CN108220603B - A kind of normal pressure alkali leaching-sulfuric acid curing-hot acid-leaching aluminium ash recovery process - Google Patents
A kind of normal pressure alkali leaching-sulfuric acid curing-hot acid-leaching aluminium ash recovery process Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B21/00—Obtaining aluminium
- C22B21/0015—Obtaining aluminium by wet processes
- C22B21/0023—Obtaining aluminium by wet processes from waste materials
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
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Abstract
The invention discloses a kind of normal pressure alkali leaching-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, specifically includes the following steps: aluminium ash is added to progress normal pressure alkali leaching in sodium carbonate liquor, concentrated sulfuric acid curing is added after the drying of alkali phase analysis, the gas generated in maturing process is absorbed with sodium aluminate alkali immersion liquid, liquid is obtained sodium aluminate, sodium chloride, sodium fluoride mixed crystallization body as aluminium founding slagging agent after evaporative crystallization is concentrated after absorption, alkali phase analysis after curing is added to progress pressurized acid leaching in acid autoclave with water and reacts, and pressurized acid leaching liquid is directly sold outside as aluminum sulfate product；High-temperature refractory is made in pressurized acid leaching slag after high temperature sintering.The present invention provides the innoxious Comprehensive recycle technologies of aluminium ash that a kind of nothing " three wastes " generate.
Description
Technical field
The invention belongs to aluminum smelting technology industry and its environmental technology fields, and in particular to a kind of normal pressure acidleach-sulfuric acid curing-adds
The aluminium ash recovery process of hot acid leaching.
Background technique
Aluminium ash is free of metal by the manual sorting of metallic aluminium, molten aluminum separation and recovery and ball milling residual Al ash after the recovery
Aluminium, the aluminium ash are called aluminium ash (as the aluminium ash of project raw material, referring to aluminium ash).Aluminium ash main component is aluminum oxide (Al2
O 3), chloride and fluoride, also containing have on a small quantity cell lining refractory material institute band silicon (Si) such as, sodium (Na), magnesium (Mg),
Calcium (Ca), and the ice crystal (Na of fusing3AlF6), aluminum fluoride (AlF) etc..Its yield is big, wherein soluble chloride and fluorine
Compound pollutes environment, belongs to dangerous waste slag.
Aluminium ash is increasingly valued by people as a kind of important aluminium secondary resource.The aluminium ash of fresh baked usually contains
There is 60% ~ 70% metallic aluminium, after conventional recovery processing, still containing the metallic aluminium of 10-15% in remaining aluminium scrap ash, leads to
Often the mode of landfill is taken to be handled, not only causes the waste of resource, while also resulting in the pollution of environment.Aluminium ash it is main at
It is divided into aluminum oxide, there is certain economic value, but how to recycle, but there is problem.By the continuous spy of many years
Rope, methods have been developed grey (slag) method of comprehensive utilization of many aluminium, such as recycle metallic aluminium, production aluminum sulfate, Brown Alundum, conjunction
At aluminium polychloride, synthetic ink aluminium oxide etc..
Above production method is unrealistic for aluminium manufacturing enterprise.Part aluminium manufacturing enterprise uses plant area
The mode of checking storehouse stockpiling, but being continuously increased with yield are built, processing pressure is big, and growing day by day.Also there is the production of part aluminium
Supporting industries situation of the enterprise according to periphery, the approach handled using the qualified professional Solid state fermentation producer of commission, processing
Outer committee's cost, increases the financial burden of aluminium manufacturing enterprise.China's aluminum current Slag treatment rate of recovery is low, and energy consumption is big and wastes
Greatly, new technology should be greatly developed and change this backward state using sophisticated equipment.Research and development is returned from industrial aluminum ash
The technology for receiving each valuable element, for improving, the economic benefit of enterprise, preserving the ecological environment has important meaning.
Summary of the invention
The purpose of the present invention is to provide a kind of normal pressure acidleach-sulfuric acid curing-hot acid-leaching aluminium ash recovery process.
The object of the present invention is achieved like this, including the leaching of normal pressure alkali, sulfuric acid curing, pressurized acid leaching and post-processing step,
It specifically includes:
A, normal pressure alkali soaks: the sodium hydroxide solution that raw material aluminium ash quality 20 ~ 100% is added in raw material aluminium ash is sized mixing,
40 ~ 90 DEG C of 0.5 ~ 8h of heat preservation are then heated to, normal pressure alkali immersion liquid a and normal pressure alkali phase analysis b is obtained by filtration；
B, sulfuric acid cures: the concentrated sulfuric acid that alkali phase analysis b mass 20 ~ 100% is added after alkali phase analysis b washing and drying is cured
Alkali phase analysis c is obtained, HF, HCl gas generated in maturing process is absorbed using normal pressure alkali immersion liquid a, after evaporative crystallization concentration
Obtain aluminium founding slagging agent；
C, pressurized acid leaching: alkali phase analysis c is placed in autoclave, and the water of 1 ~ 5 times of alkali phase analysis c volume is added, and is then added again
Entering the concentrated sulfuric acid to be adjusted to the mass percentage concentration of acid dip solution is 5 ~ 100%, is pressurizeed at 100 ~ 160 DEG C of temperature, 0.1 ~ 1MPa of pressure
1 ~ 8h of acid-leaching reaction obtains pressurized acid leaching liquid d and pressurized acid leaching slag e；Pressurized acid leaching liquid obtains aluminum sulfate after evaporative crystallization is concentrated
Product；
D, post-process: pressurized acid leaching slag e obtains high-temperature refractory after high temperature sintering.
The present invention develops a kind of with normal pressure alkali leaching-sulfuric acid curing-pressurization acid aiming at the problem that current aluminium ash treatment process
The comprehensive recycling process of leaching, the purpose of this technique be by aluminium ash Na, F, Cl and part Al alkali be dipped into solution, residue is few
The alkali phase analysis for measuring ice crystal is absorbed by the way that F is entered flue gas alkali immersion liquid with HF after sulfuric acid curing, the alkali phase analysis after sulfuric acid curing
Reacting with water progress pressurized acid leaching enters residual activity oxidation aluminium, magnesium, sodium, potassium, iron in pickle liquor, after acid leaching residue high temperature sintering
High-temperature refractory is made；Water, gas, solid three-phase material are all utilized effectively, provide a kind of nothing " three wastes " generate, environmental protection warp
The aluminium ash recovery method of Ji solves the problems, such as that F, Cl are polluted and be difficult to be utilized in aluminum current ash.
Positive effect caused by the present invention:
(1) F, Cl are transferred in sodium aluminate solution and by absorbing HF, HCl gas in sulfuric acid curing flue gas by the leaching of normal pressure alkali
Body, 95% or more F, Cl enter in alkali immersion liquid, have not only avoided the pollution of F, Cl to environment, but also can steam it with sodium aluminate solution
Aluminium founding use is made in hair crystallization, avoids environmental pollution while increasing economic benefit.
(2) alkali phase analysis is recycled by the way that F is all evaporate into flue gas after concentrated acid curing, avoids F in pressurized acid leaching liquid
Ion concentration is exceeded；
(3) reactive preferable aluminium oxide is all introduced into aluminum sulfate solution by pressurized acid leaching process as far as possible, is improved
The concentration of aluminum sulfate, in addition converts CaSO for Ca4Into in pressurized acid leaching slag.
(4) pressurized acid leaching slag passes through high temperature sintering for CaSO4In the crystallization water removing, aluminous refractory is made.
Detailed description of the invention
Fig. 1 is present invention process flow diagram.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is further illustrated, but is not subject in any way to the present invention
Limitation, based on present invention teach that it is made it is any transform or replace, all belong to the scope of protection of the present invention.
Normal pressure alkali leaching of the present invention-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, including the leaching of normal pressure alkali, sulphur
Acid curing, pressurized acid leaching and post-processing step, specifically include:
A, normal pressure alkali soaks: the sodium hydroxide solution that raw material aluminium ash quality 20 ~ 100% is added in raw material aluminium ash is sized mixing,
40 ~ 90 DEG C of 0.5 ~ 8h of heat preservation are then heated to, normal pressure alkali immersion liquid a and normal pressure alkali phase analysis b is obtained by filtration；
B, sulfuric acid cures: the concentrated sulfuric acid that alkali phase analysis b mass 20 ~ 100% is added after alkali phase analysis b washing and drying is cured
Alkali phase analysis c is obtained, HF, HCl gas generated in maturing process is absorbed using normal pressure alkali immersion liquid a, after evaporative crystallization concentration
Obtain aluminium founding slagging agent；
C, pressurized acid leaching: alkali phase analysis c is placed in autoclave, and the water of 1 ~ 5 times of alkali phase analysis c volume is added, and is then added again
Entering the concentrated sulfuric acid to be adjusted to the mass percentage concentration of acid dip solution is 5 ~ 100%, is pressurizeed at 100 ~ 160 DEG C of temperature, 0.1 ~ 1MPa of pressure
1 ~ 8h of acid-leaching reaction obtains pressurized acid leaching liquid d and pressurized acid leaching slag e；Pressurized acid leaching liquid obtains aluminum sulfate after evaporative crystallization is concentrated
Product；
D, post-process: pressurized acid leaching slag e obtains high-temperature refractory after high temperature sintering.
The additional amount of sodium hydroxide solution is the 25 ~ 50% of alkali phase analysis b mass in step A.
The mass percentage concentration of the sodium hydroxide solution is 10 ~ 30%.
The disengaging temperature that normal pressure alkali soaks in step A is 60 ~ 90 DEG C, and extraction time is 1 ~ 6h.
The additional amount of the concentrated sulfuric acid described in step B is the 50 ~ 100% of alkali phase analysis b mass.
The time cured in step B is 5 ~ 10h.
The mass percentage concentration of acid dip solution described in step C is 5 ~ 30%.
The temperature leached in step C is 120 ~ 160 DEG C.
The time that pressurized acid leaching reacts in step C is 2 ~ 6h.
The temperature of D step high temperature sintering is 1100 ~ 1400 DEG C.
Normal pressure alkali leaching of the present invention-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, concrete operations are as follows:
1, aluminium ash and sodium hydroxide solution (naoh concentration is 5 ~ 50%) 1:20 in mass ratio that aluminium founding generates ~
100% sizes mixing, and stirred tank is added after sizing mixing, and is warming up to (40 ~ 90 DEG C) 0.5 ~ 8h of reaction of reaction temperature and alkali immersion liquid and alkali is obtained by filtration
Phase analysis.The leaching key reaction of normal pressure alkali has:
2NaOH+ Al2O3=2NaAlO2+H2O (1)
2, contain NaF, NaCl, NaAlO in alkali immersion liquid2Deng；Concentrated sulfuric acid curing is added after alkali phase analysis washing and drying, due to dense
Sour maturing process aluminium oxide and sodium fluoride etc. and sulfuric acid reaction heat release, volatilization are generated HF, HCl gas and are inhaled using alkali immersion liquid
It receives, NaF, NaCl is obtained after absorption, with NaF, NaCl, NaAlO in alkali leaching liquor2Deng after being evaporated crystallization concentration together
Aluminium founding slagging agent is made.
3, the slag after sulfuric acid curing is added to progress pressurized acid leaching in autoclave with water and reacts, and high temperature and pressure is utilized to accelerate oxygen
Change the dissolution of aluminium, purpose as far as possible all leaches into active oxidation aluminum portions in solution, and leachate mainly contains aluminum sulfate, makees
It is sold for aluminum sulfate solution is directly outer.Pressurized acid leaching is reacted such as formula (2)-(5):
Al2O3+3H2SO4=Al2(SO4)3+3 H2O (2)
2NaF +H2SO4=Na2SO4+ 2 HF (3)
2Na3AlF6+6H2SO4=3Na2SO4+12 HF + Al2(SO4)3(4)
CaO+H2SO4=CaSO4+ H2O (5)
4, aluminium oxide, calcium sulfate, silica have been contained only in pressurized acid leaching slag, since three kinds of melting point compounds are higher,
High temperature sintering (1100-1400 DEG C) is used as high-temperature refractory afterwards.
Case is embodied, the present invention will be further described below:
Embodiment 1
The present embodiment aluminium ash component such as following table
| Ingredient | Al2O3 | Na | F | Cl | CaO | K | MgO | Fe | SiO2 |
| Content/% | 73.21 | 10.97 | 5.57 | 6.53 | 0.39 | 0.033 | 1.02 | 0.06 | 0.83 |
(1) by 100kg aluminium ash and 200L sodium hydroxide solution (concentration of sodium hydroxide solution 10%) be added in stirred tank into
The leaching of row alkali, is warming up to 85 DEG C of soaking time 4h, the sodium aluminate solution 185.31L of the fluorine-containing chlorine of output, ammonium acetate Al2O3
79.15g/L、Na 93.08g/L、Cl 35.21g/L、F 18.06 g/L、K0.17g/L、SiO20.1g/L；Leach slag ingredient
For Al2O3 91.18%、Na 3.44%、F 3.49%、Cl 0.2%、SiO2 1.03%, CaO 0.62%, Fe 0.09%, output leach
Slag amount 63.82kg.
(2) curing of the 31.91kg concentrated sulfuric acid is added in 63.82kg alkali phase analysis in a kettle, and concentrated acid curing condition: room temperature is normal
Pressure, time 6h, HF, HCl flue gas of output are absorbed by alkali immersion liquid；Water 191.46L, dense is added after curing in compressive reaction kettle
Sulfuric acid 6.38kg is warming up to 140 DEG C, heat preservation 3h, pressure 0.25MPa, and solid-liquor separation obtains pressurized acid leaching liquid after reaction
182.3L and pressurized acid leaching slag 41.53kg, pressurized acid leaching liquid ingredient are (g/L): Al2(SO4)3542.32(Al2O3 161.70),
Na 18.75、SiO2 0.01,0.36 Fe can be used as industrial II class aluminum sulfate solution and sell；Pressure leaching slag ingredient (%):
Al2O3 97.41、CaO 0.96、SiO2 1.62, aluminous refractory is made after 1200 DEG C of high temperature sinterings in 0.01 Fe.
(3) crystal 44.95kg is obtained after the concentration of normal pressure alkali immersion liquid evaporative crystallization, ingredient is (%): Al2O3 33.28、Na
39.14、Cl 14.81、F 12.66、K 0.04、SiO20.04；The crystalline solid can be used as the slag hitting in aluminium fusion-casting process completely
Agent uses.
Embodiment 2
The present embodiment aluminium ash component such as following table
| Ingredient | Al2O3 | Na | F | Cl | CaO | K | MgO | Fe | SiO2 |
| Content/% | 67.33 | 12.71 | 6.22 | 8.01 | 0.55 | 0.017 | 2.03 | 0.11 | 1.42 |
(1) by 150kg aluminium ash and 450L sodium hydroxide solution (concentration of sodium hydroxide solution 5%) be added in stirred tank into
The leaching of row alkali, is warming up to 60 DEG C of soaking time 6h, the sodium aluminate solution 410.24L of the fluorine-containing chlorine of output, ammonium acetate Al2O3
50.48g/L、Na 104.95g/L、Cl 30.03g/L、F 13.99g/L、K0.09g/L、SiO20.21g/L；Leach slag ingredient
For Al2O3 89.57%、Na 4.25%、F 4.16%、Cl 0.14%、SiO2 1.22%, CaO 0.65%, Fe 0.13%, output leaching
Quality of slagging tap 89.64kg.
(2) curing of the 71.71kg concentrated sulfuric acid is added in 89.64kg alkali phase analysis in a kettle, and concentrated acid curing condition: room temperature is normal
Pressure, time 4h, HF, HCl flue gas of output are absorbed by alkali immersion liquid；Water 179.28L, dense is added after curing in compressive reaction kettle
Sulfuric acid 13.45kg is warming up to 160 DEG C, heat preservation 2h, pressure 0.4MPa, and solid-liquor separation obtains pressurized acid leaching liquid after reaction
165.21L and pressurized acid leaching slag kg, pressurized acid leaching liquid ingredient are (g/L): Al2(SO4)3510.87(Al2O3 152.32), Na
21.28、SiO2 0.008,0.41 Fe can be used as industrial II class aluminum sulfate solution and sell；Pressure leaching slag ingredient (%):
Al2O3 94.90、CaO 1.45、SiO2 3.62, aluminous refractory is made after 1400 DEG C of high temperature sinterings in 0.02 Fe.
(3) crystal 87.39kg is obtained after the concentration of normal pressure alkali immersion liquid evaporative crystallization, ingredient is (%): Al2O3 23.68、Na
49.24、Cl 14.09、F 12.85、K0.04、SiO20.08；The crystalline solid can be used as the slagging agent in aluminium fusion-casting process completely
It uses.
Claims (10)
1. a kind of normal pressure alkali leaching-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that including the leaching of normal pressure alkali, sulphur
Acid curing, pressurized acid leaching and post-processing step, specifically include:
A, normal pressure alkali soaks: the sodium hydroxide solution that aluminium ash quality 20 ~ 100% is added in the aluminium ash that raw material aluminium founding is generated carries out
It sizes mixing, concentration of sodium hydroxide solution is 5 ~ 50%, then heats to 40 ~ 90 DEG C of 0.5 ~ 8h of heat preservation, normal pressure alkali immersion liquid a is obtained by filtration
With normal pressure alkali phase analysis b；
B, sulfuric acid cures: the concentrated sulfuric acid that alkali phase analysis b mass 20 ~ 100% is added after alkali phase analysis b washing and drying is cured to obtain
Alkali phase analysis c, HF, HCl gas generated in maturing process are absorbed using normal pressure alkali immersion liquid a, are obtained after evaporative crystallization concentration
Aluminium founding slagging agent；
C, pressurized acid leaching: alkali phase analysis c is placed in autoclave, and the water of 1 ~ 5 times of alkali phase analysis c volume is added, then adds dense
The mass percentage concentration that sulfuric acid is adjusted to acid dip solution is 5 ~ 100%, the pressurized acid leaching at 100 ~ 160 DEG C of temperature, 0.1 ~ 1MPa of pressure
1 ~ 8h of reaction obtains pressurized acid leaching liquid d and pressurized acid leaching slag e；Pressurized acid leaching liquid obtains aluminum sulfate production after evaporative crystallization is concentrated
Product；
D, post-process: pressurized acid leaching slag e obtains high-temperature refractory after high temperature sintering.
2. normal pressure alkali leaching according to claim 1-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that A
The additional amount of sodium hydroxide solution is the 25 ~ 50% of alkali phase analysis b mass in step.
3. normal pressure alkali leaching according to claim 1 or 2-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, feature exist
In the sodium hydroxide solution mass percentage concentration be 10 ~ 30%.
4. normal pressure alkali leaching according to claim 1-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that A
The disengaging temperature that normal pressure alkali soaks in step is 60 ~ 90 DEG C, and extraction time is 1 ~ 6h.
5. normal pressure alkali leaching according to claim 1-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that B
The additional amount of the concentrated sulfuric acid described in step is the 50 ~ 100% of alkali phase analysis b mass.
6. normal pressure alkali leaching according to claim 1-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that B
The time cured in step is 5 ~ 10h.
7. normal pressure alkali leaching according to claim 1-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that C
The mass percentage concentration of acid dip solution described in step is 5 ~ 30%.
8. normal pressure alkali leaching according to claim 1-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that C
The temperature leached in step is 120 ~ 160 DEG C.
9. normal pressure alkali leaching according to claim 1-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that C
The time that pressurized acid leaching reacts in step is 2 ~ 6h.
10. normal pressure alkali leaching according to claim 1-sulfuric acid curing-pressurized acid leaching aluminium ash recovery process, it is characterised in that
The temperature of D step high temperature sintering is 1100 ~ 1400 DEG C.
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| CN108707752B (en) * | 2018-07-05 | 2019-10-11 | 郑州中科新兴产业技术研究院 | A method of recycling vanadium and fluorine from Quadratic aluminum dust |
| CN108950227A (en) * | 2018-09-17 | 2018-12-07 | 云南云铝润鑫铝业有限公司 | A kind of aluminium ash pressurization normal pressure innocuity disposal system and processing method |
| CN111017972B (en) * | 2019-12-17 | 2022-08-05 | 沈阳北冶冶金科技有限公司 | Resource separation and recycling method of aluminum ash |
| CN112110738A (en) * | 2020-09-24 | 2020-12-22 | 西南科技大学 | Method for preparing high-alumina refractory material from aluminum ash |
| CN112340759A (en) * | 2020-10-21 | 2021-02-09 | 斯瑞尔环境科技股份有限公司 | Method for preparing polyaluminum chloride and recovering silicon simple substance by using secondary aluminum ash |
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| CN103555955B (en) * | 2013-11-13 | 2015-04-22 | 昆明冶金研究院 | Resource utilization method of aluminum ash |
| CN104445312B (en) * | 2014-10-30 | 2016-03-02 | 北京矿冶研究总院 | Method for extracting aluminum oxide by synergistic treatment of fly ash and coal gangue |
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