters, add ammoniacal liquor to get aluminum hydroxide precipitation in filtrate, washing and filtering, aluminium hydroxide solid are through the alumina product of roasting, and filtrate gets the ammonium sulfate solids recycle through evaporative crystallization.
Embodiment 2
Flyash salic 25%, silicon-dioxide 60% is levigate to 120 orders, mix after mol ratio 5:1 batching by the aluminum oxide in ammonium sulfate and flyash, add 10% tap water in the material that mixes, then granulation, grain diameter is 10mm, particle enters in rotary kiln, 370 ℃ of roasting 1h, 420 ℃ of roasting 1h.Who knows of burning till adds 4 times of quality to the deionized water that who knows, at 85 ℃ of lower stripping 1h, filters, add ammoniacal liquor to get aluminum hydroxide precipitation in filtrate, washing and filtering, aluminium hydroxide solid are through the alumina product of roasting, and filtrate gets the ammonium sulfate solids recycle through evaporative crystallization.
Flyash salic 30%, silicon-dioxide 45% is levigate to 200 orders, mix after mol ratio 6:1 batching by the aluminum oxide in ammonium sulfate and flyash, add 15% tap water in the material that mixes, then granulation, grain diameter is 15mm, particle enters in rotary kiln, 370 ℃ of roasting 0.5h, 410 ℃ of roasting 1h.Who knows of burning till adds 5 times of quality to the deionized water that who knows, at 90 ℃ of lower stripping 0.5h, filters, add ammoniacal liquor to get aluminum hydroxide precipitation in filtrate, washing and filtering, aluminium hydroxide solid are through the alumina product of roasting, and filtrate gets the ammonium sulfate solids recycle through evaporative crystallization.
Claims (6)
1. a flyash extracts the aluminum oxide method, comprises the following steps:
Step (1) is with the levigate activation of flyash, ammonium sulfate is levigate, to increase the surface-area of flyash and ammonium sulfate;
Step (2) is with the flyash after levigate and ammonium sulfate, in molar ratio with Al in flyash
2O
3: (NH
4)
2SO
4=1:3～6 are mixed to homogeneous admittedly;
Step (3) namely adds entry, granulation in flyash and ammonium sulfate mixture in the raw material that mixes homogeneous;
Step (4) is placed in the roasting apparatus roasting with particle described in step (3), calcination procedure adopts two sections method of temperature-control by, described two sections method of temperature-control by comprise respectively low-temperature zone roasting and high temperature section roasting, acting as of low-temperature zone roasting makes ammonium sulfate and the sclerosis of mixture of fly ash particle surface, control particle shape, the low-temperature zone maturing temperature is selected 350 ℃～390 ℃; The high temperature section roasting act as the increase chemical reaction rate, reduce the reaction times, the high temperature section maturing temperature is selected 390 ℃～450 ℃;
Step (5) is put into water with roasting who knows and is dissolved into solution;
The solution that step (6) filtration step (5) is made is collected respectively filter residue and filtrate;
Step (7) adds ammoniacal liquor in the middle filtrate of collecting of step (6), obtain Al (OH)
3Precipitation;
Step (8) is to Al (OH)
3Calcining obtains Al
2O
3Product.
2. according to claim 1 method, is characterized in that, the flyash of described step (1) and the levigate granularity of ammonium sulfate are 100 orders～200 orders.
3. according to claim 1 method, is characterized in that, the water that adds in described step (3) is tap water or pure water, and the quality that adds entry accounts for 5～15% of flyash and ammonium sulfate mixture quality.
4. according to claim 1 method, is characterized in that, in described step (5), to add the amount of entry when who knows be to who knows 2～6 times of quality in dissolving, and solvent temperature is 80～100 ℃, and dissolution time is 20min～90min.
5. according to claim 1 method, is characterized in that, in step (7), the amount that adds ammoniacal liquor is 3～6 times of aluminum ion mole number.
6. according to claim 1 method, is characterized in that, is rotary kiln or revolving drum at the described roasting apparatus of step (4).
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771471A (en) * | 2014-01-26 | 2014-05-07 | 乌鲁木齐金石徽龙矿业有限公司 | Method for preparing aluminum oxide through coal ash |
| CN104150515A (en) * | 2014-08-11 | 2014-11-19 | 航天推进技术研究院 | Method for extracting alumina from fly ash based on ammonium sulfate method |
| CN105366699A (en) * | 2014-08-28 | 2016-03-02 | 北京航天动力研究所 | Calcination and activation method and device for high-aluminum pulverized coal furnace flyash |
| CN113353958A (en) * | 2021-07-29 | 2021-09-07 | 上海绿麟达新材料科技有限公司 | Clean production process of hexafluorophosphate |
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|---|---|---|---|---|
| CN101117228A (en) * | 2007-07-12 | 2008-02-06 | 中国铝业股份有限公司 | Method for extracting aluminium oxide from coal ash |
| KR20090032806A (en) * | 2007-09-28 | 2009-04-01 | 한국전력공사 | Extraction method and apparatus of high pure alumina from fly ash using microwave |
| CN102120593A (en) * | 2010-01-08 | 2011-07-13 | 北京世纪地和科技有限公司 | Method for extracting aluminum oxide from pulverized flue ash |
| CN102583468A (en) * | 2012-03-08 | 2012-07-18 | 航天推进技术研究院 | Method for extracting aluminum oxide from fly ash based on ammonium sulfate activation process |
-
2013
- 2013-02-28 CN CN2013100629220A patent/CN103086412A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117228A (en) * | 2007-07-12 | 2008-02-06 | 中国铝业股份有限公司 | Method for extracting aluminium oxide from coal ash |
| KR20090032806A (en) * | 2007-09-28 | 2009-04-01 | 한국전력공사 | Extraction method and apparatus of high pure alumina from fly ash using microwave |
| CN102120593A (en) * | 2010-01-08 | 2011-07-13 | 北京世纪地和科技有限公司 | Method for extracting aluminum oxide from pulverized flue ash |
| CN102583468A (en) * | 2012-03-08 | 2012-07-18 | 航天推进技术研究院 | Method for extracting aluminum oxide from fly ash based on ammonium sulfate activation process |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771471A (en) * | 2014-01-26 | 2014-05-07 | 乌鲁木齐金石徽龙矿业有限公司 | Method for preparing aluminum oxide through coal ash |
| CN103771471B (en) * | 2014-01-26 | 2015-02-25 | 乌鲁木齐金石徽龙矿业有限公司 | Method for preparing aluminum oxide through coal ash |
| CN104150515A (en) * | 2014-08-11 | 2014-11-19 | 航天推进技术研究院 | Method for extracting alumina from fly ash based on ammonium sulfate method |
| CN104150515B (en) * | 2014-08-11 | 2015-08-26 | 航天推进技术研究院 | From flyash, the method for aluminum oxide is extracted based on ammonium sulfate method |
| CN105366699A (en) * | 2014-08-28 | 2016-03-02 | 北京航天动力研究所 | Calcination and activation method and device for high-aluminum pulverized coal furnace flyash |
| CN113353958A (en) * | 2021-07-29 | 2021-09-07 | 上海绿麟达新材料科技有限公司 | Clean production process of hexafluorophosphate |
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