CN113562771A - Full-quantization integral utilization method for recycling iron, sodium and tailings from Bayer process red mud step by step - Google Patents
Full-quantization integral utilization method for recycling iron, sodium and tailings from Bayer process red mud step by step Download PDFInfo
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- CN113562771A CN113562771A CN202110848858.3A CN202110848858A CN113562771A CN 113562771 A CN113562771 A CN 113562771A CN 202110848858 A CN202110848858 A CN 202110848858A CN 113562771 A CN113562771 A CN 113562771A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 75
- 239000011734 sodium Substances 0.000 title claims abstract description 65
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 51
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 45
- 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 title claims abstract description 31
- 238000004064 recycling Methods 0.000 title claims abstract description 25
- 238000004131 Bayer process Methods 0.000 title claims abstract description 24
- 238000013139 quantization Methods 0.000 title description 2
- 238000002386 leaching Methods 0.000 claims abstract description 61
- 239000007787 solid Substances 0.000 claims abstract description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 13
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000000919 ceramic Substances 0.000 claims abstract description 10
- 239000012065 filter cake Substances 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 5
- 239000007832 Na2SO4 Substances 0.000 claims abstract description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 4
- 239000006104 solid solution Substances 0.000 claims abstract description 4
- 238000001238 wet grinding Methods 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 238000011084 recovery Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 239000011449 brick Substances 0.000 claims description 9
- 239000000292 calcium oxide Substances 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 230000001276 controlling effect Effects 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 239000002440 industrial waste Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- NJFMNPFATSYWHB-UHFFFAOYSA-N ac1l9hgr Chemical compound [Fe].[Fe] NJFMNPFATSYWHB-UHFFFAOYSA-N 0.000 claims description 3
- 239000012615 aggregate Substances 0.000 claims description 3
- 239000010881 fly ash Substances 0.000 claims description 3
- 239000010440 gypsum Substances 0.000 claims description 3
- 229910052602 gypsum Inorganic materials 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 2
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- 239000010459 dolomite Substances 0.000 claims description 2
- 229910000514 dolomite Inorganic materials 0.000 claims description 2
- 239000010433 feldspar Substances 0.000 claims description 2
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004579 marble Substances 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000748 compression moulding Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 6
- 229910001570 bauxite Inorganic materials 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000007885 magnetic separation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000011074 autoclave method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/004—Preparation in the form of granules, pieces or other shaped products
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
-
- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/142—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/04—Clay; Kaolin
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
- C04B33/1322—Red mud
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/16—Lean materials, e.g. grog, quartz
-
- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- 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
- C22B7/007—Wet processes by acid leaching
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
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Abstract
Hair brushThe invention discloses a full-scale integral utilization method for recycling iron, sodium and tailings step by step from Bayer process red mud, which is characterized in that the red mud raw material is levigated and added with sulfuric acid for acid leaching to dissolve Fe and Na; adding excessive ammonia water into the leachate to obtain Fe (OH)3Solid, p-Fe (OH)3Calcining the solid to obtain Fe2O3Producing a product; separation of Fe (OH) from the solid3Adding NaOH into the solid solution to carry out chemical reaction, and carrying out evaporative crystallization on the residual solution after the chemical reaction to obtain sodium salt Na2SO4(ii) a And carrying out filter pressing on the leaching tailings, adding auxiliary materials into a filter cake, and carrying out wet grinding, uniform mixing, compression molding and sintering to obtain the building ceramic products with different purposes. The method not only recovers iron and sodium resources in the red mud, but also utilizes the leaching tailings by 100 percent, realizes simple full-scale integral utilization and treatment process of the red mud, has the characteristics of low cost and environmental protection, and can be popularized and applied in industrial production.
Description
Technical Field
The invention belongs to the field of red mud recycling technology, and particularly relates to a Bayer process red mud comprehensive utilization method, which is particularly suitable for Al2O3+SiO2+TiO248.0-68.0% of + CaO + MgO, Fe2O325.0-42.0% of Na2The total resource utilization of the Bayer process red mud with the O content of 4.0-10.0% and the other component content of 1.0-5.0%.
Background
The red mud is a large amount of industrial waste residue generated after bauxite is leached out of Al in the bauxite by a high-concentration NaOH solution. The specific process comprises the following steps: al in bauxite under the experimental conditions of high temperature and high pressure2O3Will react with NaOH solution to generate sodium aluminate. With formation of sodium aluminate, other constituents of bauxite, e.g. SiO2、Fe2O3、TiO2Oxides and the like do not react with bases. Separating the solid which is insoluble in NaOH solution and still exists in solid form to obtain the red mud. In the process of solid-liquid separation, a part of NaOH solution is still separated with the solid matter, therefore, the finally obtained waste is usually a slurry-like fluid, and because the Fe content is slightly excessive2O3These wastes usually appear dark red or brick red, so they are called red mud.
The red mud is industrial solid waste with low comprehensive utilization rate, the resource attribute of the red mud is widely concerned, but the recycling of the red mud is always a difficult problem and a technical difficulty in the alumina industry. Reported in the literature, 1 ton of Al per produced2O3In this case, about 1.5 to 2.0 tons of red mud must be produced. China, as the first major alumina producing country in the world, discharges nearly hundred million tons of red mud every year, and the accumulated stockpiled red mud exceeds 13 million tons. Fe in red mud2O3The content of the sodium-containing compound is generally high, and further, the sodium-containing compound contains 4 to 10 percent of Na2And O. The large amount of stockpiling of the red mud not only occupies a large amount of land and causes serious pollution to the environment, but also causes serious waste of bauxite resources with larger gaps in the market; in addition, most of the existing aluminum factories at home and abroad adopt conveying yards, damming wet-process stockpiling or dry-process stockpiling for the treatment of the red mud, and alkali-containing waste liquid in the red mud can pollute the ground surface and underground water sources, thereby seriously damaging the ecological natural environment. In conclusion, Fe in red mud is fully and reasonably recovered2O3And Na2O, and the tailings are utilized to prepare the building material, thereby effectively realizing the graded full-scale utilization of the red mud, reducing and harmlessly treating the red mud,Resource utilization, and has obvious and profound environmental, social and economic significance.
Currently, many studies are made on recovery of iron resources from red mud. The system of the 'research progress on extraction and recycling of iron in red mud' published in 2018, 9 th paragraph summarizes the research progress of the methods and process routes for extracting and recycling iron in red mud at home and abroad, and proposes to generalize the method for extracting and recycling iron from red mud into a direct physical separation method, a reduction-magnetic separation method and a wet extraction method. But the grade of the iron ore concentrate obtained by adopting a direct physical separation method is less than 50 percent, and the recovery rate is less than 55.0 percent; the reduction-magnetic separation method has high energy consumption, high production cost and serious environmental pollution, and a certain amount of additives including magnesium salt, calcium salt, sodium salt and double salt are also needed in the reduction roasting process, so the reduction-magnetic separation method is difficult to popularize and apply in actual production; although the energy consumption for extracting iron by wet separation is lower than that of a reduction-magnetic separation method, the dissolution time of iron in acid is long, the leaching rate is low, and the subsequent separation and purification operation with AL and Ti is also needed; the most important problem is that the integral comprehensive utilization of the red mud is not realized and new solid waste is generated.
In order to solve the problems, a great deal of research and exploration is carried out on the treatment and application of the red mud for a long time at home and abroad. The sodium removal of the red mud is easy to realize, but Fe in the red mud2O3There is currently no suitable method for recovery. The main methods at the present stage include an acid method and an alkali method: the acid-soluble method has high yield of alumina and low energy consumption, but has no proper idea for the treatment of ions in subsequent solution and the treatment of tailings, which also results in that the method is not applied to mature industrialization; the alkaline method mainly comprises a sodium carbonate decomposition method, a hydrothermal reaction method, an autoclave reaction method and the like, the recovery rate of alumina in the sodium carbonate decomposition method is low, the concentration of alumina in a solution obtained by the hydrothermal method is low and is difficult to match with a Bayer process main body dissolution process, and a part of sodium in the alumina can be recovered by the autoclave method, but the temperature of the alumina generally reaches over 260-280 ℃, and high-temperature and high-pressure operation usually causes high production energy consumption and has large requirements on equipment, so that the requirement on equipment is limited to a certain extentThe application of the method.
Therefore, in view of the above-mentioned current situation, it is necessary to further search for research and treatment of red mud, and a new method capable of treating and utilizing red mud on a large scale is proposed.
Disclosure of Invention
The invention aims to solve the problems of low comprehensive utilization rate, high cost, easy secondary pollution to the environment and the like of the existing red mud utilization technology, and provides a method for recycling iron and sodium resources comprehensively, simple in treatment process, low in cost and environment-friendly in a gradient manner, and recycling iron and sodium resources and tailings in the red mud in a full-scale manner.
In order to realize the purpose, the invention provides a full-quantitative integral utilization method for recycling iron, sodium and tailings from Bayer process red mud step by step, which is used for Al2O3+SiO2+TiO248.0-68.0% of + CaO + MgO, Fe2O325.0-42.0% of Na2The full-quantitative resource utilization of the Bayer process red mud with the O content of 4.0-10.0% and the other component content of 1.0-5.0% specifically adopts the following process and steps:
1) raw material treatment
The red mud raw material is crushed or ball-milled into fine red mud material with the granularity of-0.074 mu m and the mass percentage content of 60-95%. Generally, the mass percentage content of the fine red mud material with the granularity controlled at-0.074 mu m is preferably 75-90%, so that the requirement of the red mud treatment process can be met, and the energy consumption of ore grinding is saved. .
2) Acid leaching
And (3) dissolving Fe and Na in the fine red mud under the conditions that the liquid-solid ratio is 20-60 mL/g and the mass concentration of sulfuric acid is 10-40%, controlling the leaching time to be 30-120 min and the leaching temperature to be 25-90 ℃, and performing solid-liquid separation to obtain a leaching solution and leaching tailings. The principle of optimizing and selecting the process parameters of liquid-solid ratio, sulfuric acid mass concentration, leaching time and leaching temperature in the step is to comprehensively consider the leaching rate of Fe, the leaching rate of Na, the system processing capacity and the production cost, generally, the liquid-solid ratio is 40-60 mL/g, the sulfuric acid mass concentration is 25-40%, and the leaching rate of Fe is more than or equal to 85.0% and the leaching rate of Na is more than or equal to 80.0% by comprehensively regulating and controlling the liquid-solid ratio, the sulfuric acid mass concentration, the leaching time and the leaching temperature.
3) Recovery of iron-iron resource from ammonia water
In the solution after the steps, Fe is Fe3+Exist in the form of (1). At this time, excessive ammonia water is added to the leachate obtained in the step 2) to react, and flocculent precipitate Fe (OH) is generated in the solution3(ii) a For the flocculent precipitate Fe (OH)3The solution of (2) is subjected to solid-liquid separation to obtain Fe (OH)3Solid, p-Fe (OH)3Calcining the solid to obtain Fe2O3And (5) producing the product.
4) Sodium resource recovery
The ammonia water is used as a precipitator, and Fe (OH) is separated out in the step 3) through solid-liquid separation3The solid solution contains more NH4 +、Na+And SO4 2-Adding NaOH to carry out chemical reaction, and returning ammonia gas generated by the chemical reaction to the step 3) to carry out ammonia water iron precipitation; evaporating and crystallizing the residual solution after the chemical reaction to obtain the sodium salt Na2SO4。
5) Full-scale utilization of leaching tailings
Filter-pressing the leaching tailings obtained in the step 2), adding auxiliary materials, namely a silicon-rich aluminum raw material, a calcium-rich magnesium raw material and quartz into a filter cake, testing the water content and designing the addition ratios of different auxiliary materials, and controlling the mass percentage content of each component of the mixture according to the phase composition and the components in the ceramic raw material, namely: 50-85% of leaching tailings, 0-10% of quartz, 5-35% of silicon-aluminum-rich raw material and 0-20% of calcium-magnesium-rich raw material; the silicon-rich aluminum raw material comprises one or a mixture of two or more of clay, gangue, shale or feldspar; the calcium-rich magnesium raw material is one or a mixture of two or more of dolomite, stone processing leftover materials, marble and nickel-iron slag; and then, building ceramic products with different purposes can be obtained by wet grinding, uniform mixing, press forming and sintering, so that the step full-scale utilization of iron and sodium resources in the red mud and the leached tailings is realized.
Naturally, according to market demands, the leaching tailings obtained in the step 2) are subjected to filter pressing, auxiliary materials, namely fly ash, aggregate and industrial waste gypsum, are added into a filter cake, the phase composition and components are controlled according to the requirements of the raw materials of the autoclaved brick, and the solid or hollow autoclaved brick is finally prepared through wet grinding, uniform mixing, semi-dry press forming and autoclaved curing, so that the iron and sodium resources in the red mud and the leaching tailings are utilized in a gradient full-scale manner.
Through experimental research, in the treated Bayer process red mud component, (Al)2O3+SiO2) 35.0 to 50.0%, 15.0 to 22.0% of (CaO + MgO), and Fe2O325.0-42.0% of TiO23.5-7.0% of Na2The O content is preferably 4.0 to 10.0%.
Compared with the prior art, the full-quantitative integral utilization method for recycling iron, sodium and tailings from Bayer process red mud step by step has the following beneficial effects:
(1) the method utilizes CaO and SiO in dilute acid solution2And Al2O3Is low, mainly because the several components are mostly present as mineral phases. And Fe2O3And Na2The O can be better dissolved in the acid liquor because the iron component mainly exists as hematite which is easy to dissolve in the acid liquor, and the sodium component is derived from the added salt, so the method can realize the separation of Fe and Na resources from other oxides, and has higher separation efficiency.
(2) Compared with the large-scale application methods reported at home and abroad, such as calcium oxide sintering method, hydrothermal method and high-temperature high-pressure water chemical method, the scheme provided by the method is carried out under mild conditions of low temperature and low pressure, and Fe is realized2O3With Na2High recovery rate of O, and Fe in red mud2O3With Na2The final recovery rates of O reach more than 85.0 percent and 80.0 percent respectively.
(3) The method provided by the invention realizes energy conservation and consumption reduction in the red mud recycling process, realizes the step recycling of various resources in the red mud, and improves the resource utilization rate. In addition, the method also eliminates the pollution of alkali carried by the red mud to the environment, and is a red mud treatment process with large-scale application prospect.
(4) In addition, the liquid used in the method is basically in closed-loop circulation, and has low pollution and no tail gas.
(5) The method not only recovers iron and sodium resources in the red mud, but also utilizes the leached tailings by 100 percent, thereby realizing the full-scale integral utilization of the red mud.
Drawings
FIG. 1 is a technical scheme of a full-scale integral utilization method for recycling iron, sodium and tailings from Bayer process red mud by steps.
Detailed Description
The method is characterized in that Bayer process red mud is used as a raw material, and a low-temperature low-pressure hydrochemical method is adopted to recover Fe in the red mud2O3With Na2And O, realizing the step recycling of different resources in the red mud component. In order to describe the present invention, the following will explain the whole utilization method of the bayer process red mud for fractional recovery of iron, sodium and tailings in detail with reference to the examples. The present invention is not limited to the embodiments, and simple modifications made according to the essence of the present invention should be covered within the scope of the present invention.
The bayer process red mud used in the examples of the present invention has the following main component composition (wt.%) in table 1 below:
TABLE 1 Bayer Process Red mud Main chemical composition (wt.%)
| Composition (I) | Al2O3 | SiO2 | Fe2O3 | CaO | TiO2 | Na2O | MgO |
| Content (%) | 23.38 | 17.55 | 27.72 | 16.65 | 4.21 | 4.69 | 2.62 |
As can be seen from the technical route chart of the full-quantitative integral utilization method for recycling iron, sodium and tailings from Bayer process red mud step by step shown in FIG. 1, the technical route of the method of the invention is as follows: raw material treatment (fine grinding), acid leaching, iron precipitation by ammonia water, iron resource recovery, sodium resource recovery (evaporative crystallization), and full-scale utilization of leaching tailings (ceramsite, sintered brick and ceramic tile).
The specific treatment process comprises the following steps:
1) adding a certain amount of red mud into 30-40 wt% sulfuric acid solution, and adding H2SO4The liquid-solid ratio of the red mud and the red mud are respectively 50mL/g and 60mL/g, the mixture is transferred into a three-neck flask after being uniformly mixed, the stirring speed is regulated, the temperature control program is set, the water bath kettle is heated to 90 ℃ and reacts for 120min, and thenThen the circulating water in the condensing pipe is opened. In addition, in order to verify the influence of the leaching temperature on the leaching behavior of Fe and Na, the leaching behavior of Fe and Na in red mud was studied under experimental conditions of room temperature (25 ℃), a sulfuric acid concentration of 25%, a liquid-solid ratio of 50mL/g, and a leaching time of 1 hour. After the reaction is finished, slurry is filtered while hot, liquid and solid are separated, and the red mud filter cake is reserved. Then, a proper amount of the red mud filter cake is weighed for standby.
2) In the reaction step 1), the leachate obtained under different leaching conditions is subjected to ICP-MS analysis, so that the method can be known as follows: when the concentration of sulfuric acid is 30 percent, H2SO4The liquid-solid ratio of the Fe-Na-containing red mud to the red mud is 50mL/g, the leaching time is 0.5min, and the concentration of the Fe and the Na can reach 72.5mg/L and 45.7mg/L when the leaching temperature is 25 ℃; when the concentration of sulfuric acid is 30 percent, H2SO4When the liquid-solid ratio of the Fe-Na mixed solution to the red mud is 50mL/g, the leaching time is 120min and the leaching temperature is 90 ℃, the volume is determined to be 250mL of solution, and the concentrations of Fe and Na can reach 341mg/L and 54.2 mg/L; when the concentration of sulfuric acid is 30 percent, H2SO4The liquid-solid ratio of the Fe-Na mixed solution to the red mud is 60mL/g, the leaching time is 120min, and the leaching temperature is 90 ℃, the volume is determined to be 250mL of solution, and the concentrations of Fe and Na can reach 567mg/L and 83.4 mg/L; when the concentration of sulfuric acid is 40 percent, H2SO4The liquid-solid ratio of the Fe-Na mixed solution to the red mud is 60mL/g, the leaching time is 120min, and the leaching temperature is 90 ℃, the volume is determined to be 250mL of solution, and the concentrations of Fe and Na can reach 641mg/L and 104 mg/L. The experimental data show that the leaching rate of Fe and Na in the raw ore can be increased by increasing the liquid-solid ratio in the system and obviously increasing the solubility of Fe and Na in the leaching solution. At the moment, the leaching rate of Fe and Na can reach 85.47 percent and 80.14 percent;
3) transferring the filtrate obtained in step 2) to an erlenmeyer flask, wherein the solution contains a large amount of Fe3+. To be able to remove Fe in solution3+Converting into precipitate and recovering, wherein OH in the solution is adjusted-The solubility of the ions. The probe of the pH meter was added to the solution and the aqueous ammonia solution was added continuously to the flask. Filtering the solution until the content of floc in the conical flask is no longer changed to obtain Fe (OH)3Further realizing Fe in the red mudAnd (4) recovering.
4) Adding NaOH into the filtrate obtained by separating the slurry obtained in the step 3), recovering ammonia gas, and heating, evaporating and crystallizing on an electric heating plate after no gas overflows, so as to obtain Na salt, thereby realizing the recovery of Na resources in the red mud.
5) Testing the water content of the red mud filter cake obtained in the step 1), designing different addition ratios of silicon-rich aluminum raw materials and calcium-rich magnesium raw materials as auxiliary materials, grinding, uniformly mixing, preparing and sintering by a wet method, obtaining different types of ceramic products, such as building ceramic products like ceramic granules, ceramic tiles, sintered bricks and the like, and realizing the step full-scale utilization of the red mud resource. Or adding auxiliary materials, namely fly ash, aggregate and industrial waste gypsum, into the filter cake according to market demands, controlling phase composition and components according to the requirements of the raw materials of the autoclaved brick, grinding and uniformly mixing by a wet method, press-forming by a semi-dry method, and carrying out autoclaved curing to finally prepare the solid or hollow autoclaved brick
The method for recycling Fe and Na resources from red mud step by step and utilizing the leaching tailings thereof for large-scale high-value utilization has the advantages of simple treatment process, low cost, no introduction of other secondary pollution, avoidance of an atmosphere control process and generation of a large amount of polluting gases in the conventional iron recycling process, good application prospect in the field of comprehensive utilization of red mud, and suitability for industrial popularization.
Claims (6)
1. Full-quantitative integral utilization method for recycling iron, sodium and tailings from Bayer process red mud step by step, and application of full-quantitative integral utilization method to Al2O3+SiO2+TiO248.0-68.0% of + CaO + MgO, Fe2O325.0-42.0% of Na2The full-quantitative resource utilization of the Bayer process red mud with the O content of 4.0-10.0% and the other component content of 1.0-5.0% is characterized by comprising the following steps:
1) raw material treatment
Crushing or ball-milling the red mud raw material into fine red mud material with the granularity of-0.074 mu m and the mass percentage content of 60-95%;
2) acid leaching
Dissolving Fe and Na in the fine red mud under the conditions that the liquid-solid ratio is 20-60 mL/g and the mass concentration of sulfuric acid is 10-40%, controlling the leaching time to be 30-120 min and the leaching temperature to be 25-90 ℃, and performing solid-liquid separation to obtain a leaching solution and leaching tailings;
3) recovery of iron-iron resource from ammonia water
Adding excessive ammonia water into the leachate obtained in the step 2) for reaction to generate flocculent precipitate Fe (OH)3(ii) a For the flocculent precipitate Fe (OH)3The solution of (2) is subjected to solid-liquid separation to obtain Fe (OH)3Solid, p-Fe (OH)3Calcining the solid to obtain Fe2O3Producing a product;
4) sodium resource recovery
Step 3) solid-liquid separation of Fe (OH)3The solid solution contains more NH4 +、Na+And SO4 2-Adding NaOH to carry out chemical reaction, and returning ammonia gas generated by the chemical reaction to the step 3) to carry out ammonia water iron precipitation; evaporating and crystallizing the residual solution after the chemical reaction to obtain the sodium salt Na2SO4；
5) Full-scale utilization of leaching tailings
Filter-pressing the leaching tailings obtained in the step 2), adding auxiliary materials, namely a silicon-rich aluminum raw material, a calcium-rich magnesium raw material and quartz into a filter cake, testing the water content and designing the addition ratios of different auxiliary materials, and controlling the mass percentage content of each component of the mixture according to the phase composition and the components in the ceramic raw material, namely: 50-85% of leaching tailings, 0-10% of quartz, 5-35% of silicon-aluminum-rich raw material and 0-20% of calcium-magnesium-rich raw material; the silicon-rich aluminum raw material comprises one or a mixture of two or more of clay, gangue, shale or feldspar; the calcium-rich magnesium raw material is one or a mixture of two or more of dolomite, stone processing leftover materials, marble and nickel-iron slag; and then, building ceramic products with different purposes can be obtained by wet grinding, uniform mixing, press forming and sintering, so that the step full-scale utilization of iron and sodium resources in the red mud and the leached tailings is realized.
2. Full-quantitative integral utilization method for recycling iron, sodium and tailings from Bayer process red mud step by step, and application of full-quantitative integral utilization method to Al2O3+SiO2+TiO248.0-68.0% of + CaO + MgO, Fe2O325.0-42.0% of Na2The full-quantitative resource utilization of the Bayer process red mud with the O content of 4.0-10.0% and the other component content of 1.0-5.0% is characterized by comprising the following steps:
1) raw material treatment
Crushing or ball-milling the red mud raw material into fine red mud material with the granularity of-0.074 mu m and the mass percentage content of 60-95%;
2) acid leaching
Dissolving Fe and Na in the fine red mud under the conditions that the liquid-solid ratio is 20-60 mL/g and the mass concentration of sulfuric acid is 10-40%, controlling the leaching time to be 30-120 min and the leaching temperature to be 25-90 ℃, and performing solid-liquid separation to obtain a leaching solution and leaching tailings;
3) recovery of iron-iron resource from ammonia water
Adding excessive ammonia water into the leachate obtained in the step 2) for reaction to generate flocculent precipitate Fe (OH)3(ii) a For the flocculent precipitate Fe (OH)3The solution of (2) is subjected to solid-liquid separation to obtain Fe (OH)3Solid, p-Fe (OH)3Calcining the solid to obtain Fe2O3Producing a product;
4) sodium resource recovery
Step 3) solid-liquid separation of Fe (OH)3The solid solution contains more NH4 +、Na+And SO4 2-Adding NaOH to carry out chemical reaction, and returning ammonia gas generated by the chemical reaction to the step 3) to carry out ammonia water iron precipitation; evaporating and crystallizing the residual solution after the chemical reaction to obtain the sodium salt Na2SO4；
5) Full-scale utilization of leaching tailings
Carrying out filter pressing on the leaching tailings obtained in the step 2), adding auxiliary materials, namely fly ash, aggregate and industrial waste gypsum, into a filter cake, controlling phase composition and components according to the requirements of the raw materials of the autoclaved brick, and finally preparing the solid or hollow autoclaved brick through wet-method grinding and uniform mixing, semi-dry-method press forming and autoclaved curing, thereby realizing the step full-scale utilization of iron and sodium resources in the red mud and the leaching tailings.
3. The full-quantitative and integral utilization method for recycling iron, sodium and tailings from Bayer process red mud in steps according to claim 1, which is characterized in that the red mud comprises the following components in percentage by mass: (Al)2O3+SiO2)35.0～50.0％、(CaO+MgO)15.0～22.0％、Fe2O325.0～42.0％、TiO23.5～7.0％、Na2O4.0-10.0%, and the balance of other components.
4. The full-quantitative and integral utilization method for recycling iron, sodium and tailings from Bayer process red mud in a stepwise manner as claimed in claim 1, 2 or 3, which is characterized in that: the granularity of discharged materials in the grinding procedure in the step 5) is more than 95 percent of minus 0.178 mm.
5. The full-quantitative and integral utilization method for recycling iron, sodium and tailings from Bayer process red mud in a stepwise manner, according to claim 4, is characterized in that: the mass percentage of the granularity of the fine red mud material in the step 1) is controlled to be-0.074 mu m, and the content is 75-90%.
6. The full-quantitative and integral utilization method for recycling iron, sodium and tailings from Bayer process red mud in a stepwise manner, according to claim 5, is characterized in that: in the step 2), the liquid-solid ratio is 40-60 mL/g, and the mass concentration of sulfuric acid is 25-40%; the liquid-solid ratio, the mass concentration of sulfuric acid, the leaching time and the leaching temperature are comprehensively regulated and controlled, so that the leaching rate of Fe is more than or equal to 85.0 percent, and the leaching rate of Na is more than or equal to 80.0 percent.
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| PCT/CN2021/116009 WO2023004927A1 (en) | 2021-07-26 | 2021-09-01 | Full-quantitative overall utilization method for step-by-step recovery of iron, sodium and tailings from bayer red mud |
| ZA2022/04725A ZA202204725B (en) | 2021-07-26 | 2022-04-28 | Full-quantitative overall utilization method for stepwise recycling iron, sodium and tailings from bayer red mud |
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| CN102276219B (en) * | 2011-05-26 | 2013-12-11 | 四川方大新型建材科技开发有限责任公司 | Autoclaved red mud brick and preparation method thereof |
| CN102757078B (en) * | 2012-07-18 | 2014-03-05 | 潘爱芳 | Method for separating useful components from bayer process red mud |
| CN102826560A (en) * | 2012-08-29 | 2012-12-19 | 潘国雄 | Red mud resource utilization method |
| CN104340995B (en) * | 2013-07-24 | 2016-05-11 | 沈阳铝镁设计研究院有限公司 | A kind of method of red mud comprehensive utilization |
| CN105693210A (en) * | 2016-01-28 | 2016-06-22 | 北京科技大学 | Ceramic material prepared from red mud, and preparation method of ceramic material |
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| 中国冶金百科全书总编辑委员会《有色金属冶金》卷编辑委员会等: "《中国冶金百科全书 有色金属冶金》", 31 January 1999, 冶金工业出版社 * |
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