CN106115751A - A kind of method utilizing two-part acid reaction method to extract aluminium oxide - Google Patents
A kind of method utilizing two-part acid reaction method to extract aluminium oxide Download PDFInfo
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- CN106115751A CN106115751A CN201610464185.0A CN201610464185A CN106115751A CN 106115751 A CN106115751 A CN 106115751A CN 201610464185 A CN201610464185 A CN 201610464185A CN 106115751 A CN106115751 A CN 106115751A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/26—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with sulfuric acids or sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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Abstract
The invention belongs to chemical technology field, relate to the extraction of aluminium oxide, it is provided that a kind of method utilizing two-part acid reaction method to extract aluminium oxide.The present invention is that activator decomposes through low-temperature bake, middle temperature initially with concentrated sulphuric acid, obtains active silica-alumina material, then uses " a step acid pasting " Low-temperature acid soluble to extract alumina component therein.The inventive method flow process is simple, and alumina extraction ratio is high, and magazins' layout is thorough, operates safety.
Description
Technical field
The invention belongs to chemical technology field, relate to the extraction of aluminium oxide.
Technical background
Coal-powder boiler flyash is coal-fired remaining solid waste after high-temp combustion.Sial component in aluminous fly-ash
Mainly exist mutually with crystallizations such as mullite, corundum and quartz, and the silicate glass matter containing inequality, wherein Al2O3And SiO2
Content all reaches more than 30-40%, can be as the raw material of alumina extraction.At present, from bauxite, aluminium oxide is extracted both at home and abroad
Technics comparing is ripe, predominantly Bayer process.The research extracting aluminium oxide from other high alumina materials is concentrated mainly on flyash side
Face, the method related to includes alkaline process, soda lime sintering process, acid system etc., the only alkaline process of application of putting into production.
The principle of alkaline process is under highly basic effect, and the aluminium oxide in flyash generates sodium aluminate with silicon dioxide with alkali effect
And sodium silicate, obtain siliceous sodium aluminate solution, desiliconization afterwards, preparing hydrogen aluminium oxide through water-soluble, finally obtain aluminium oxide.Tool
Body technology includes Bayer process, sintering process.
The principle of soda lime method is under conditions of with the presence of calcium oxide, uses caustic digestion flyash so that it is middle major part silicon
React generation silico-calcium compound with calcium, separate under the conditions of water-soluble with the sodium aluminate generated simultaneously.
Alkali process is the highest to equipment requirements, and bayer process is ripe, but due in high silicon materials silicone content big, cause
In alkaline environment, a large amount of dissolutions of silicon make sial separating difficulty strengthen, and production cost is high, and it is big to produce the quantity of slag.
The feature of acid technological process is: under strongly acidic conditions, utilizes the both sexes feature of aluminium oxide by its dissolution, it is achieved with greatly
The separation of amount siliceous oxide, then obtain alumina product through further remove impurity.Representative is sulfuric acid process and fluid bed
The hydrochloric acid acid pasting of ash.Sulphuric acid method is used to include aqueous sulfuric acid and concentrated sulphuric acid calcination method.Aqueous sulfuric acid is used often to need
Reaction temperature that will be higher, more than 180 DEG C；Some researcheres use and add a small amount of additive such as fluoride promotion reaction etc.,
The corrosion-resistant problem of container causing reaction system is serious, it is difficult to industrial applications.
Wu Ping, " extracting the research of high-purity ultra-fine alumina mechanism and technique from flyash ", University Of Tianjin 2005 is large
Scholar's paper.
Zhu Shi is bony, " extracting the microwave method test of aluminum sulfate and iron sulfate from flyash ", Ningxia engineering,
2001,3 (1): 48-50.
Wang Wen waits quietly, and " condition of acidity extraction aluminium oxide selects ", energy environment is protected, 2003, (4): 17-19.
Use the research of simple concentrated sulfuric acid roasting method, i.e. use excess concentrated sulphuric acid to be heated to roasting under decomposition temperature and divide
After solving flyash, more unnecessary sulphuric acid is thermally decomposed removal at a higher temperature, it is thus achieved that water soluble sulfate solid, pass through water
Molten separate with siliceous.
Mu Wenning, " coal ash for manufacturing is for the technical study of aluminum sulfate ", Northeastern University's Master's thesis in 2008.
Wu Yan, " from flyash, extracting aluminium oxide and the research of silicon dioxide ", Northeastern University's thesis for the doctorate in 2008.
White light brightness etc., " flyash sulfuric acid process carries the heart technological parameter of aluminum and studies ", coal science and technology, 2008,36 (9):
106-109。
The principle of sulfate process is to utilize sulfate aluminium oxide in sial material to respond activity and several to silicon dioxide
Nonreactive feature, mixes flyash with sulfate, and heated decomposition occurs solid state reaction, makes aluminium oxide in flyash divide
Solving and generate aluminum sulfate salt, aluminum sulfate salt further decomposes acquisition aluminium oxide.In ammonium sulfate method, the acquisition of alumina product needs
Decomposition of ammonium sulfate to be experienced, produces a large amount of ammonia, then experiences liquid phase scrubbing formation Burnt ammonium alum, sulphate decomposition and sulfur trioxide
The multi-step gas-liquid processes such as absorption realize circulation.
CN1868884 Li Yu discloses " method extracting aluminium oxide co-producing white carbon black simultaneously in flyash " by fine coal ashing
Powder, adds ammonium sulfate, then adds water in reactant, filter, add ammonia, obtain aluminium hydroxide and hydrogen in filtrate after activation
Ferrum oxide mixed precipitation, passes through to add kind of carbon again and gets pure hydrogen-oxygen after finally being melted by aluminum hydroxide precipitation with sodium hydroxide solution
Change aluminum, finally fire to obtain Al2O3.Using ammonium sulfate is that circulatory mediator extracts aluminium oxide, because ammonium sulfate does not reacts with silicon, in system
Take and alumina process eliminates numerous and diverse desiliconization process.
CN101117228 Yin middle forest discloses " a kind of method extracting aluminium oxide from flyash ", is to be joined by ammonium sulfate
Entering flyash to be sintered, gained solid obtains the solution of sulfur acid aluminum ammonium after dissolution, and this solution is obtained by the method for crystallization
Burnt ammonium alum to solid.Solid aluminum sulfate ammonium and ammonia reaction obtain aluminium hydroxide and ammonium sulfate, by washing and filtering, obtain
The aluminium hydroxide of solid, available alumina product after aluminium hydroxide is fired；The ammonium sulfate of entrance liquid phase, after evaporation, continues
Recycle.
The CN101734698A Zhai Yu spring etc. discloses " a kind of method being prepared aluminium oxide by aluminiferous material ".A kind of by alum clay
Prepared by the aluminiferous materials such as ore deposit, high-iron bauxite, alunite, Kaolin, bauxite, flyash, gangue, aluminum ash, nepheline, clay
The method of the products such as aluminium oxide, the method comprises the following steps: aluminiferous material is crushed by (1), levigate after mix roasting with ammonium sulfate
Burn；(2) product of roasting (grog) is water-soluble, be filtrated to get aluminum ammonium sulfate solution and filtering residue；(3) with ammonia, aluminum ammonium sulfate solution is removed
Ferrum, heavy aluminum or recrystallization prepare aluminium oxide, reclaim ammonium sulfate simultaneously；(4) filtering residue prepares silica product, recrement iron content, makees
For iron-smelting raw material.
CN201010300143.6 Zhang Kaiyuan discloses " a kind of method extracting aluminium oxide from flyash ", and method includes
Following steps: after flyash fine grinding, and carry out except ferrum processes；It is sintered after mixing with ammonium sulfate except the flyash after ferrum
Rear generation solids and ammonia；The solids generated after sintering is carried out dissolution, then carries out filtering or settlement separate, the most again
The solution containing Burnt ammonium alum is obtained after washing；Carry out the solution containing Burnt ammonium alum crystallizing the Burnt ammonium alum obtaining solid；
It is configured to solution after being dissolved by the Burnt ammonium alum of solid to carry out reacting 0.5 at temperature is 20 DEG C～50 DEG C with ammonia or ammonia
Hour～within 6 hours, generate aluminium hydroxide and ammonium sulfate；Aluminium oxide is obtained after aluminium hydroxide is carried out roasting.
CN102515221A deposits Wei such as younger brother etc. and discloses one and " extract aluminium oxide and amorphous state two from flyash or gangue
The method of silicon oxide ", use simple pyrosulfate method activation decomposed powder coal ash method relatively easy, alleviate equipment corrosion
Problem, but salt method common feature to be salt consumption big, relatively costly.
Above-mentioned aluminium oxide method of extracting from flyash cuts both ways, and acid pasting is high to equipment requirements, and production operation is dangerous
Greatly, cumbersome, salt method (ammonium sulfate, pyrosulfate) salt dosage is big, relatively costly；Ammonium salt process not only cost is high, and a large amount of ammonia
Gas is easily generated danger.Therefore, current industrialized production is still based on traditional alkaline process.
Summary of the invention
Present invention aims to the deficiency of above-mentioned prior art, it is provided that a kind of two sections of acid reaction modes activate decomposition
Coal-powder boiler flyash and aluminium silicate mineral extract the new method of aluminium oxide.
It is an object of the invention to be achieved through the following technical solutions:
A kind of method utilizing two-part acid reaction method to extract aluminium oxide, comprises the following steps:
1) press aluminium oxide in material generate sulphuric acid required for aluminum sulfate theoretical amount 1～1.5 times (preferably, 1～
1.2 times) add concentrated sulphuric acid (mass content be 98% and more than) mix homogeneously；At 240～315 DEG C (preferably, 260～300
DEG C) under the conditions of roasting 1～8 hours (preferably, 3～5 hours), be warming up to 800～900 DEG C keep 3-6 hour, cooling take out；
Preferably, the sulfur trioxide gas that roasting produces uses water to absorb extracting sulfuric acid；
2) to step 1) product that obtains according to wherein alumina content, add needed for reaction generates aluminum chloride or aluminum sulfate
The hydrochloric acid of the theoretical amount wanted or sulphuric acid, stir, temperature 100 DEG C～180 DEG C (preferably, 120～150 DEG C), keep 1～
10 hours (preferably 2～6 hours), solid-liquid separation, obtain solubility aluminum chloride or aluminum sulfate solution；Solid is amorphous state dioxy
SiClx；
3) aluminium salt in aluminum chloride or aluminum sulfate solution is changed into aluminium oxide；Preferably, to liquor alumini chloridi or sulphuric acid
Aluminum solutions concentration, crystallization, roasting, obtain aluminium oxide；Preferably, the hydrogen chloride or the sulfur trioxide gas water that produce roasting are inhaled
Receive, obtain hydrochloric acid or sulphuric acid.
Wherein, any one during described material is coal-powder boiler flyash, mullite or high aluminosilicate.
Preferably, to step 2) aluminum chloride that obtains or aluminum sulfate solution first carry out except ferrum；Preferably, utilize except ferrum adsorbs
Resin removes ferrum.
The present invention uses concentrated sulphuric acid to be that activator decomposes through low-temperature bake, middle temperature, obtains active silica-alumina material, this sial
Material is amorphous state, activity is high, do not scab, be prone to material transfer.On this basis, " a step acid pasting " Low-temperature acid soluble is used to carry
Take alumina component therein.The method is applicable to all kinds of difficult activation decomposing sial material and decomposes.Sulphuric acid with single process
Aqua-solution method, concentrated sulfuric acid roasting method are compared with sulfating roasting method, and present invention process flow process is simple, and alumina extraction ratio is high, miscellaneous
Matter separates thoroughly, operates safety.
Detailed description of the invention
Present invention will be described in detail according to detailed description of the invention below, but present invention will be not limited to this.
As no specific instructions, the reagent used in following example, instrument are all this area conventional reagent, instrument, can
To obtain from being commonly purchased approach；The method used is this area conventional method, and those skilled in the art can be according to hereafter
Describe content repeat embodiment process and realize described result.
The two-part acid reaction method of the present invention extract the method for aluminium oxide be first by material with sulfuric acid activated, recycling is sour molten
Aluminium oxide is obtained in conjunction with conventional crystallization, method of roasting.Described material can be coal-powder boiler flyash, mullite or high aluminum silicate
The contour aluminium-containing substance of salt.
Specifically, the method comprises the following steps:
1) generate, by aluminium oxide in material, 1～1.5 times of addition that the theory (mole) of the sulphuric acid required for aluminum sulfate measures dense
Sulphuric acid (mass content be 98% and more than) mix homogeneously；Roasting 1～8 hours under the conditions of 240～315 DEG C, be warming up to 800
～900 DEG C keep 3-6 hour, cooling take out.
According to routine operation, before this step, the alumina content in conventional method detection material can be first passed through, thus
Judge to need to use how much sulphuric acid.In this step, the actually used amount of sulphuric acid, equal to or more than theoretical usage amount, is in order to fully
Activation material.Those skilled in the art according to actual needs, can adjust the usage amount of sulphuric acid, reaction temperature, time etc..One
In a little embodiments, the concentrated sulphuric acid amount of addition is 1～1.2 times of theoretical amount.Sintering temperature can be 260～300 DEG C, during roasting
Between can be 3～5 hours.
Sulfur trioxide gas will be produced in roasting process, water can be used to absorb extracting sulfuric acid, it is achieved following of raw material
Ring utilizes.
2) to step 1) product that obtains according to wherein alumina content, add needed for reaction generates aluminum chloride or aluminum sulfate
The hydrochloric acid of the theoretical molar amount wanted or sulphuric acid, stir, and temperature, at 100 DEG C～180 DEG C, keeps 1～10 hour, and solid-liquid divides
From, obtain solubility aluminum chloride or aluminum sulfate solution；Solid is amorphous silicon di-oxide.
Similarly, before implementing this step, can be first with the alumina content of conventional method detection product, to judge
The acid amount added.In some embodiments, reaction temperature can be 120～150 DEG C, and the time is 2～6 hours.
Aluminum chloride that this step obtains or aluminum sulfate solution usually contain ferrum.For obtaining pure aluminium oxide, the most first
Carry out except ferrum.This area conventional method can be used except ferrum.In a preferred embodiment, utilize except ferrum adsorbent resin is except ferrum.
3) aluminium salt in aluminum chloride or aluminum sulfate solution is changed into aluminium oxide.This can utilize methods known in the art
Carry out, such as, to liquor alumini chloridi or aluminum sulfate solution concentration, crystallization, roasting, obtain aluminium oxide.Chlorination produced by roasting
Hydrogen or sulfur trioxide gas can absorb with water, obtain hydrochloric acid or sulphuric acid.
Embodiment 1
Table 1: coal-powder boiler flyash
A. take table coal-powder boiler flyash 10g to activate with 10ml concentrated sulphuric acid (98%wt), under the conditions of 260 DEG C, be incubated 5 little
Time, it being warming up to 850 DEG C afterwards and be incubated 3 hours, cooling is taken out.The sulfur trioxide gas water of generation is absorbed extracting sulfuric acid；
B. the product after sulfuric acid baking activation being decomposed adds 25wt% hydrochloric acid 38 milliliters, and mix homogeneously is at politef
In liner reactor, take out after 140 DEG C are incubated 2 hours；
C. sour molten disposed slurry being carried out solid-liquid separation, solid is amorphous silicon di-oxide, and liquid is solubility aluminum chloride water
Solution；
D. by aluminum chloride aqueous solution by except ferrum resin absorption is except ferrum, temperature of charge is at 40 DEG C, and even velocity of flow, effluent is
Aluminum sulfate solution except ferrofining；
E. the solution condensing crystallizing after processing except ferrum, obtains crystal aluminum chloride；
F. being moved into by crystal aluminum chloride decomposes in kiln, and 850 DEG C of Roasting Decompositions are incubated 6 hours, the hydrogen chloride gas of generation
Absorb with water, obtain hydrochloric acid, after calcining and decomposing, obtain γ-Al2O3；
G. by γ-Al2O3Solid, calcines 2 hours through 1150 DEG C, obtains α-Al2O3。
After testing, alumina recovery rate reaches 89%.
Embodiment 2
A. take mullite powder 10g and 1.4ml concentrated sulphuric acid (98%wt) to mix, under the conditions of 300 DEG C, be incubated 3 hours；Afterwards
It is warming up to 870 DEG C and is incubated 2 hours；The sulfur trioxide gas water of generation is absorbed extracting sulfuric acid；
B. the product after sulfuric acid baking activation being decomposed adds 25wt% hydrochloric acid 50 milliliters, and mix homogeneously is at politef
In liner reactor, take out after 130 DEG C are incubated 3 hours；
C. sour molten disposed slurry being carried out solid-liquid separation, solid is amorphous silicon di-oxide, and liquid is solubility aluminum chloride water
Solution,
D. by aluminum chloride aqueous solution by except ferrum resin absorption is except ferrum, temperature of charge is at 40 DEG C, and even velocity of flow, effluent is
Aluminum sulfate solution except ferrofining；
E. the solution condensing crystallizing after processing except ferrum, obtains crystal aluminum chloride；
F. being moved into by crystal aluminum chloride decomposes in kiln, and 860 DEG C of Roasting Decompositions are incubated 3 hours, the hydrogen chloride gas of generation
Absorb with water, obtain hydrochloric acid, after calcining and decomposing, obtain γ-Al2O3；
G. by γ-Al2O3Solid, calcines 2 hours through 1150 DEG C, obtains α-Al2O3。
After testing, alumina recovery rate reaches 91%.
Embodiment 3
A. coal-powder boiler flyash 10g and the 1.0ml concentrated sulphuric acid in Example 1 mixes, and is incubated 3 little under the conditions of 280 DEG C
Time；It is warming up to 860 DEG C afterwards and is incubated 3 hours；The sulfur trioxide gas water of generation is absorbed extracting sulfuric acid；
B. the material after sulfuric acid baking activation being decomposed adds 30 milliliters of 30wt% sulphuric acid, and mix homogeneously is at politef
In liner reactor, take out after 130 DEG C are incubated 4 hours；
C. sour molten disposed slurry being carried out solid-liquid separation, solid is amorphous silicon di-oxide, and liquid is solubility aluminum sulfate salt
Aqueous solution；
D. by aluminum sulfate salt aqueous solution by recrystallization method remove impurity, crystallization, crystalline sulfuric acid aluminum is obtained；
F. being moved into by aluminum sulfate decomposes in kiln, and 870 DEG C of Roasting Decompositions are incubated 4 hours, and the sulfur trioxide gas of generation is used
Water absorbs, and obtains sulphuric acid, obtains γ-Al after calcining and decomposing2O3；
G. by γ-Al2O3Solid is calcined 2 hours through 1100 DEG C, obtains α-Al2O3。
After testing, alumina recovery rate is 92%.
Claims (8)
1. the method utilizing two-part acid reaction method to extract aluminium oxide, comprises the following steps:
1) generate 1～1.5 times of addition concentrated sulphuric acid of the theoretical amount of sulphuric acid required for aluminum sulfate by aluminium oxide in material and mix
Uniformly；Roasting 1～8 hours under the conditions of 240～315 DEG C, be warming up to 800～900 DEG C and keep 3-6 hour, cooling；
2) to step 1) product that obtains according to wherein alumina content, add reaction and generate required for aluminum chloride or aluminum sulfate
The hydrochloric acid of theoretical amount or sulphuric acid, stir, and temperature, at 100 DEG C～180 DEG C, keeps 1～10 hour, and solid-liquid separation, obtaining can
Dissolubility aluminum chloride or aluminum sulfate solution；
3) aluminium salt in aluminum chloride or aluminum sulfate solution is changed into aluminium oxide；
Wherein, any one during described material is coal-powder boiler flyash, mullite or high aluminosilicate.
Method the most according to claim 1, wherein, step 1) in, required for aluminium oxide generation aluminum sulfate in material
1～1.2 times of addition concentrated sulphuric acid of the theoretical amount of sulphuric acid.
Method the most according to claim 2, wherein, step 1) in, after adding concentrated sulphuric acid, under the conditions of 260～300 DEG C
Roasting 3～5 hours.
Method the most according to claim 3, wherein, step 2) in, temperature, at 120 DEG C～150 DEG C, keeps 2～6 hours.
5. according to the method described in any one of Claims 1 to 4, wherein, step 3) in, to liquor alumini chloridi or aluminum sulfate solution
Concentration, crystallization, roasting, obtain aluminium oxide.
Method the most according to claim 5, wherein to step 2) aluminum chloride that obtains or aluminum sulfate solution first carry out except ferrum.
Method the most according to claim 6, wherein, utilizes except ferrum adsorbent resin is except ferrum.
Method the most according to claim 5, wherein, for step 1) and 3) in roasting produce hydrogen chloride or sulfur trioxide
Gas uses water to absorb, and obtains hydrochloric acid or sulphuric acid.
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Cited By (6)
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| CN106966416A (en) * | 2017-04-11 | 2017-07-21 | 中国神华能源股份有限公司 | A kind of method that high purity aluminium oxide is extracted from coal-powder boiler flyash |
| CN108130432A (en) * | 2017-12-21 | 2018-06-08 | 武汉理工大学 | A kind of method of kaolin low-temperature activation Aluminum |
| CN108220630A (en) * | 2017-12-28 | 2018-06-29 | 中国神华能源股份有限公司 | A kind of method of the Extraction of rare earth from flyash |
| CN110759368A (en) * | 2019-11-29 | 2020-02-07 | 神华准能资源综合开发有限公司 | Method for extracting aluminum oxide by activating fly ash |
| CN111233014A (en) * | 2020-03-04 | 2020-06-05 | 神华准能资源综合开发有限公司 | Method for enhanced dissolution of fly ash |
| CN113044866A (en) * | 2019-12-26 | 2021-06-29 | 国家能源投资集团有限责任公司 | Method for preparing aluminum sulfate from aluminum-containing acid treatment liquid |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966416A (en) * | 2017-04-11 | 2017-07-21 | 中国神华能源股份有限公司 | A kind of method that high purity aluminium oxide is extracted from coal-powder boiler flyash |
| CN108130432A (en) * | 2017-12-21 | 2018-06-08 | 武汉理工大学 | A kind of method of kaolin low-temperature activation Aluminum |
| CN108130432B (en) * | 2017-12-21 | 2020-08-25 | 武汉理工大学 | Method for dissolving out aluminum by low-temperature activation of kaolin |
| CN108220630A (en) * | 2017-12-28 | 2018-06-29 | 中国神华能源股份有限公司 | A kind of method of the Extraction of rare earth from flyash |
| CN110759368A (en) * | 2019-11-29 | 2020-02-07 | 神华准能资源综合开发有限公司 | Method for extracting aluminum oxide by activating fly ash |
| CN113044866A (en) * | 2019-12-26 | 2021-06-29 | 国家能源投资集团有限责任公司 | Method for preparing aluminum sulfate from aluminum-containing acid treatment liquid |
| CN113044866B (en) * | 2019-12-26 | 2022-05-27 | 国家能源投资集团有限责任公司 | Method for preparing aluminum sulfate from aluminum-containing acid treatment liquid |
| CN111233014A (en) * | 2020-03-04 | 2020-06-05 | 神华准能资源综合开发有限公司 | Method for enhanced dissolution of fly ash |
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| CN106115751B (en) | 2017-08-25 |
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