CN112299721A - Method for preparing alumina and co-producing microcrystalline glass based on pulverized coal furnace fly ash and product - Google Patents
Method for preparing alumina and co-producing microcrystalline glass based on pulverized coal furnace fly ash and product Download PDFInfo
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- CN112299721A CN112299721A CN202011193034.9A CN202011193034A CN112299721A CN 112299721 A CN112299721 A CN 112299721A CN 202011193034 A CN202011193034 A CN 202011193034A CN 112299721 A CN112299721 A CN 112299721A
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- hydrochloric acid
- fly ash
- alumina
- aluminum chloride
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000010881 fly ash Substances 0.000 title claims abstract description 38
- 239000011521 glass Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000003245 coal Substances 0.000 title claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 66
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 29
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000004090 dissolution Methods 0.000 claims abstract description 18
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000012045 crude solution Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000395 magnesium oxide Substances 0.000 claims description 20
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 20
- 238000002425 crystallisation Methods 0.000 claims description 17
- 230000008025 crystallization Effects 0.000 claims description 17
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 9
- 238000001953 recrystallisation Methods 0.000 claims description 9
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910001424 calcium ion Inorganic materials 0.000 claims description 8
- 239000000292 calcium oxide Substances 0.000 claims description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 230000000536 complexating effect Effects 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 238000010128 melt processing Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000243 solution Substances 0.000 abstract description 8
- 238000005266 casting Methods 0.000 abstract description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011575 calcium Substances 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 abstract 2
- 238000002386 leaching Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 18
- 235000012245 magnesium oxide Nutrition 0.000 description 13
- 230000035484 reaction time Effects 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 235000012255 calcium oxide Nutrition 0.000 description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 4
- 235000011941 Tilia x europaea Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012527 feed solution Substances 0.000 description 4
- 239000004571 lime Substances 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 3
- 239000010883 coal ash Substances 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002956 ash Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- WVMPCBWWBLZKPD-UHFFFAOYSA-N dilithium oxido-[oxido(oxo)silyl]oxy-oxosilane Chemical compound [Li+].[Li+].[O-][Si](=O)O[Si]([O-])=O WVMPCBWWBLZKPD-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 2
- 229910052912 lithium silicate Inorganic materials 0.000 description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 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
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000006017 silicate glass-ceramic Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0063—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing waste materials, e.g. slags
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/22—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with halides or halogen acids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/302—Hydrolysis or oxidation of gaseous aluminium compounds in the gaseous phase
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
- C01F7/62—Purification
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Geology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a method for preparing alumina and coproducing microcrystalline glass based on pulverized coal of a pulverized coal furnace and a product, wherein the method comprises the following steps: pulverizing pulverized coal furnace fly ash and pretreating with dilute acid; mixing the pretreated material with hydrochloric acid for acid dissolution to obtain dissolved slurry; solid-liquid separation is carried out on the dissolved slurry to obtain white mud and crude liquid; adding concentrated sulfuric acid and potassium permanganate into the crude solution to remove impurities such as calcium, iron and the like, and filtering after the reaction is finished to obtain refined solution; evaporating and crystallizing the refined solution, and filtering to obtain crystalline aluminum chloride; roasting the crystallized aluminum chloride in a steam environment to obtain aluminum oxide, and then washing and drying to obtain an aluminum oxide product; drying the white mud, and mixing with added oxides such as LiBr; melting the ingredients, casting to obtain a glass body, and cooling to room temperature; and then putting the glass into a muffle furnace for primary and secondary heat treatment to obtain the microcrystalline glass. The alumina leaching rate of the invention is high, the performance of the prepared glass ceramics is excellent, the high-efficiency utilization of the coal powder furnace fly ash can be realized, and the economic benefit is good.
Description
Technical Field
The invention relates to a novel method for preparing alumina and coproducing microcrystalline glass based on high-temperature dissolution of pulverized fuel ash in a pulverized fuel furnace and a prepared product, and belongs to the field of pulverized fuel ash recycling.
Background
The coal powder furnace coal ash and slag have special mineral phase structures which are mainly characterized by mullite, corundum and glass phase, the activity of alumina is extremely poor, the direct dissolution by acid, alkali and the like is difficult, and most processes need to pretreat the coal ash during the extraction of the alumina. Such as: the technological processes of lime and soda lime sintering, calcium chloride and villiaumite fluxing, ammonium salt activating, acid-alkali combining, salt melting and the like all need to pretreat the coal powder furnace fly ash to improve the dissolution rate of alumina. The process has the advantages of large slag yield (5 tons of slag are produced by processing one ton of fly ash), unqualified environmental protection, high cost, equipment limitation, poor safety and the like, and has great significance in finding an economic and feasible industrialized technical route for extracting the alumina from the fly ash of the pulverized coal furnace.
CN102145905B discloses a method for preparing metallurgical alumina by using fluidized bed fly ash as a raw material, which comprises the steps of reacting fly ash subjected to magnetic separation and iron removal with hydrochloric acid to prepare an aluminum chloride solution, then carrying out deep purification by macroporous cation resin to obtain a refined aluminum chloride solution, and then carrying out concentration crystallization and roasting to finally prepare the metallurgical alumina. CN103889391A discloses a lithium silicate glass ceramic containing Li in an amount of 12.1-20.0 wt%2O, 55.0-85.0 wt% SiO2The main synthesis method comprises the following steps: (1) heat-treating at 470 ℃ -560 ℃ for a time of 10-120 minutes to obtain a nucleated glass suitable for forming lithium disilicate crystals; (2) the nucleated glass is heat treated at a temperature of 600-750 ℃ for 10 minutes to 120 minutes to form a glass-ceramic having lithium disilicate as a main crystal phase. Similar patents for preparing the glass by extracting the alumina and the lithium silicate from the fly ash are more, but most of the patents have the problems of high cost, complex process flow and difficult industrialization. .
Disclosure of Invention
The invention aims to provide a method for preparing alumina and coproducing microcrystalline glass based on pulverized coal furnace fly ash, which realizes extraction of alumina from pulverized coal furnace fly ash and comprehensive utilization of white mud, has high alumina yield, excellent microcrystalline glass performance and simple process and can be used for industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing alumina and coproducing microcrystalline glass based on pulverized coal furnace fly ash comprises the following steps:
(1) crushing pulverized coal furnace fly ash, and then adding dilute hydrochloric acid into the crushed material to perform acid dissolution pretreatment; wherein, the pulverized coal furnace fly ash is crushed to be below 100 meshes in the step (1); the concentration of the dilute hydrochloric acid is 0.2% -5.0%, wherein the molar ratio of HCl to the sum of the mass of calcium oxide and magnesium oxide in the crushed material is 0.7: 1-2: 1;
(2) placing the pretreated material and hydrochloric acid into a reaction kettle for acid dissolution reaction, wherein the concentration of the hydrochloric acid is 16% -36.4%, and the molar ratio of HCl to alumina in the crushed material is 3: 1-5: 1; reaction temperature: 190 ℃ to 220 ℃;
(3) carrying out solid-liquid separation on the acid-soluble reaction product to obtain crude liquid and white mud;
(4) adding concentrated sulfuric acid and potassium permanganate into the obtained crude liquid for complexing impurity removal, wherein the amount of sulfuric acid in the concentrated sulfuric acid is 0.7-1.5 times of the molar amount of calcium ions in the crude liquid; the adding amount of the potassium permanganate is 0.07-0.28 percent of the mass content of the potassium permanganate in the crude liquid; reaction temperature: 60-100 ℃; then filtering and removing impurities to obtain refined liquid;
(5) heating and evaporating the obtained refined liquid, crystallizing, then carrying out solid-liquid separation and washing to obtain crystalline aluminum chloride; optionally, further carrying out recrystallization treatment on the obtained crystalline aluminum chloride;
(6) introducing steam at the temperature of 700-;
(7) drying the obtained white mud, and then adding LiBr and Al into the white mud2O3、TiO2MgO and CeO2Mixing to obtain a mixture, wherein the white mud and the added LiBr and Al are calculated on a dry basis in the mixture2O3、TiO2MgO and CeO2The mass contents are respectively 60-70%, 10-20%, 5-12%, 2-8%, 1-7% and 2-5%;
(8) melting the obtained mixture at 1350-;
(9) and putting the obtained glass body into a muffle furnace for primary heat treatment at 500-650 ℃ for 0.5-2.0 h, then performing secondary heat treatment at 750-880 ℃ for 0.5-3.0 h, taking out and cooling to obtain the glass ceramics.
In the step (1) of the invention, pulverized coal furnace fly ash is pulverized to be less than 100 meshes (namely, the pulverized coal furnace fly ash can pass through a standard sieve of 100 meshes), and then diluted hydrochloric acid pretreatment is carried out on the pulverized coal ash, so that calcium and magnesium oxides are initially reacted and consumed, the subsequent dissolution treatment of alumina in the fly ash is facilitated, and the consumption of hydrochloric acid is low. Preferably, the molar ratio of HCl in the dilute hydrochloric acid to the sum of the masses of calcium oxide and magnesium oxide in the crushed material in the step (1) is 0.85: 1-1: 1, such as 0.9: 1; the dilute hydrochloric acid has a concentration of 0.5-2%, such as 0.8%, 1.0% or 1.5%. The fly ash is well known in the art as a raw material for the present invention, and in one embodiment, the fly ash contains, in parts by weight, 40 to 46 parts (e.g., 42 or 44 parts) of silica, 44 to 50 parts (e.g., 44, 45 or 46 parts) of alumina, 1.5 to 2 parts (e.g., 1.8 parts) of titania, 1.5 to 3 parts (e.g., 2 or 2.5 parts) of calcium oxide, 0.1 to 0.4 parts (e.g., 0.2 or 0.3 part) of magnesium oxide, 2 to 4 parts (e.g., 2.5, 3 or 3.5 parts) of iron oxide, 0.2 to 0.6 parts (e.g., 0.3 or 0.5 part) of potassium oxide and sodium oxide, and the balance is substantially loss on ignition. In addition, it will be understood by those skilled in the art that the feedstock used may also include larger particle slag.
In step (2), performing an alumina dissolution reaction on the product pretreated in step (1) by using hydrochloric acid, preferably, the molar ratio of the hydrochloric acid to alumina in the crushed material in step (2) is 3.5: 1-5: 1, such as 4: 1; the hydrochloric acid concentration is 20% -31%, such as 25%; the reaction temperature is 200 ℃ to 220 ℃, such as 202 or 210 ℃. It is understood by those skilled in the art that the acid dissolution time also affects the dissolution effect of alumina or other oxides, and therefore the acid dissolution time is generally preferred to dissolve the target alumina as much as possible, for example, 3 to 10 hours, in consideration of time cost.
In step (3) of the present invention, the acid-soluble product is subjected to solid-liquid separation for subsequent separate recycling.
In the step (4) of the present invention, concentrated sulfuric acid and potassium permanganate are added to the crude solution to remove impurities, such as calcium and iron, in the crude solution, preferably, the molar ratio of sulfuric acid in the concentrated sulfuric acid in the step (4) to calcium ions in the feed solution is 0.8-1.2:1, such as 1: 1; the mass content of potassium permanganate in the crude solution is 0.1-0.18 percent, such as 0.12 or 0.15 percent; the reaction temperature is 70-90 deg.C, such as 80 deg.C. The impurity removal process is simple to operate and good in impurity removal effect.
In the step (5) of the present invention, the obtained purified liquid may be subjected to a heating evaporation and crystallization treatment, and a recrystallization treatment may be further performed to improve the purity. Preferably, the evaporation temperature in step (5): evaporating at 90-130 deg.C, such as 100 or 120 deg.C, until aluminum chloride is saturated; the crystallization temperature is 50-85 deg.C, such as 60 or 80 deg.C; the pressure in the above process can be controlled at 0.01-0.04MPa, such as 0.02 or 0.03 MPa; preferably, in the recrystallization, the crystalline aluminum chloride is dissolved in water, and the aluminum chloride dissolution temperature is controlled to be 100-: 100-: 20-60 ℃, preferably: 20-40 deg.C, such as 30 deg.C.
In the step (6) of the present invention, the calcination decomposition of crystalline aluminum chloride is promoted in the presence of water vapor to obtain alumina, and then further distilled water is added to remove impurities such as potassium, sodium and the like; preferably, the calcination temperature in step (6) is 900-980 ℃, the calcination time is 2-7 hours, preferably 3-4 hours, and the steam flow rate is 1.2-5m per kg of the crystalline aluminum chloride3H, preferably from 1.5 to 2.85m3H; distilled water washing temperature: 70-100 ℃, preferably: 80-90 ℃.
In the step (7) of the invention, the obtained white mud is dried, and the microcrystalline glass is prepared by material proportioning. Preferably, the white mud and the added LiBr and Al are calculated on a dry basis in the ingredients obtained in the step (7)2O3、TiO2MgO and CeO2The mass contents are respectively 60-70%, 10-15%, 5-10%, 3-7%, 2-5% and 3-5%.
In the step (8) of the present invention, the batch materials are melted to obtain the glass body, and preferably, the melting temperature in the step (8) is 1400 ℃ and 1530 ℃, and the treatment time is 3-4 hours.
In step (9) of the present invention, the obtained glass body is subjected to primary heat treatment and secondary heat treatment in a high-temperature furnace, respectively, to obtain a glass-ceramic. Preferably, the temperature of the primary heat treatment in the step (9) is 600-650 ℃; the crystallization time is 0.5-1.0 h; the secondary heat treatment temperature is 750-800 ℃; the crystallization time is 1.5-2.5 h.
The invention also provides the alumina and the glass ceramics prepared by the method.
Unless otherwise specified, the contents described herein are mass contents.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, dilute hydrochloric acid pretreatment is carried out on the materials before acid dissolution, so that the dissolution of alumina in the fly ash is promoted, and the dissolution efficiency is improved.
(2) According to the invention, concentrated sulfuric acid and potassium permanganate are added into the crude solution to remove impurities, wherein sulfuric acid not only reacts with calcium ions, but also can promote potassium permanganate to be used for complex impurity removal, so that two purposes are achieved, and the operation is simple and the impurity removal effect is good.
(3) The invention extracts the aluminum oxide product meeting the national first-grade product standard from the fly ash, simultaneously fully recycles the white mud, realizes the comprehensive utilization of the fly ash and has good industrialization prospect.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the examples.
The pulverized coal furnace fly ash used in the following examples is a byproduct generated by coal used in power plants, and the main components and contents thereof are shown in the following table 1:
TABLE 1 pulverized coal furnace fly ash ingredient table
| Composition (I) | SiO2 | Al2O3 | TiO2 | CaO | MgO | Fe2O3 | K2O | Na2O | P2O5 | LOI | Total of | Unit of |
| Content (wt.) | 42.58 | 45.92 | 1.77 | 2.31 | 0.24 | 2.60 | 0.39 | 0.09 | 0.00 | 4.05 | 99.95 | ％ |
Examples 1 to 5
(1) Weighing one kilogram of fly ash and grinding the fly ash to be below 100 meshes; the molar ratio of the hydrochloric acid to the calcium oxide and the magnesium oxide in the fly ash is as follows: 0.85: 1; hydrochloric acid concentration: 0.5 percent; reaction time: 50 min; stirring speed: 100 revolutions per minute.
(2) Reacting the pretreated material with hydrochloric acid in a high-temperature reaction kettle, wherein the molar ratio of the hydrochloric acid to alumina in the fly ash is as follows: 3.5: 1; hydrochloric acid concentration: 16.1% -36.4%; reaction time: 3.5-9.5 h; reaction temperature: 205 deg.C; stirring speed: 100 rpm.
(3) After the reaction is finished, carrying out solid-liquid separation and washing to obtain crude liquid and white mud.
(4) Adding concentrated sulfuric acid and potassium permanganate into the crude solution to remove impurities, wherein the molar ratio of concentrated sulfuric acid to calcium ion in the feed solution is 0.8: 1; the adding concentration of potassium permanganate is 0.12 percent; reaction time: 1 hour; reaction temperature: 90 ℃; then filtering to obtain refined liquid, wherein the removal rate of iron element is not less than 99.99%.
(5) Evaporation crystallization control temperature: 110 ℃; controlling the temperature of the crystallizer to be 65 ℃; and (3) pressure control: 0.01 Mpa; after the reaction is finished, carrying out solid-liquid separation and washing to obtain the crystalline aluminum chloride. Then heating again to dissolve in water, and cooling to recrystallize the aluminum chloride solution, wherein the recrystallization temperature is as follows: at 40 ℃.
(6) Calcination was carried out at 890 ℃ for 3 hours, with steam per kg of crystalline aluminum chloride: 2m3/h to obtain an alumina product. Adding the alumina product into distilled water, reacting for 1h at 90 ℃, and stirring: 100 rpm. Drying temperature: 105 ℃, time: and obtaining an alumina product meeting the first-grade standard after 2 hours.
(7) Dried white mud, LiBr and proper amount of Al2O3、TiO2、MgO、CeO2Mixing the materials according to a certain proportion. Wherein m (dry lime mud) and m (Al)2O3)、m(LiBr)、m(TiO2)、m(MgO)、m(CeO2) 60%, 15%, 10%, 7%, 3%, 5%, respectively.
(8) Putting the mixed materials into a platinum crucible, wherein the melting temperature is as follows: melting for 2h at 1500 ℃. Taking out the crucible after melting, casting to obtain a glass cylinder, and cooling for 1 h.
(9) Primary heat treatment temperature for heat-treating glass in a muffle furnace: 600 ℃, crystallization time: 1.0 h. Secondary heat treatment temperature: 780 ℃, crystallization time: and (5) h. And obtaining the microcrystalline glass product.
The relevant parameters are shown in table 2 below:
examples 6 to 10
(1) Weighing one kilogram of fly ash and grinding the fly ash to be below 100 meshes; the molar ratio of the hydrochloric acid to the calcium oxide and the magnesium oxide in the fly ash is as follows: 1: 1; hydrochloric acid concentration: 0.5 percent; reaction time: 50 min; stirring speed: 100 revolutions per minute.
(2) Reacting the pretreated material with hydrochloric acid in a high-temperature reaction kettle, wherein the molar ratio of the hydrochloric acid to alumina in the fly ash is as follows: 4: 1; hydrochloric acid concentration: 16.1% -36.4%; reaction time: 3.5-9.5 h; reaction temperature: 220 ℃; stirring speed: 100 rpm.
(3) After the reaction is finished, carrying out solid-liquid separation and washing to obtain crude liquid and white mud.
(4) Adding concentrated sulfuric acid and potassium permanganate into the crude solution to remove impurities, wherein the molar ratio of sulfuric acid in the concentrated sulfuric acid to calcium ion in the feed solution is 1: 1; the adding concentration of potassium permanganate is 0.15 percent; reaction time: 1 hour; reaction temperature: 90 ℃; then filtering to obtain refined liquid, wherein the removal rate of iron element is not less than 99.99%.
(5) Evaporation crystallization control temperature: 110 ℃; controlling the temperature of the crystallizer to be 65 ℃; and (3) pressure control: 0.01 Mpa; after the reaction is finished, carrying out solid-liquid separation and washing to obtain the crystalline aluminum chloride. Then heating again to dissolve in water, and cooling to recrystallize the aluminum chloride solution, wherein the recrystallization temperature is as follows: at 40 ℃.
(6) Calcination was carried out at 890 ℃ for 3 hours, with steam per kg of crystalline aluminum chloride: 2.5m3/h to obtain an alumina product. Adding the alumina product into distilled water, reacting for 1h at 90 ℃, and stirring: 100 rpm. Drying temperature: 105 ℃, time: and obtaining an alumina product meeting the first-grade standard after 2 hours.
(7) Dried white mud, LiBr and proper amount of Al2O3、TiO2、MgO、CeO2Mixing the materials according to a certain proportion. Wherein m (dry lime mud) and m (Al)2O3)、m(LiBr)、m(TiO2)、m(MgO)、m(CeO2) 70%, 10%, 4%, 2%, 4%, respectively.
(8) Putting the mixed materials into a platinum crucible, wherein the melting temperature is as follows: and melting at 1530 ℃ for 2 h. Taking out the crucible after melting, casting to obtain a glass cylinder, and cooling for 1 h.
(9) Primary heat treatment temperature for heat-treating glass in a muffle furnace: 650 ℃, crystallization time: 1.0 h. Secondary heat treatment temperature: 760 ℃, crystallization time: and 2 h. And obtaining the microcrystalline glass product.
The relevant parameters are shown in table 3 below:
comparative examples 1 to 5
(1) One kilogram of fly ash was weighed out and ground to below 100 mesh.
(2) Reacting the crushed material with hydrochloric acid in a high-temperature reaction kettle, wherein the molar ratio of the hydrochloric acid to alumina in the fly ash is as follows: 5: 1; hydrochloric acid concentration: 16.1% -36.4%; reaction time: 3.5-9.5 h; reaction temperature: 160 ℃; stirring speed: 100 rpm.
(3) After the reaction is finished, carrying out solid-liquid separation and washing to obtain crude liquid and white mud.
(4) Adding concentrated sulfuric acid and potassium permanganate into the crude solution to remove impurities, wherein the molar ratio of sulfuric acid in the concentrated sulfuric acid to calcium ion in the feed solution is as follows: 1: 1; the adding concentration of potassium permanganate is 0.15 percent; reaction time: 1 hour; reaction temperature: 90 ℃; then, the resulting mixture was filtered to obtain a purified solution.
(5) Evaporation crystallization control temperature: 110 ℃; controlling the temperature of the crystallizer to be 65 ℃; and (3) pressure control: 0.01 Mpa; after the reaction is finished, carrying out solid-liquid separation and washing to obtain the crystalline aluminum chloride. Then heating again to dissolve in water, and cooling to recrystallize the aluminum chloride solution, wherein the recrystallization temperature is as follows: at 40 ℃.
(6) Calcination was carried out at 890 ℃ for 3 hours, with steam per kg of crystalline aluminum chloride: 2.5m3/h to obtain an alumina product. Adding the alumina product into distilled water, reacting for 1h at 90 ℃, and stirring: 100 rpm. Drying temperature: 105 ℃, time: and obtaining an alumina product meeting the first-grade standard after 2 hours.
(7) Dried white mud, LiBr and proper amount of Al2O3、TiO2、MgO、CeO2Mixing the materials according to a certain proportion. Wherein m (dry lime mud) and m (Al)2O3)、m(LiBr)、m(TiO2)、m(MgO)、m(CeO2) 70%, 10%, 5%, 7%, 5%, 3%, respectively.
(8) Putting the mixed materials into a platinum crucible, wherein the melting temperature is as follows: melting for 2h at 1500 ℃. Taking out the crucible after melting, casting to obtain a glass cylinder, and cooling for 1 h.
(9) Primary heat treatment temperature for heat-treating glass in a muffle furnace: 550 ℃, crystallization time: 1.0 h. Secondary heat treatment temperature: 780 ℃, crystallization time: and (5) h. And obtaining the microcrystalline glass product.
The relevant parameters are shown in table 4 below:
Claims (10)
1. a method for preparing alumina and coproducing microcrystalline glass based on pulverized coal furnace fly ash comprises the following steps:
(1) crushing pulverized coal furnace fly ash, and then adding dilute hydrochloric acid into the crushed material to perform acid dissolution pretreatment; wherein, the pulverized coal furnace fly ash is crushed to be below 100 meshes in the step (1); the concentration of the dilute hydrochloric acid is 0.2% -5.0%, wherein the molar ratio of HCl to the sum of the mass of calcium oxide and magnesium oxide in the crushed material is 0.7: 1-2: 1;
(2) placing the pretreated material and hydrochloric acid into a reaction kettle for acid dissolution reaction, wherein the concentration of the hydrochloric acid is 16% -36.4%, and the molar ratio of HCl to alumina in the crushed material is 3: 1-5: 1; reaction temperature: 190 ℃ to 220 ℃;
(3) carrying out solid-liquid separation on the acid-soluble reaction product to obtain crude liquid and white mud;
(4) adding concentrated sulfuric acid and potassium permanganate into the obtained crude liquid for complexing impurity removal, wherein the amount of sulfuric acid in the concentrated sulfuric acid is 0.7-1.5 times of the molar amount of calcium ions in the crude liquid; the adding amount of the potassium permanganate is 0.07-0.28 percent of the mass content of the potassium permanganate in the crude liquid; reaction temperature: 60-100 ℃; then filtering and removing impurities to obtain refined liquid;
(5) heating and evaporating the obtained refined liquid, crystallizing, then carrying out solid-liquid separation and washing to obtain crystalline aluminum chloride; optionally, further carrying out recrystallization treatment on the obtained crystalline aluminum chloride;
(6) introducing steam at the temperature of 700-;
(7) drying the obtained white mud, and then adding LiBr and Al into the white mud2O3、TiO2MgO and CeO2Mixing to obtain a mixture, wherein the white mud and the added LiBr and Al are calculated on a dry basis in the mixture2O3、TiO2MgO and CeO2The mass contents are respectively 60-70%, 10-20%, 5-12%, 2-8%, 1-7% and 2-5%;
(8) melting the obtained mixture at 1350-;
(9) and putting the obtained glass body into a muffle furnace for primary heat treatment at 500-650 ℃ for 0.5-2.0 h, then performing secondary heat treatment at 750-880 ℃ for 0.5-3.0 h, taking out and cooling to obtain the glass ceramics.
2. The method according to claim 1, wherein the molar ratio of HCl in the dilute hydrochloric acid to the sum of the amounts of calcium oxide and magnesium oxide in the crushed material in step (1) is 0.85: 1-1: 1; the concentration of the dilute hydrochloric acid is 0.5-2%.
3. The method according to claim 1 or 2, wherein the molar ratio of the hydrochloric acid in the step (2) to the alumina in the crushed material is 3.5: 1-5: 1; the concentration of the hydrochloric acid is 20% -31%; the reaction temperature is 200-220 ℃.
4. The method according to any one of claims 1 to 3, wherein the molar ratio of sulfuric acid in the concentrated sulfuric acid to calcium ions in the feed liquid in step (4) is 0.8-1.2: 1; the mass of potassium permanganate in the crude solution is 0.1-0.18%; the reaction temperature is 70-90 ℃.
5. The method according to any one of claims 1 to 4, wherein the evaporation temperature in step (5): evaporating at 90-130 deg.C until aluminum chloride is saturated; the crystallization temperature is 50-85 ℃; controlling the pressure at 0.01-0.04 MPa;
during recrystallization, crystalline aluminum chloride is dissolved in water, the dissolution temperature of the aluminum chloride is controlled to be 100-130 ℃, and the following steps are preferred: 100 ℃ and 120 ℃, and the recrystallization temperature of aluminum chloride: 20-60 ℃, preferably: 20-40 ℃.
6. The process as claimed in any of claims 1 to 5, characterized in that the calcination temperature in step (6) is 900-3H, preferably from 1.5 to 2.85m3H; distilled water washing temperature: 70-100 ℃, preferably: 80-90 ℃.
7. The method according to any one of claims 1 to 6, wherein the white mud and the added LiBr, Al are added to the mixture obtained in step (7) on a dry basis2O3、TiO2MgO and CeO2The mass contents are respectively 60-70%, 10-15%, 5-10%, 3-7%, 2-5% and 3-5%.
8. The method as claimed in any one of the preceding claims, wherein the melt processing temperature in step (8) is 1400 ℃ and 1530 ℃ and the processing time is 3-4 hours.
9. The method according to any one of the preceding claims, wherein the primary heat treatment temperature in step (9) is 550 to 600 ℃; the crystallization time is 0.5-1.0 h; the secondary heat treatment temperature is 750-800 ℃; the crystallization time is 1.5-2.5 h.
10. Alumina and glass ceramics obtainable by a process according to any one of claims 1 to 9.
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