CN101838000A - Method for producing metallurgical aluminum oxide by using iron-containing solution of aluminum chloride - Google Patents
Method for producing metallurgical aluminum oxide by using iron-containing solution of aluminum chloride Download PDFInfo
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- CN101838000A CN101838000A CN201010161885A CN201010161885A CN101838000A CN 101838000 A CN101838000 A CN 101838000A CN 201010161885 A CN201010161885 A CN 201010161885A CN 201010161885 A CN201010161885 A CN 201010161885A CN 101838000 A CN101838000 A CN 101838000A
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- hydrochloric acid
- aluminum oxide
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 76
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 46
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000011347 resin Substances 0.000 claims abstract description 61
- 229920005989 resin Polymers 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 50
- 239000013078 crystal Substances 0.000 claims description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 239000003480 eluent Substances 0.000 claims description 14
- 230000008929 regeneration Effects 0.000 claims description 12
- 238000011069 regeneration method Methods 0.000 claims description 12
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 5
- 230000008719 thickening Effects 0.000 claims description 5
- 150000001768 cations Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 125000002091 cationic group Chemical group 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 12
- 238000002425 crystallisation Methods 0.000 abstract description 5
- 230000008025 crystallization Effects 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 20
- 239000000126 substance Substances 0.000 description 14
- 239000004615 ingredient Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 229910001570 bauxite Inorganic materials 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 238000011017 operating method Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000000274 adsorptive effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229940037003 alum Drugs 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 229910052622 kaolinite Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a method for producing metallurgical aluminum oxide by using iron-containing solution of aluminum chloride as a raw material, which comprises: 1, introducing the iron-containing solution of aluminum chloride to a resin column to obtain refined solution of aluminum chloride; 2, concentrating the refined solution obtained by the step 1 under vacuum, cooling the concentrated liquid, and performing crystallization and solid-liquid separation to obtain crystalline aluminum chloride; and 3, calcining the crystalline aluminum chloride obtained by the step 2 to obtain a metallurgical aluminum oxide product. The method has the advantages of simple production process, easy production process control, low production cost and stable product quality.
Description
Technical field
The present invention relates to a kind of technology of producing aluminum oxide, especially is the technology of raw material production metallurgical-grade aluminum oxide with the iron content liquor alumini chloridi.
Background technology
Metallurgical-grade aluminum oxide is the important source material that is used for the electrolysis production metallic aluminium.In industrial production, all metallurgical-grade aluminum oxide products all obtain from alkali systems at present, and the sodium aluminate solution that is about to alkalescence makes aluminium hydroxide by the method that kind of branch or carbon divide, then through calcining preparation metallurgical-grade aluminum oxide.It is low to have iron-holder via the aluminum oxide of alkali systems preparation, and production technique is simple relatively, and energy consumption is low, to advantages such as the corrodibility of equipment are little, is fit to large-scale commercial production.It is produced the raw material that aluminum oxide adopted and is mainly bauxite.
Along with the rapid expansion of Chinese aluminum oxide production capacity, the demand of bauxite also increases substantially.According to US Geological Survey (USGS) statistics, China's explored reserves of bauxite at present is 700,000,000 tons, to the demand status of bauxite, can only keep about 20 years production according at present.In addition, Chinese most bauxite exploitation and smelting difficulty are big.In order to keep the ordinary production of aluminum oxide enterprise, China needs a large amount of bauxite of import every year.
Along with the exhaustion day by day of bauxite resource and the rapid expansion of aluminum oxide production capacity, adopting other aluminum-containing mineral or containing waste slag of aluminum is that raw material extracts aluminum oxide, is that the useful of alumina producing replenished.Because these raw materials are different with the chemical constitution and the reactive behavior of bauxite, in extracting alumina process, adopt acid system sometimes, promptly prepare aluminum oxide via tart aluminum chloride or alum liquor.
" a kind of preparation method of alumina " disclosed as patent CN200610017139.2, the employing circulating fluid bed coal ash is a raw material, through hydrochloric acid or sulfuric acid dissolution, make aluminum chloride/alum liquor, prepare metallurgical-grade aluminum oxide through condensing crystal, calcining, the molten deironing of alkali again.
Patent CN1107807 discloses " preparing aluminium hydroxide technology with coal gangue ", is raw material with the coal gangue, obtains wherein aluminum oxide with hydrochloric acid or sulfuric acid to leach.
Patent CN1334240 discloses " utilizing kaolinite (soil) to produce the technology of ultrapure aluminum oxide ", and kaolinite (soil) and acid-respons are generated aluminum salt solution, removes impurity such as de-iron, titanium again with alkali reaction.More than these methods all be with aluminum-containing mineral or to contain waste slag of aluminum be raw material, extract aluminum oxide through acid system.Advantages such as it is simple that acid system has technology, and energy consumption is low, and the waste residue amount is few.But in acidic solution, impurity such as iron exist with highly stable ionic species, are difficult to remove, so contain impurity such as more iron in the alumina product of acid system preparation usually.At this problem, deironing in basic solution usually, it is molten to be about to the aluminum oxide alkali that acid system obtains, and make it to change into soluble sodium metaaluminate, and iron becomes ferric hydroxide precipitate, through solid-liquid separation iron is removed.Address in three patents as the front and all to adopt this method deironing.This technology of acid back alkali earlier that adopts makes complex manufacturingization, has also increased production cost.Therefore, exploitation is a kind of is that the method for raw material direct production metallurgical-grade aluminum oxide is significant with ferruginous acid chlorization aluminum solutions.
Summary of the invention
The objective of the invention is at above-mentioned the deficiencies in the prior art, providing a kind of is the method for feedstock production metallurgical-grade aluminum oxide with the liquor alumini chloridi, and wherein liquor alumini chloridi contains iron.
Provided by the present invention is the method for feedstock production metallurgical-grade aluminum oxide with the iron content liquor alumini chloridi, may further comprise the steps:
(1) the iron content liquor alumini chloridi is fed the resin column deironing, make refined crystalline aluminium chloride liquid;
(2) step (1) gained refined liquid is carried out negative pressure and concentrate, the liquid after concentrating obtains crystal aluminum chloride after cooling, crystallization, solid-liquid separation;
(3) the resulting crystal aluminum chloride calcining of step (2) is obtained the metallurgical-grade aluminum oxide product.
In the step of the method for the invention (1): the iron content liquor alumini chloridi is fed the macroporous type cationic resin column carry out degree of depth deironing, make refined crystalline aluminium chloride liquid, treatment temp is room temperature～90 ℃, and preferable range is 60～80 ℃; The pickling liquor flow velocity be 1～4 times of resin volume/hour, preferable range be 2～3 times of resin volumes/hour; The mode that goes out on advancing below the pickling liquor during processing is by resin column, and solution is piston-like and upwards flows in the resin space.Resin column can adopt the mode of single-column or twin columns polyphone.
Described macroporous type resin cation (R.C.) can be selected D001,732,742,7020H, 7120H, JK008 or SPC-1 resin for use.
After described macroporous type resin cation (R.C.) absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent adopts the hydrochloric acid of water or 2～10wt%, and preferable range is 3～5wt%; Eluting temperature is room temperature～60 ℃, and the eluent consumption is 1～3 times of resin volume, the eluent flow velocity be 1～3 times of resin volume/hour, eluent passes through resin column in the enterprising mode that goes out down during wash-out; Adopt the hydrochloric acid of 2～10wt% during regeneration, preferable range is 3～5wt%, and temperature is room temperature～60 ℃, and the hydrochloric acid consumption is 1～2 times of resin volume, the hydrochloric acid flow velocity be 1～3 times of resin volume/hour, hydrochloric acid passes through resin column in the enterprising mode that goes out down during regeneration.
In the described step (2): step (1) gained refined liquid is carried out negative pressure concentrate, concentrate pressure and be-0.03～-0.07MPa, preferable range is-0.04～-0.06MPa; Thickening temperature is 50～110 ℃, and preferable range is 70～80 ℃; Liquid cooling after concentrating is separated out crystal aluminum chloride, obtains the crystal aluminum chloride product through solid-liquid separation.
In the described step (2), in when cooling, the crystal weight that control is separated out account for the former weight of refined crystalline aluminium chloride liquid 40～65% between, most of aluminum chloride crystallization is separated out, and impurity such as minute quantity iron(ic) chloride are still stayed in the middle of the solution because concentration is lower.The residue mother liquor returns refined liquid condensing crystal again.When Recycling Mother Solution arrives certain number of times, when foreign matter content is higher, need carries out the resin deironing again to mother liquor and handle, or use it for anything else in addition.
Described solid-liquid separation can adopt the routine operation method, uses centrifugation or vacuum belt filter.
In the described step (3): at 900～1200 ℃, preferable range is 950～1100 ℃, carries out calcining and decomposing, obtains the metallurgical-grade aluminum oxide product with the crystal aluminum chloride product that obtains in the step (2).
Described calcining can be adopted one-part form calcining or sectional type calcining.One-part form calcining is that calcination time 1～4 hour obtains alumina product after the thermolysis with crystal aluminum chloride direct heating to 900～1200 ℃.The sectional type calcining is at first crystal aluminum chloride to be heated 1～2 hour at 300～500 ℃, and most of crystal aluminum chloride is decomposed, and is warming up to 900～1200 ℃ of calcinings 1～3 hour then, obtains alumina product.
The beneficial effect that the present invention had is that compared with prior art, production technique is simple, production process is easy to control, low, the constant product quality of production cost.The present invention selects for use the iron content liquor alumini chloridi as raw material, adopts the method deironing of resin absorption, compares with the technology of alkaline process deironing in the past, and this method operation steps is simple, production cost is low, good iron removal effect.Utilize the resulting alumina product of method of the present invention, its Al
2O
3Content is not less than 98.9wt%, Fe
2O
3Content is not higher than 0.004wt%, SiO
2Content is not higher than 0.02wt%, Na
2O content is not higher than 0.08wt%, all reaches or is higher than in People's Republic of China's non-ferrous metal industry standard " (YS/T 274-1998 aluminum oxide " purity requirement to the metallurgical-grade aluminum oxide first grade.Fe wherein
2O
3And Na
2O content is than the low several times of 0.02wt%, 0.5wt% of standard.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Further describe method of the present invention with the following examples in conjunction with the accompanying drawings, but therefore the present invention is not subjected to any restriction.
Embodiment 1
Chemical ingredients of table 1 liquor alumini chloridi (g/L) and pH value
| Composition | ??Al 2O 3 | ??Fe 2O 3 | ??SiO 2 | ??TiO 2 | ??CaO | ??MgO | ??K 2O | ??Na 2O | ??pH |
| Solution 1 | ??85.60 | ??1.09 | ??0.11 | ??0.005 | ??0.97 | ??0.44 | ??0.64 | ??0.074 | ??1.6 |
| Solution 2 | ??107.10 | ??2.24 | ??0.19 | ??0.009 | ??1.12 | ??0.65 | ??0.48 | ??0.067 | ??1.3 |
(1), be 1.6 with the pH value, aluminium content (in aluminum oxide) is 85.60g/L, iron level (in ferric oxide) is that the liquor alumini chloridi of 1.09g/L is a raw material, its chemical ingredients is as shown in table 1.Resin column with D001 (Wan Dong chemical plant, Anhui) resin is housed carries out deironing with the mode of single-column, during processing the pickling liquor flow velocity be 2 times of resin volumes/hour, 60 ℃ of treatment temps obtain refined crystalline aluminium chloride liquid;
After resin absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: it is the hydrochloric acid of 4wt% that eluent adopts concentration, and eluting temperature is 50 ℃, the hydrochloric acid flow velocity be resin 1 times of volume/hour, adopt the eluent of 2 times of resin volumes to carry out wash-out altogether; Adopting concentration during regeneration is the hydrochloric acid of 4wt%, and temperature is 30 ℃, the hydrochloric acid flow velocity be resin 2 times of volumes/hour, adopt the hydrochloric acid of 1 times of resin volume to regenerate altogether.
(2), the refined crystalline aluminium chloride liquid with step (1) gained carries out evaporation concentration, pressure is-0.04MPa when concentrating, and 80 ℃ of thickening temperatures are through concentrating postcooling, crystallization, the crystal that control is separated out accounts for 65% of the former weight of aluminum chloride liquid, obtains crystal aluminum chloride through solid-liquid separation.
(3) step (2) gained crystal aluminum chloride was calcined 2 hours at 400 ℃, 1100 ℃ of calcinings 2 hours, obtained aluminum oxide then.After measured, the chemical ingredients of alumina product is as shown in table 2.
Embodiment 2
Except that step (1), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in the step (1) is adjusted into:
(1) with the iron content liquor alumini chloridi with the resin column of 732 (Anhui Samsung resin Science and Technology Ltd.) resin is housed, carry out deironing with the mode of twin columns polyphone, during processing the pickling liquor flow velocity be 4 times of resin volumes/hour, obtain refined crystalline aluminium chloride liquid;
After resin absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent adopts water, and eluting temperature is 60 ℃, water flow velocity be resin 1 times of volume/hour, adopt the eluent of 3 times of resin volumes to carry out wash-out altogether; Adopting concentration during regeneration is the hydrochloric acid of 6wt%, and temperature is 50 ℃, the hydrochloric acid flow velocity be resin 3 times of volumes/hour, adopt the hydrochloric acid of 2 times of resin volumes to regenerate altogether.
After measured, the chemical ingredients of alumina product is as shown in table 2.
Embodiment 3
The employed resin of step (1) among the embodiment 2 is changed to JK008 (Wan Dong chemical plant, Anhui) resin, and other processing condition are constant.
After resin absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: it is the hydrochloric acid of 8wt% that eluent adopts concentration, and eluting temperature is 30 ℃, the hydrochloric acid flow velocity be 2 times of resin volumes/hour, adopt the eluent of 1 times of resin volume to carry out wash-out altogether; Adopting concentration during regeneration is the hydrochloric acid of 2wt%, and temperature is a room temperature, the hydrochloric acid flow velocity be resin 2 times of volumes/hour, adopt the hydrochloric acid of 1 times of resin volume to regenerate altogether.
After measured, the chemical ingredients of alumina product is as shown in table 2.
Embodiment 4
Except that step (2), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in the step (2) is adjusted into:
(2) the refined crystalline aluminium chloride liquid with step (1) gained carries out evaporation concentration, pressure is-0.06MPa when concentrating, and 70 ℃ of thickening temperatures concentrate postcooling, crystallization, the crystal that control is separated out accounts for 40% of the former weight of aluminum chloride liquid, obtains crystal aluminum chloride through solid-liquid separation.
After measured, the chemical ingredients of alumina product is as shown in table 2.
Embodiment 5
Except that step (3), other operating procedure conditions are all identical with embodiment 1.Operating procedure condition in the step (3) is adjusted into:
(3) crystal aluminum chloride that obtains in the step (2) was obtained alumina product in 2 hours 1100 ℃ of calcinings.
After measured, the chemical ingredients of alumina product is as shown in table 2.
Embodiment 6
It is 1.3 that liquor alumini chloridi among the embodiment 1 is changed to the pH value, and aluminium content (in aluminum oxide) is 107.10g/L, iron level (in ferric oxide) be the liquor alumini chloridi of 2.24g/L as raw material, its chemical ingredients is as shown in table 1.Other operating procedure condition is constant.
After measured, the chemical ingredients of alumina product is as shown in table 2.
The comparative example
Step (1) is omitted with embodiment 1 in step (2), (3), i.e. liquor alumini chloridi directly condensing crystal, calcining without the resins exchange deironing obtains alumina product.
After measured, the chemical ingredients of alumina product is as shown in table 2.
The chemical ingredients of table 2 alumina product
| Embodiment 1 | ??99.2 | ??0.018 | ??0.002 | ??0.06 | ??0.7 |
| Embodiment 2 | ??99.1 | ??0.019 | ??0.004 | ??0.08 | ??0.8 |
| Embodiment 3 | ??99.1 | ??0.019 | ??0.003 | ??0.07 | ??0.8 |
| Embodiment 4 | ??99.2 | ??0.015 | ??0.002 | ??0.05 | ??0.7 |
| Embodiment 5 | ??98.9 | ??0.020 | ??0.004 | ??0.07 | ??1.0 |
| Embodiment 6 | ??99.1 | ??0.019 | ??0.004 | ??0.05 | ??0.8 |
| The comparative example | ??95.3 | ??0.020 | ??3.525 | ??0.07 | ??1.1 |
Annotate: Al
2O
3Content is 100% to deduct the surplus of listed impurity summation in the table.
Claims (10)
1. one kind with iron content liquor alumini chloridi production method of alumina, it is characterized in that described method comprises:
(1): the iron content liquor alumini chloridi is fed the macroporous type cationic resin column carry out deironing, make refined crystalline aluminium chloride liquid, treatment temp is room temperature～90 ℃; The pickling liquor flow velocity be 1～4 times of resin volume/hour; The mode that goes out on advancing below the pickling liquor during processing is passed through resin column;
(2): step (1) gained refined crystalline aluminium chloride liquid is carried out negative pressure concentrate, concentrate pressure and be-0.03～-0.07MPa, thickening temperature is 50～110 ℃; Liquid cooling after concentrating is separated out crystal aluminum chloride, through solid-liquid separation, obtains the crystal aluminum chloride product;
(3): the crystal aluminum chloride product that obtains in the step (2) is carried out calcining and decomposing at 900～1200 ℃, calcination time 1～4 hour; Or with crystal aluminum chloride 300～500 ℃ the heating 1～2 hour, be warming up to then 900～1200 ℃ the calcining 1～3 hour, obtain the metallurgical-grade aluminum oxide product.
2. method according to claim 1 is characterized in that, the treatment temp in the step (1) is 60～80 ℃.
3. method according to claim 1 is characterized in that, in the step (1) the pickling liquor flow velocity be 2～3 times of resin volumes/hour.
4. method according to claim 1 is characterized in that, resin column adopts the mode of single-column or twin columns polyphone.
5. method according to claim 1 is characterized in that, the macroporous type resin cation (R.C.) is D001,732,742,7020H, 7120H, JK008 or SPC-1.
6. method according to claim 1, it is characterized in that, after the absorption of macroporous type resin cation (R.C.), it is carried out wash-out and regeneration, and elution requirement is: eluent adopts the hydrochloric acid of water or 2～10wt%, is preferably 3～5wt%, eluting temperature is room temperature～60 ℃, the eluent consumption is 1～3 times of resin volume, the eluent flow velocity be 1～3 times of resin volume/hour, eluent passes through resin column in the enterprising mode that goes out down during wash-out; Adopt the hydrochloric acid of 2～10wt% during regeneration, be preferably 3～5wt%, temperature is room temperature～60 ℃, and the hydrochloric acid consumption is 1～2 times of resin volume, the hydrochloric acid flow velocity be 1～3 times of resin volume/hour, hydrochloric acid passes through resin column in the enterprising mode that goes out down during regeneration.
7. method according to claim 1 is characterized in that, concentrate pressure in the step (2) and be-0.04～-0.06MPa, thickening temperature is 70～80 ℃.
8. method according to claim 1 is characterized in that, the crystal aluminum chloride weight that cooling is separated out in the step (2) accounts for 40%～65% of the former weight of refined crystalline aluminium chloride liquid.
9. method according to claim 1 is characterized in that, solid-liquid separation adopts centrifugation or vacuum belt filter in the step (2).
10. method according to claim 1 is characterized in that, calcination temperature range is 950～1100 ℃ in the step (3).
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010161885A CN101838000A (en) | 2010-04-27 | 2010-04-27 | Method for producing metallurgical aluminum oxide by using iron-containing solution of aluminum chloride |
| CN 201110104102 CN102153118A (en) | 2010-04-27 | 2011-04-25 | Method for producing metallurgical-grade aluminum oxide by using iron-containing aluminum chloride solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010161885A CN101838000A (en) | 2010-04-27 | 2010-04-27 | Method for producing metallurgical aluminum oxide by using iron-containing solution of aluminum chloride |
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| CN 201110104102 Pending CN102153118A (en) | 2010-04-27 | 2011-04-25 | Method for producing metallurgical-grade aluminum oxide by using iron-containing aluminum chloride solution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092751A (en) * | 2010-11-19 | 2011-06-15 | 西安三瑞实业有限公司 | Method for preparing aluminum oxide and co-producing hydrochloric acid from aluminum chloride hexahydrate through pyrolytic crystallization |
| CN104507868A (en) * | 2012-08-01 | 2015-04-08 | 俄罗斯工程技术中心 | Method for producing alumina |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
| CN107827135A (en) * | 2017-12-04 | 2018-03-23 | 朱晓燕 | A kind of preparation method of high-purity superfine alumina powder |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4107266A (en) * | 1977-07-22 | 1978-08-15 | The United States Of America As Represented By The Secretary Of The Interior | Production of pure alumina from iron contaminated sulfate liquors |
| AU553950B2 (en) * | 1981-04-29 | 1986-07-31 | Comalco Aluminium Limited | Recovery of alumina from aluminous ores |
| US4652433A (en) * | 1986-01-29 | 1987-03-24 | Florida Progress Corporation | Method for the recovery of minerals and production of by-products from coal ash |
| US4710369A (en) * | 1986-06-10 | 1987-12-01 | Toth Aluminum Corporation | Oxidation method for production of special aluminas from pure aluminum chloride |
| CN1083023A (en) * | 1992-08-25 | 1994-03-02 | 王海舟 | Improved acid eduction process for producing alumina |
-
2010
- 2010-04-27 CN CN201010161885A patent/CN101838000A/en active Pending
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2011
- 2011-04-25 CN CN 201110104102 patent/CN102153118A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092751A (en) * | 2010-11-19 | 2011-06-15 | 西安三瑞实业有限公司 | Method for preparing aluminum oxide and co-producing hydrochloric acid from aluminum chloride hexahydrate through pyrolytic crystallization |
| CN102092751B (en) * | 2010-11-19 | 2013-04-03 | 西安三瑞实业有限公司 | Method for preparing aluminum oxide and co-producing hydrochloric acid from aluminum chloride hexahydrate through pyrolytic crystallization |
| CN104507868A (en) * | 2012-08-01 | 2015-04-08 | 俄罗斯工程技术中心 | Method for producing alumina |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
| CN107827135A (en) * | 2017-12-04 | 2018-03-23 | 朱晓燕 | A kind of preparation method of high-purity superfine alumina powder |
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| CN102153118A (en) | 2011-08-17 |
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