CN102432052B - Method for extracting aluminum oxide from pulverized fuel ash by using potassium sulfate - Google Patents
Method for extracting aluminum oxide from pulverized fuel ash by using potassium sulfate Download PDFInfo
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- CN102432052B CN102432052B CN201110288031.8A CN201110288031A CN102432052B CN 102432052 B CN102432052 B CN 102432052B CN 201110288031 A CN201110288031 A CN 201110288031A CN 102432052 B CN102432052 B CN 102432052B
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Abstract
The invention relates to a method for extracting aluminum oxide from pulverized fuel ash by using potassium sulfate. The conventional alkaline process for extracting the aluminum oxide from the pulverized fuel ash has a long process flow, makes equipment complicated, is low in economic benefits and makes large-scale application restrained. The method comprises the following steps of: performing roasting activation or mechanical lapping activation on the pulverized fuel ash, dissolving the obtained solid by using sulfuric acid, and then filtering to remove solid residues; adding potassium sulfate solids into the solution; reacting for a certain period of time to obtain a aluminum potassium sulfate solution; removing impurities in the solution by a chemical or resin adsorption method; crystallizing the solution to obtain solid aluminum potassium sulfate dodecahydrate; roasting the aluminum potassium sulfate dodecahydrate to obtain the aluminum oxide, the potassium sulfate solids and sulfur trioxide gas; and washing a solid phase, filtering, and thus obtaining an aluminum oxide product. By a cooling and crystallizing method, aluminum potassium sulfate solids are obtained, and energy consumption is reduced; during crystallization, impurities can be effectively removed, and investments in impurity removing systems are reduced; and the potassium sulfate and the sulfuric acid can be recycled, so that the economic benefit of industrialized production is high.
Description
Technical field
the invention belongs to flyash processing technology field, be specifically related to a kind of method utilizing potassium sulfate to extract aluminum oxide from flyash.
Background technology
Flyash is a kind of solid waste that coal burning produces, and accounts for the 10-40% of coal amount.The flyash that current Power Plant in China and other coal firing boiler discharge every year, up to 3.3 hundred million tons, is mainly used in production of construction materials, construction work, builds the road, fertiliser production, improvement soil and backfill etc.Because the market requirement is saturated and the reason such as flyash activity, China's flyash often has the accumulation of 100,000,000 tons every year, ends 2008, and China's flyash adds up accumulation more than 2,700,000,000 tons.The generation of the flyash of flood tide, both air, soil and water resources were polluted, and took again limited vacant lot (comprising arable land), have a strong impact on the living environment of the people, therefore for the clean utilization of coal, the harmless treatment of flyash is become to one of important content of China's energy strategy.
China's aluminum oxide industry development in recent years is rapid, and 2006 annual production leap to No. 1 in the world, and 2008 annual production account for 27.36% of Gross World Product.Aluminum oxide is produced by Bayer process primarily of alum clay rich ore at present, but 3.12% of China's bauxite resource Jin Zhan world total reserves, and most of grade is lower, therefore China maintains the development of aluminum oxide industry at present mainly through a large amount of import bauxite, from 880,000 tons of rapid growths of 2004 by 2008 2,579 ten thousand tons of bauxite import volume.The alternate resources finding bauxite is imperative in China.In China's flyash, aluminum oxide average content is 27%, and some areas, up to 50%, are very important bauxite resources.Aluminum oxide technology prepared by development powder coal ash, effectively can not only solve occupying cultivated land and problem of environmental pollution of flyash, also can solve China's alumina producing raw material and to hide weary predicament, have great environment and economy meaning.
The technique utilizing flyash to prepare aluminum oxide as bauxite resource is mainly divided into acid system and alkaline process, be by activation after flyash with acid or alkali reaction generate aluminium salt, then obtain aluminum oxide through steps such as purification & isolation, drying, pyrolytic decompositions.It is long to there is technical process in current technological process control, and the shortcomings such as equipment complexity, deficiency in economic performance, constrain large-scale application.
Summary of the invention
The object of this invention is to provide a kind of technique potassium sulfate that utilizes that is comparatively simple, that be easy to heavy industrialization application from flyash, extract the method for aluminum oxide.
The technical solution adopted in the present invention is:
Utilize potassium sulfate from flyash, extract a method for aluminum oxide, it is characterized in that:
Realized by following steps:
Step one: flyash is activated, gained solid 20-90 DEG C, be the sulfuric acid stripping of 10%-85% through massfraction under 0.1-1MPa condition, slagging-off, obtains the solution of sulfur acid aluminium;
Step 2: add potassium sulfate solid in the solution of the sulfur acid aluminium obtained in step one, the mass ratio adding potassium sulfate solid and initial flyash is 1:1.1-2.5, and at 80-100 DEG C of temperature, synthesis under normal pressure 0.1-3 hour, obtains removal of impurities after aluminum potassium sulfate solution;
Step 3: solution step 2 obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by the method for crystallisation by cooling or multiple-effect evaporation crystallization, after the roasting that temperature is 900-1300 DEG C, obtain aluminum oxide, potassium sulfate and sulphur trioxide, solid phase obtains alumina product through washing, filtration, drying.
Activation in step one refers to calcination activation, and maturing temperature is 500-800 DEG C, and roasting time is 0.1-6 hour.
Activation in step one refers to that mechanical mill activates, and after grinding, granularity is 2-50 μm.
Slagging-off in step one adopts vertical plate-and-frame filter press.
Removal of impurities in step 2 adopts ihleite method or cation exchange resin processes.
In step 3, the temperature of crystallisation by cooling is for drop to 20-40 DEG C from 80-100 DEG C.
The present invention has the following advantages:
Adopt method of the present invention to extract aluminum oxide from flyash, obtain potassium aluminium sulfate solid by energy-conservation crystallisation by cooling method, reduce energy consumption; Effectively can remove impurity while crystallization, especially iron ion, reduce impurity removed system investment; Potassium sulfate and sulfuric acid (with sulphur trioxide form) can recycle, and suitability for industrialized production high financial profit, is easy to industrial applications.
Embodiment
Below in conjunction with embodiment, the present invention will be described in detail.
Method of the present invention, based on the following principles of chemistry:
Stripping is reacted: Al
2o
3+ 3H
2sO
4=Al
2(SO
4)
3+ 3H
2o
React in solution: Al
2(SO
4)
3+ K
2sO
4=2KAl (SO
4)
2
Decomposition reaction: 2KAl (SO
4)
2=K
2sO
4+ Al
2o
3+ 3SO
3↑
A kind of method extracting aluminum oxide from flyash of the present invention, by flyash calcination activation or carry out mechanical mill activation at a certain temperature, gained solid filters after sulfuric acid stripping removes solid residue, potassium sulfate solid is added in solution, aluminum potassium sulfate solution is obtained after reaction for some time, and the impurity removed by method that is chemical or resin absorption in solution, this solution obtains the Potassium aluminum sulfate dodecahydrate of solid by the method for crystallization, Potassium aluminum sulfate dodecahydrate obtains aluminum oxide after roasting, potassium sulfate solid and sulfur trioxide gas, solid phase is through washing, filtration obtains alumina product.Potassium sulfate enters liquid phase, and liquid phase obtains potassium sulfate through concentrated and crystallisation by cooling, and gas phase obtains sulfuric acid through absorbing, and continues to recycle.
The flyash overwhelming majority is vitreous state, Al
2o
3for inactive form, poor activity.Aluminum oxide to be extracted from flyash, Al-Si key must be opened by the method for physics or chemistry, namely carry out activation treatment, make the aluminum oxide in flyash become activated alumina.
Utilize present method to extract aluminum oxide from flyash, the extraction yield of aluminum oxide is greater than 89%, and impurity iron content is lower than 0.025%.
Embodiment 1:
A kind of method utilizing potassium sulfate to extract aluminum oxide from flyash of the present invention, is realized by following steps:
Step one: calcination activation is carried out to flyash, maturing temperature is 500 DEG C, and roasting time is 0.1 hour; Gained solid 20 DEG C, under 0.1MPa condition through massfraction be 10% sulfuric acid stripping, adopt vertical plate-and-frame filter press to remove the gred, obtain the solution of sulfur acid aluminium;
Step 2: add potassium sulfate solid in the solution of the sulfur acid aluminium obtained in step one, adding potassium sulfate solid with the mass ratio of flyash is 1:1.1, at 80 DEG C of temperature, synthesis under normal pressure 0.1 hour, after obtaining aluminum potassium sulfate solution, the removal of impurities of employing ihleite method;
Step 3: solution step 2 obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, crystallisation by cooling temperature is for drop to 20 DEG C from 80 DEG C; After the roasting that temperature is 900 DEG C, obtain aluminum oxide, potassium sulfate and sulphur trioxide, solid phase obtains alumina product through washing, filtration, drying.
Embodiment 2:
A kind of method utilizing potassium sulfate to extract aluminum oxide from flyash of the present invention, is realized by following steps:
Step one: calcination activation is carried out to flyash, maturing temperature is 650 DEG C, and roasting time is 3 hours; Gained solid 55 DEG C, under 0.5MPa condition through massfraction be 45% sulfuric acid stripping, adopt vertical plate-and-frame filter press to remove the gred, obtain the solution of sulfur acid aluminium;
Step 2: add potassium sulfate solid in the solution of the sulfur acid aluminium obtained in step one, adding potassium sulfate solid with the mass ratio of flyash is 1:1.8, at 90 DEG C of temperature, synthesis under normal pressure 1.5 hours, after obtaining aluminum potassium sulfate solution, the removal of impurities of employing ihleite method;
Step 3: solution step 2 obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, crystallisation by cooling temperature is for drop to 30 DEG C from 90 DEG C; After the roasting that temperature is 1100 DEG C, obtain aluminum oxide, potassium sulfate and sulphur trioxide, solid phase obtains alumina product through washing, filtration, drying.
Embodiment 3:
A kind of method utilizing potassium sulfate to extract aluminum oxide from flyash of the present invention, is realized by following steps:
Step one: calcination activation is carried out to flyash, maturing temperature is 1100 DEG C, and roasting time is 6 hours; Gained solid 90 DEG C, under 1MPa condition through massfraction be 85% sulfuric acid stripping, adopt vertical plate-and-frame filter press to remove the gred, obtain the solution of sulfur acid aluminium;
Step 2: add potassium sulfate solid in the solution of the sulfur acid aluminium obtained in step one, adding potassium sulfate solid with the mass ratio of flyash is 1:2.5, at 100 DEG C of temperature, synthesis under normal pressure 3 hours, after obtaining aluminum potassium sulfate solution, the removal of impurities of employing ihleite method;
Step 3: solution step 2 obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, crystallisation by cooling temperature is for drop to 40 DEG C from 100 DEG C; After the roasting that temperature is 1300 DEG C, obtain aluminum oxide, potassium sulfate and sulphur trioxide, solid phase obtains alumina product through washing, filtration, drying.
Embodiment 4:
A kind of method utilizing potassium sulfate to extract aluminum oxide from flyash of the present invention, is realized by following steps:
A kind of method extracting aluminum oxide from flyash of the present invention, is realized by following steps:
Step one: mechanical mill activation is carried out to flyash, after grinding, granularity is 2 μm; Gained solid 20 DEG C, under 0.1MPa condition through massfraction be 10% sulfuric acid stripping, adopt vertical plate-and-frame filter press to remove the gred, obtain the solution of sulfur acid aluminium;
Step 2: add potassium sulfate solid in the solution of the sulfur acid aluminium obtained in step one, the mass ratio adding potassium sulfate solid and flyash is 1:1.1, at 80 DEG C of temperature, and synthesis under normal pressure 0.1 hour, after obtaining aluminum potassium sulfate solution, adopt cation exchange resin processes removal of impurities;
Step 3: solution step 2 obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by the method for multiple-effect evaporation crystallization; Be obtain aluminum oxide, potassium sulfate and sulphur trioxide after 900 DEG C of roastings through temperature, solid phase through washing, filter, drying obtains alumina product.
Embodiment 5:
A kind of method utilizing potassium sulfate to extract aluminum oxide from flyash of the present invention, is realized by following steps:
Step one: mechanical mill activation is carried out to flyash, after grinding, granularity is 25 μm; Gained solid 55 DEG C, under 0.5MPa condition through massfraction be 45% sulfuric acid stripping, adopt vertical plate-and-frame filter press to remove the gred, obtain the solution of sulfur acid aluminium;
Step 2: add potassium sulfate solid in the solution of the sulfur acid aluminium obtained in step one, the mass ratio adding potassium sulfate solid and flyash is 1:1.8, at 90 DEG C of temperature, and synthesis under normal pressure 1.5 hours, after obtaining aluminum potassium sulfate solution, adopt cation exchange resin processes removal of impurities;
Step 3: solution step 2 obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by the method for multiple-effect evaporation crystallization; After the roasting that temperature is 1100 DEG C, obtain aluminum oxide, potassium sulfate and sulphur trioxide, solid phase obtains alumina product through washing, filtration, drying.
Embodiment 6:
A kind of method utilizing potassium sulfate to extract aluminum oxide from flyash of the present invention, is realized by following steps:
Step one: mechanical mill activation is carried out to flyash, after grinding, granularity is 50 μm; Gained solid 90 DEG C, under 1MPa condition through massfraction be 85% sulfuric acid stripping, adopt vertical plate-and-frame filter press to remove the gred, obtain the solution of sulfur acid aluminium;
Step 2: add potassium sulfate solid in the solution of the sulfur acid aluminium obtained in step one, the mass ratio adding potassium sulfate solid and flyash is 1:2.5, at 100 DEG C of temperature, and synthesis under normal pressure 3 hours, after obtaining aluminum potassium sulfate solution, adopt cation exchange resin processes removal of impurities;
Step 3: solution step 2 obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by the method for multiple-effect evaporation crystallization; After the roasting that temperature is 1300 DEG C, obtain aluminum oxide, potassium sulfate and sulphur trioxide, solid phase obtains alumina product through washing, filtration, drying.
Claims (1)
1. utilize potassium sulfate from flyash, extract a method for aluminum oxide, it is characterized in that:
Realized by following steps:
Step one: calcination activation is carried out to flyash, maturing temperature is 500 DEG C, and roasting time is 0.1 hour; Gained solid 20 DEG C, under 0.1MPa condition through massfraction be 10% sulfuric acid stripping, adopt vertical plate-and-frame filter press to remove the gred, obtain the solution of sulfur acid aluminium;
Step 2: add potassium sulfate solid in the solution of the sulfur acid aluminium obtained in step one, adding potassium sulfate solid with the mass ratio of flyash is 1:1.1, at 80 DEG C of temperature, synthesis under normal pressure 0.1 hour, after obtaining aluminum potassium sulfate solution, the removal of impurities of employing ihleite method;
Step 3: solution step 2 obtained obtains the Potassium aluminum sulfate dodecahydrate of solid by crystallisation by cooling, crystallisation by cooling temperature is for drop to 20 DEG C from 80 DEG C; After the roasting that temperature is 900 DEG C, obtain aluminum oxide, potassium sulfate and sulphur trioxide, solid phase obtains alumina product through washing, filtration, drying.
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| CN103663511B (en) * | 2012-08-31 | 2015-11-04 | 沈阳铝镁设计研究院有限公司 | HCl treatment coal ash for manufacturing is for the method for aluminum oxide |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515494A (en) * | 2003-01-03 | 2004-07-28 | 王如声 | Production method of crystal alum |
| CN101607259A (en) * | 2009-07-17 | 2009-12-23 | 华东理工大学 | A kind of method of activating fly ash at low temperature and application thereof |
| CN101660204A (en) * | 2009-09-09 | 2010-03-03 | 中国科学院青海盐湖研究所 | Preparation method of hexagonal piece aluminum oxide whisker material |
| CN101948126A (en) * | 2009-09-08 | 2011-01-19 | 华东理工大学 | Method for activating fly ash by high-temperature microwave |
-
2011
- 2011-09-26 CN CN201110288031.8A patent/CN102432052B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515494A (en) * | 2003-01-03 | 2004-07-28 | 王如声 | Production method of crystal alum |
| CN101607259A (en) * | 2009-07-17 | 2009-12-23 | 华东理工大学 | A kind of method of activating fly ash at low temperature and application thereof |
| CN101948126A (en) * | 2009-09-08 | 2011-01-19 | 华东理工大学 | Method for activating fly ash by high-temperature microwave |
| CN101660204A (en) * | 2009-09-09 | 2010-03-03 | 中国科学院青海盐湖研究所 | Preparation method of hexagonal piece aluminum oxide whisker material |
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