CN102351227B - Method for extracting aluminum oxide from fly ash by one-step process - Google Patents
Method for extracting aluminum oxide from fly ash by one-step process Download PDFInfo
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- CN102351227B CN102351227B CN 201110288032 CN201110288032A CN102351227B CN 102351227 B CN102351227 B CN 102351227B CN 201110288032 CN201110288032 CN 201110288032 CN 201110288032 A CN201110288032 A CN 201110288032A CN 102351227 B CN102351227 B CN 102351227B
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Abstract
The invention relates to a method for extracting aluminum oxide from fly ash by a one-step process. The technique for extracting aluminum oxide from fly ash by an acid-process/alkali-process has the defects of long technological procedure, complex equipment and poor economic performance, and restricts the large-scale application. The method comprises the following steps: mixing fly ash and potassium sulfate in concentrated sulfuric acid to carry out granulation; roasting for activation at certain temperature; dissolving out the solid in water or sulfuric acid to remove solid residues; removing the impurity iron from the solution by a jarosite process; crystallizing the solution to obtain solid potassium aluminum sulfate dodecahydrate; roasting the potassium aluminum sulfate dodecahydrate to obtain aluminum oxide, potassium sulfate solid and sulfur trioxide gas; and washing the solid phase, and filtering to obtain the aluminum oxide product. The potassium aluminum sulfate solid is obtained by cooling crystallization, thereby lowering the energy consumption; the impurities can be effectively removed in the crystallization process, thereby reducing the investment for the impurity removal system; and the potassium sulfate and sulfuric acid can be recycled, so the economic benefit of industrial production is high.
Description
Technical field
The invention belongs to the flyash processing technology field, be specifically related to a kind of from flyash one step extract method of alumina.
Background technology
Aluminous fly-ash is in the last few years along with the exploitation of the western coal resources of China and the construction of large-size thermal power plant, appear at a kind of new flyash type of central and west regions, Inner Mongol, its Al2O3 content can reach about 50% usually, is equivalent to the content of Al2O3 in China's middle-low bauxite.
In recent years, along with the high speed development of China's aluminium industry, the contradiction of bauxite and aluminum oxide short supply becomes increasingly conspicuous.At present, the retained reserve of China's bauxite only is about 2,000,000,000 tons, and the high-quality bauxite resource is relatively deficienter, and most of bauxite and aluminum oxide need external import.In order to satisfy China's aluminium industrial expansion demand, utilize this rare coal aluminium mineral association resource of aluminous fly-ash for scientific development simultaneously, reduce the transportation of flyash and hoard occupation of land and the problem of environmental pollution of generation in a large number, utilize aluminous fly-ash to produce aluminum oxide and more and more cause people's attention.
From flyash, extract method of alumina at present and mainly contain acid system and alkaline process.Alkaline process has mainly followed bauxite and has extracted method of alumina, and this method technical process is long, and the level of residue that produces behind the extraction aluminum oxide is that the flyash amount gets several times, does not meet national requirements for environmental protection; It is shorter that acid system is compared technical process, but hydrochloric acid to the equipment material seriously corroded, corresponding facility investment is higher; If use evaporation operation in the acid system system energy consumption is increased considerably, economy is not high.
Summary of the invention
The purpose of this invention is to provide the one step extraction method of alumina from flyash that a kind of processing method is simple, be easy to the heavy industrialization application.
The technical solution adopted in the present invention is:
A kind of from flyash one step extract method of alumina, it is characterized in that:
Realized by following steps:
Step 1: be mixing granulation in the sulfuric acid of 70%-90% by the mass ratio of 1-2:1 at massfraction with flyash and vitriolate of tartar, at 400-700 ℃ of following calcination activation, roasting reaction is 0.1-5 hour, and the gained solid is that the sulfuric acid stripping after-filtration of 30-60% is removed solid residue through water or massfraction under 60-100 ℃, condition of normal pressure;
Step 2: the solution that step 1 is obtained is removed impurity iron in the solution by the ihleite method;
Step 3: the solution that step 2 is obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, Potassium aluminum sulfate dodecahydrate obtains aluminum oxide, vitriolate of tartar and sulphur trioxide after 900-1300 ℃ of roasting, solid phase obtains alumina product through washing, filtration, drying.
The particle diameter of the granulation in the step 1 is between the 1-5mm.
The temperature of the crystallisation by cooling in the step 3 drops to 20-40 ℃ from 80-100 ℃.
The present invention has the following advantages:
Adopt method of the present invention, can be in calcination activation single step reaction generate potassium aluminium sulfate, can utilize repeatedly crystallisation by cooling technology to finish crystallization simultaneously after the stripping and remove the two steps operation of impurity iron ion, cut down the consumption of energy significantly and invest; Add sulfuric acid and the fully recycle of vitriolate of tartar of this system, meet national recycling economy strategy, have good industrial applications prospect.
Embodiment
The present invention will be described in detail below in conjunction with embodiment.
Method of the present invention, based on the following principles of chemistry:
Roasting reaction: Al
2O
3+ K
2SO
4+ 3H
2SO
4=2KAl (SO
4)
2+ 3H
2O
Decomposition reaction: 2KAl (SO
4)
2=K
2SO
4+ Al
2O
3+ 3SO
3↑
Of the present invention from flyash one step extract method of alumina, it is characterized in that its method is mixing granulation in the vitriol oil with flyash and vitriolate of tartar, calcination activation at a certain temperature, the gained solid is removed solid residue through water or sulfuric acid stripping after-filtration, by the impurity in the ihleite method removal solution, this solution obtains the Potassium aluminum sulfate dodecahydrate of solid by cooling crystallization method, Potassium aluminum sulfate dodecahydrate obtains aluminum oxide, vitriolate of tartar solid and sulfur trioxide gas after roasting, solid phase obtains alumina product through washing, filtration, and vitriolate of tartar enters liquid phase; Liquid phase obtains vitriolate of tartar through concentrated and crystallisation by cooling, and gas phase obtains sulfuric acid through absorption, continues to recycle.
The flyash overwhelming majority is vitreous state, Al
2O
3Be nonactive body, poor activity.To from flyash, extract aluminum oxide and must open the Al-Si key by the method for physics or chemistry, namely carry out activation treatment, make the aluminum oxide in the flyash become activated alumina.
Granulation: for guarantee flyash activation and with the vitriolate of tartar reaction process in each material can fully contact, can improve simultaneously the mobile of material and reduction dust to the pollution of environment.
Utilize present method to carry out alumina extraction, the extraction yield of aluminum oxide is greater than 85%, and impurity iron content is lower than 0.03%.
Embodiment one:
Of the present invention from flyash one step extract method of alumina, realized by following steps:
Step 1: be in 70% sulfuric acid mixing granulation by the mass ratio of 1:1 at massfraction with flyash and vitriolate of tartar, particle diameter is 1mm; At 400 ℃ of following calcination activations, the roasting reaction times is 0.1 hour, and the gained solid goes out after-filtration and removes solid residue through water-soluble under 60 ℃, condition of normal pressure;
Step 2: the solution that step 1 is obtained is removed impurity iron in the solution by the ihleite method;
Step 3: the solution that step 2 is obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, and the temperature of crystallisation by cooling drops to 20 ℃ from 80 ℃; Potassium aluminum sulfate dodecahydrate obtains aluminum oxide, vitriolate of tartar and sulphur trioxide after 900 ℃ of roastings, solid phase obtains alumina product through washing, filtration, drying.
Embodiment two:
Of the present invention from flyash one step extract method of alumina, realized by following steps:
Step 1: be in 80% sulfuric acid mixing granulation by the mass ratio of 1.5:1 at massfraction with flyash and vitriolate of tartar, particle diameter is 1mm; At 500 ℃ of following calcination activations, roasting reaction is 0.1 hour, and the gained solid is that 30% sulfuric acid stripping after-filtration is removed solid residue through massfraction under 70 ℃, condition of normal pressure;
Step 2: the solution that step 1 is obtained is removed impurity iron in the solution by the ihleite method;
Step 3: the solution that step 2 is obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, and the temperature of crystallisation by cooling drops to 30 ℃ from 90 ℃; Potassium aluminum sulfate dodecahydrate obtains aluminum oxide, vitriolate of tartar and sulphur trioxide after 1000 ℃ of roastings, solid phase obtains alumina product through washing, filtration, drying.
Embodiment three:
Of the present invention from flyash one step extract method of alumina, realized by following steps:
Step 1: be in 80% sulfuric acid mixing granulation by the mass ratio of 1.5:1 at massfraction with flyash and vitriolate of tartar, particle diameter is 3mm; At 600 ℃ of following calcination activations, roasting reaction is 2.5 hours, and the gained solid is that 45% sulfuric acid stripping after-filtration is removed solid residue through massfraction under 90 ℃, condition of normal pressure;
Step 2: the solution that step 1 is obtained is removed impurity iron in the solution by the ihleite method;
Step 3: the solution that step 2 is obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, and the temperature of crystallisation by cooling drops to 30 ℃ from 90 ℃; Potassium aluminum sulfate dodecahydrate obtains aluminum oxide, vitriolate of tartar and sulphur trioxide after 1100 ℃ of roastings, solid phase obtains alumina product through washing, filtration, drying.
Embodiment four:
Of the present invention from flyash one step extract method of alumina, realized by following steps:
Step 1: be in 90% sulfuric acid mixing granulation by the mass ratio of 2:1 at massfraction with flyash and vitriolate of tartar, particle diameter is 5mm; At 700 ℃ of following calcination activations, roasting reaction is 5 hours, and the gained solid is that 60% sulfuric acid stripping after-filtration is removed solid residue through massfraction under 100 ℃, condition of normal pressure;
Step 2: the solution that step 1 is obtained is removed impurity iron in the solution by the ihleite method;
Step 3: the solution that step 2 is obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, and the temperature of crystallisation by cooling drops to 40 ℃ from 100 ℃; Potassium aluminum sulfate dodecahydrate obtains aluminum oxide, vitriolate of tartar and sulphur trioxide after 1300 ℃ of roastings, solid phase obtains alumina product through washing, filtration, drying.
Claims (2)
- One kind from flyash one step extract method of alumina, it is characterized in that:Realized by following steps:Step 1: be mixing granulation in the sulfuric acid of 70%-90% by the mass ratio of 1-2:1 at massfraction with flyash and vitriolate of tartar, at 400-700 ℃ of following calcination activation, roasting reaction is 0.1-5 hour, and the gained solid is that the sulfuric acid stripping after-filtration of 30-60% is removed solid residue through water or massfraction under 60-100 ℃, condition of normal pressure;Step 2: the solution that step 1 is obtained is removed impurity iron in the solution by the ihleite method;Step 3: the solution that step 2 is obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, Potassium aluminum sulfate dodecahydrate obtains aluminum oxide, vitriolate of tartar and sulphur trioxide after 900-1300 ℃ of roasting, solid phase obtains alumina product through washing, filtration, drying;The particle diameter of the granulation in the step 1 is between the 1-5mm.
- According to claim 1 a kind of from flyash one step extract method of alumina, it is characterized in that:The temperature of the crystallisation by cooling in the step 3 drops to 20-40 ℃ from 80-100 ℃.
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| CN 201110288032 CN102351227B (en) | 2011-09-26 | 2011-09-26 | Method for extracting aluminum oxide from fly ash by one-step process |
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| CN 201110288032 CN102351227B (en) | 2011-09-26 | 2011-09-26 | Method for extracting aluminum oxide from fly ash by one-step process |
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| CN102351227B true CN102351227B (en) | 2013-08-21 |
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| CN102703692B (en) * | 2012-04-17 | 2014-09-03 | 昆明理工大学 | Method for removing ferrotitanium in low-grade bauxite by curing process with sulfuric acid |
| CN103880012B (en) * | 2014-01-27 | 2015-12-09 | 吉林大学 | A kind of method that sial material activating decomposes |
| CN106477606B (en) * | 2016-10-12 | 2018-03-20 | 北京矿冶研究总院 | Method for extracting aluminum oxide from fly ash based on sulfuric acid curing |
| CN108996533A (en) * | 2018-07-24 | 2018-12-14 | 山西大学 | A kind of coupling activation method of flyash, gangue |
| CN112125325A (en) * | 2020-09-29 | 2020-12-25 | 福州大学 | Process for producing alumina by aluminosilicate mineral acid method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515494A (en) * | 2003-01-03 | 2004-07-28 | 王如声 | Production method of crystal alum |
| CN100503901C (en) * | 2007-07-25 | 2009-06-24 | 中国科学院青海盐湖研究所 | Process for producing aluminum oxide crystal whisker |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515494A (en) * | 2003-01-03 | 2004-07-28 | 王如声 | Production method of crystal alum |
| CN100503901C (en) * | 2007-07-25 | 2009-06-24 | 中国科学院青海盐湖研究所 | Process for producing aluminum oxide crystal whisker |
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