CN112110726A - Recycling and separating method of yttrium-stabilized zirconia bricks of waste furnace lining - Google Patents
Recycling and separating method of yttrium-stabilized zirconia bricks of waste furnace lining Download PDFInfo
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- 239000011449 brick Substances 0.000 title claims abstract description 46
- 239000002699 waste material Substances 0.000 title claims abstract description 30
- 229910002076 stabilized zirconia Inorganic materials 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004064 recycling Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 37
- 238000001354 calcination Methods 0.000 claims abstract description 28
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 8
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 33
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- 239000002585 base Substances 0.000 claims description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 15
- GNKHOVDJZALMGA-UHFFFAOYSA-N [Y].[Zr] Chemical compound [Y].[Zr] GNKHOVDJZALMGA-UHFFFAOYSA-N 0.000 claims description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 15
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 15
- 239000002131 composite material Substances 0.000 claims description 15
- 239000000654 additive Substances 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- -1 iron ions Chemical class 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000020477 pH reduction Effects 0.000 claims description 7
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 claims description 5
- 208000005156 Dehydration Diseases 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- 238000005260 corrosion Methods 0.000 claims description 5
- 230000007797 corrosion Effects 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 229960004887 ferric hydroxide Drugs 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000007781 pre-processing Methods 0.000 claims description 5
- DEXZEPDUSNRVTN-UHFFFAOYSA-K yttrium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Y+3] DEXZEPDUSNRVTN-UHFFFAOYSA-K 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 7
- 229910052594 sapphire Inorganic materials 0.000 abstract description 7
- 239000010980 sapphire Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000000919 ceramic Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 239000002910 solid waste Substances 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract 1
- 238000011069 regeneration method Methods 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- C22B59/00—Obtaining rare earth metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
-
- 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/06—Sulfating roasting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/14—Obtaining zirconium or hafnium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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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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Abstract
The invention discloses a recycling and separating method of yttrium-stabilized zirconia bricks of waste furnace linings, which relates to the field of zirconia ceramics and comprises the following steps: disassembling, pretreating, crushing, acidifying, roasting, separating in the first step, extracting and purifying in the first step, separating in the second step, extracting and purifying in the second step, concentrating and calcining; the invention reduces the burden and treatment cost brought by the waste solid generation of downstream customers, increases the utilization rate of resources, fills up the domestic blank, makes great contribution to the recycling of high-temperature application material wastes in the field of artificial sapphire crystal growth in China, fully utilizes the advantages of the yttrium stabilized zirconia waste furnace lining brick regeneration resources, can reduce the comprehensive use cost for the customers, increases the raw material business of companies, can reduce the comprehensive use cost to more than 40 percent of the original application products, promotes the comprehensive recycling of resources, reduces the generation of solid waste, promotes environment-friendly production and increases the green cycle benefit of enterprises.
Description
Technical Field
The invention relates to the field of zirconia ceramics, in particular to a recycling and separating method of yttrium-stabilized zirconia bricks of waste furnace linings.
Background
The service life of yttrium-stabilized zirconia bricks of sapphire crystal growth furnace linings is about 2-3 years generally, and because the yttrium-stabilized zirconia bricks are used for a long time in the environment of 2050 ℃, a large amount of metal oxides and alumina are attached to the yttrium-stabilized zirconia bricks in the using process, the yttrium-stabilized zirconia bricks cannot be directly reused, and if the removed waste furnace lining bricks are discarded and buried, resources are wasted and the environment is polluted. As is known, the production of domestic artificial sapphire crystals and other high-temperature fields all relate to materials using yttrium-stabilized zirconia in batches, the surfaces and a large number of pores of used waste furnace lining bricks contain a large number of oxides, the specific components are 10-20% of alumina, 60-85% of zirconia and 5-20% of yttria, and because the materials such as the zirconia, the rare earth yttria and the like are expensive, particularly the Y in the materials203The rare elements are separated for reuse along with the gradual reduction of the reserves of the rare elements, the importance of the rare elements for repeated reuse is more remarkable, and great economic benefits and social benefits can be generated, so that the recycling value of the used materials is particularly remarkable and important, and the method has great significance for recycling the used materials.
The technology treatment is not available for the reutilization of the ceramic lining bricks of the sapphire crystal growth furnace at home and abroad after the service life is over, and no relevant resource reutilization documents and patents related to the abandoned yttrium-stabilized zirconia furnace lining bricks used by the artificial sapphire crystal growth furnace are available at home and abroad according to knowledge and inquiry.
Disclosure of Invention
The recycling and separating method of the yttrium-stabilized zirconia bricks of the waste furnace lining provided by the invention solves the problems in the background technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
the recycling and separating method of the yttrium-stabilized zirconia bricks of the waste furnace lining specifically comprises the following steps:
s1, disassembling, namely disassembling the lining brick in the waste furnace, and washing the surface of the lining brick by using clear water to remove dust and impurities attached to the surface of the lining brick;
s2, preprocessing and crushing, namely putting the lining bricks disassembled in the step S1 into a double-helix crusher for crushing, and collecting crushed materials;
s3, acidifying, namely putting the material pretreated and crushed in the step S2 into a stirrer, adding sulfuric acid for acidifying, and passing through an acid-base regulator;
s4, roasting, namely adding an additive into the mixed solution subjected to the acidification treatment in the step S3, introducing the mixed solution into a roasting furnace for roasting treatment to obtain an acidified roasted material, and roasting for 0.5h at the roasting temperature of 200-300 ℃;
s5, first-step separation, namely adding hydrogen peroxide into the acidified roasted material obtained in the step S4, placing the acidified roasted material on a stirrer, and stirring for 0.5-1 h, wherein bivalent iron ions in the acidified roasted material are oxidized into trivalent iron ions by the hydrogen peroxide to form a solution a;
s6, performing first-step extraction and purification, namely putting the solution a in the step S5 on a centrifugal extractor for centrifugal extraction and separation to separate out a reddish-brown ferric hydroxide solution, wherein the remaining solution b contains yttrium and zirconium;
s7, separating in a second step, namely putting the solution b obtained in the step S6 into a stirrer to be stirred, adding additives, and simultaneously adding ammonium sulfate and ammonia water to generate a zirconium-yttrium composite material precursor;
s8, extracting and purifying, namely introducing deionized water into the zirconium-yttrium composite material precursor generated in the step S7 for washing, filtering by using a filter screen, and dropwise adding an acid-base regulator to adjust the pH value to be neutral to obtain a precipitate a;
s9, concentrating, namely putting the precipitate a obtained in the step S8 into a concentrator for dehydration treatment, and drying to obtain a precipitate b, wherein the precipitate b is specifically a zirconium hydroxide precipitate and a yttrium hydroxide precipitate;
and S10, calcining, namely putting the precipitate b obtained in the step S8 into a high-temperature calcining furnace for calcining, and calcining to obtain the zirconium-yttrium composite powder.
Preferably, the additives used in S4 and S7 are mainly wine polyethylene glycol additives.
Preferably, the PH value adjusted by adding the acid-base modifier during the acidification treatment in S3 is 3-5, and the PH value adjusted to be 7 by adding the acid-base modifier in S8.
Preferably, when the ammonium sulfate and the ammonia water are dropwise added into the S7, the solution b is slowly dropwise added, and the temperature of the solution b is controlled to be 50-70 ℃.
Preferably, the filter screen used in S8 is specifically an acid and alkali corrosion resistant filter screen, and the mesh number of the filter screen is specifically 200 meshes.
Preferably, the temperature of the concentration in the S9 is controlled to be 300-350 ℃.
Preferably, the temperature of the calcination in S10 is controlled to be 1250-1400 ℃, and the calcination time is 1-1.5 h.
In the invention: the invention greatly reduces the burden and the treatment cost brought by the waste solid generation of downstream customers, increases the utilization rate of resources, fills the domestic blank, makes great contribution to the recycling of high-temperature application material wastes in the field of artificial sapphire crystal growth in China, fully utilizes the advantages of the regenerated resources of the yttrium stabilized zirconia waste furnace lining bricks, can reduce the comprehensive use cost for the customers, increases the raw material business of companies, and can reduce the comprehensive use cost to more than 40 percent of the original application product; the method promotes the comprehensive reuse of resources, reduces the generation of solid wastes, promotes the environment-friendly production, increases the green cycle benefits of enterprises, and has wide popularization and application prospects.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example one
The recycling and separating method of the yttrium-stabilized zirconia bricks of the waste furnace lining specifically comprises the following steps:
s1, disassembling, namely disassembling the lining brick in the waste furnace, and washing the surface of the lining brick by using clear water to remove dust and impurities attached to the surface of the lining brick;
s2, preprocessing and crushing, namely putting the lining bricks disassembled in the step S1 into a double-helix crusher for crushing, and collecting crushed materials;
s3, acidifying, namely putting the material pretreated and crushed in the step S2 into a stirrer, adding sulfuric acid for acidifying, and regulating the acidity to be 3 by using an acid-base regulator;
s4, roasting, namely adding a polyethylene glycol additive into the mixed solution subjected to the acidification treatment in the step S3, introducing the mixed solution into a roasting furnace for roasting treatment to obtain an acidified roasted material, and roasting for 0.5h at the roasting temperature of 200 ℃;
s5, first-step separation, namely adding hydrogen peroxide into the acidified roasted material obtained in the step S4, and stirring the acidified roasted material on a stirrer for 0.5h, wherein bivalent iron ions in the acidified roasted material are oxidized into trivalent iron ions by the hydrogen peroxide to form a solution a;
s6, performing first-step extraction and purification, namely putting the solution a in the step S5 on a centrifugal extractor for centrifugal extraction and separation to separate out a reddish-brown ferric hydroxide solution, wherein the remaining solution b contains yttrium and zirconium;
s7, separating in a second step, namely putting the solution b obtained in the step S6 into a stirrer, stirring, adding a polyethylene glycol additive, simultaneously adding ammonium sulfate and ammonia water, slowly adding the ammonium sulfate and the ammonia water when adding the ammonium sulfate and the ammonia water, and controlling the temperature of the solution b to be 50 ℃ when adding the ammonium sulfate and the ammonia water to generate a zirconium-yttrium composite material precursor;
s8, performing second-step extraction and purification, namely introducing deionized water into the zirconium-yttrium composite material precursor generated in the step S7 for washing, filtering by using a filter screen, wherein the used filter screen is specifically an acid-base corrosion resistant filter screen, the mesh number of the filter screen is specifically 200 meshes, and dropwise adding an acid-base regulator to adjust the pH value to be neutral 7 to obtain a precipitate a;
s9, concentrating, namely putting the precipitate a obtained in the step S8 into a concentrator for dehydration treatment, and drying to obtain a precipitate b, wherein the precipitate b is specifically a zirconium hydroxide precipitate and a yttrium hydroxide precipitate, and the temperature during concentration is controlled at 300 ℃;
and S10, calcining, namely calcining the precipitate b obtained in the step S8 in a high-temperature calcining furnace, controlling the temperature in the calcining process at 1250 ℃ and the calcining time at 1h to obtain the zirconium-yttrium composite powder.
Example two
The recycling and separating method of the yttrium-stabilized zirconia bricks of the waste furnace lining specifically comprises the following steps:
s1, disassembling, namely disassembling the lining brick in the waste furnace, and washing the surface of the lining brick by using clear water to remove dust and impurities attached to the surface of the lining brick;
s2, preprocessing and crushing, namely putting the lining bricks disassembled in the step S1 into a double-helix crusher for crushing, and collecting crushed materials;
s3, acidifying, namely putting the material pretreated and crushed in the step S2 into a stirrer, adding sulfuric acid for acidifying, and regulating the acidity to be 4 by using an acid-base regulator;
s4, roasting, namely adding a polyethylene glycol additive into the mixed solution subjected to the acidification treatment in the step S3, introducing the mixed solution into a roasting furnace for roasting treatment to obtain an acidified roasted material, and roasting for 0.5h at the roasting temperature of 250 ℃;
s5, first-step separation, namely adding hydrogen peroxide into the acidified roasted material obtained in the step S4, and stirring the acidified roasted material on a stirrer for 0.75h, wherein bivalent iron ions in the acidified roasted material are oxidized into trivalent iron ions by the hydrogen peroxide to form a solution a;
s6, performing first-step extraction and purification, namely putting the solution a in the step S5 on a centrifugal extractor for centrifugal extraction and separation to separate out a reddish-brown ferric hydroxide solution, wherein the remaining solution b contains yttrium and zirconium;
s7, separating in a second step, namely putting the solution b obtained in the step S6 into a stirrer, stirring, adding a polyethylene glycol additive, simultaneously adding ammonium sulfate and ammonia water, slowly adding the ammonium sulfate and the ammonia water when adding the ammonium sulfate and the ammonia water, and controlling the temperature of the solution b to be 60 ℃ when adding the ammonium sulfate and the ammonia water to generate a zirconium-yttrium composite material precursor;
s8, performing second-step extraction and purification, namely introducing deionized water into the zirconium-yttrium composite material precursor generated in the step S7 for washing, filtering by using a filter screen, wherein the used filter screen is specifically an acid-base corrosion resistant filter screen, the mesh number of the filter screen is specifically 200 meshes, and dropwise adding an acid-base regulator to adjust the pH value to be neutral 7 to obtain a precipitate a;
s9, concentrating, namely putting the precipitate a obtained in the step S8 into a concentrator for dehydration treatment, and drying to obtain a precipitate b, wherein the precipitate b is specifically a zirconium hydroxide precipitate and a yttrium hydroxide precipitate, and the temperature during concentration is controlled at 330 ℃;
and S10, calcining, namely calcining the precipitate b obtained in the step S8 in a high-temperature calcining furnace, controlling the temperature in the calcining process to 1325 ℃, and calcining for 1h to obtain the zirconium-yttrium composite powder.
EXAMPLE III
The recycling and separating method of the yttrium-stabilized zirconia bricks of the waste furnace lining specifically comprises the following steps:
s1, disassembling, namely disassembling the lining brick in the waste furnace, and washing the surface of the lining brick by using clear water to remove dust and impurities attached to the surface of the lining brick;
s2, preprocessing and crushing, namely putting the lining bricks disassembled in the step S1 into a double-helix crusher for crushing, and collecting crushed materials;
s3, acidifying, namely putting the material pretreated and crushed in the step S2 into a stirrer, adding sulfuric acid for acidifying, and adjusting the acidity to be 5 by using an acid-base regulator;
s4, roasting, namely adding a polyethylene glycol additive into the mixed solution subjected to the acidification treatment in the step S3, introducing the mixed solution into a roasting furnace for roasting treatment to obtain an acidified roasted material, and roasting for 0.5h at the roasting temperature of 300 ℃;
s5, first-step separation, namely adding hydrogen peroxide into the acidified roasted material obtained in the step S4, and stirring the acidified roasted material on a stirrer for 1h, wherein bivalent iron ions in the acidified roasted material are oxidized into trivalent iron ions by the hydrogen peroxide to form a solution a;
s6, performing first-step extraction and purification, namely putting the solution a in the step S5 on a centrifugal extractor for centrifugal extraction and separation to separate out a reddish-brown ferric hydroxide solution, wherein the remaining solution b contains yttrium and zirconium;
s7, separating in a second step, namely putting the solution b obtained in the step S6 into a stirrer, stirring, adding a polyethylene glycol additive, simultaneously adding ammonium sulfate and ammonia water, slowly adding the ammonium sulfate and the ammonia water when adding the ammonium sulfate and the ammonia water, and controlling the temperature of the solution b to be 70 ℃ when adding the solution b to generate a zirconium-yttrium composite material precursor;
s8, performing second-step extraction and purification, namely introducing deionized water into the zirconium-yttrium composite material precursor generated in the step S7 for washing, filtering by using a filter screen, wherein the used filter screen is specifically an acid-base corrosion resistant filter screen, the mesh number of the filter screen is specifically 200 meshes, and dropwise adding an acid-base regulator to adjust the pH value to be neutral 7 to obtain a precipitate a;
s9, concentrating, namely putting the precipitate a obtained in the step S8 into a concentrator for dehydration treatment, and drying to obtain a precipitate b, wherein the precipitate b is specifically a zirconium hydroxide precipitate and a yttrium hydroxide precipitate, and the temperature during concentration is controlled at 350 ℃;
and S10, calcining, namely calcining the precipitate b obtained in the step S8 in a high-temperature calcining furnace, controlling the temperature at 1400 ℃ during calcining, and calcining for 1h to obtain the zirconium-yttrium composite powder.
The performance indexes that various elements after the yttrium stabilized zirconia of the waste furnace lining of the sapphire crystal growth furnace is converted and decomposed can be actually achieved are as follows:
although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The recycling and separating method of the yttrium-stabilized zirconia bricks of the waste furnace lining is characterized by comprising the following steps:
s1, disassembling, namely disassembling the lining brick in the waste furnace, and washing the surface of the lining brick by using clear water to remove dust and impurities attached to the surface of the lining brick;
s2, preprocessing and crushing, namely putting the lining bricks disassembled in the step S1 into a double-helix crusher for crushing, and collecting crushed materials;
s3, acidifying, namely putting the material pretreated and crushed in the step S2 into a stirrer, adding sulfuric acid for acidifying, and passing through an acid-base regulator;
s4, roasting, namely adding an additive into the mixed solution subjected to the acidification treatment in the step S3, introducing the mixed solution into a roasting furnace for roasting treatment to obtain an acidified roasted material, and roasting for 0.5h at the roasting temperature of 200-300 ℃;
s5, first-step separation, namely adding hydrogen peroxide into the acidified roasted material obtained in the step S4, placing the acidified roasted material on a stirrer, and stirring for 0.5-1 h, wherein bivalent iron ions in the acidified roasted material are oxidized into trivalent iron ions by the hydrogen peroxide to form a solution a;
s6, performing first-step extraction and purification, namely putting the solution a in the step S5 on a centrifugal extractor for centrifugal extraction and separation to separate out a reddish-brown ferric hydroxide solution, wherein the remaining solution b contains yttrium and zirconium;
s7, separating in a second step, namely putting the solution b obtained in the step S6 into a stirrer to be stirred, adding additives, and simultaneously adding ammonium sulfate and ammonia water to generate a zirconium-yttrium composite material precursor;
s8, extracting and purifying, namely introducing deionized water into the zirconium-yttrium composite material precursor generated in the step S7 for washing, filtering by using a filter screen, and dropwise adding an acid-base regulator to adjust the pH value to be neutral to obtain a precipitate a;
s9, concentrating, namely putting the precipitate a obtained in the step S8 into a concentrator for dehydration treatment, and drying to obtain a precipitate b, wherein the precipitate b is specifically a zirconium hydroxide precipitate and a yttrium hydroxide precipitate;
and S10, calcining, namely putting the precipitate b obtained in the step S8 into a high-temperature calcining furnace for calcining, and calcining to obtain the zirconium-yttrium composite powder.
2. The method for recycling and separating yttrium-stabilized zirconia bricks of waste furnace linings according to claim 1, characterized by comprising the following steps: the additives used in S4 and S7 are mainly wine polyethylene glycol additives.
3. The method for recycling and separating yttrium-stabilized zirconia bricks of waste furnace linings according to claim 1, characterized by comprising the following steps: and the pH value adjusted by adding an acid-base regulator in the acidification treatment in the S3 is 3-5, and the pH value adjusted to be 7 by adding the acid-base regulator in the S8.
4. The method for recycling and separating yttrium-stabilized zirconia bricks of waste furnace linings according to claim 1, characterized by comprising the following steps: and slowly dripping ammonium sulfate and ammonia water in the S7, and controlling the temperature of the solution b to be 50-70 ℃ during dripping.
5. The method for recycling and separating yttrium-stabilized zirconia bricks of waste furnace linings according to claim 1, characterized by comprising the following steps: the filter screen used in the S8 is specifically an acid and alkali corrosion resistant filter screen, and the mesh number of the filter screen is specifically 200 meshes.
6. The method for recycling and separating yttrium-stabilized zirconia bricks of waste furnace linings according to claim 1, characterized by comprising the following steps: the temperature of the S9 during concentration is controlled to be 300-350 ℃.
7. The method for recycling and separating yttrium-stabilized zirconia bricks of waste furnace linings according to claim 1, characterized by comprising the following steps: the temperature of the calcination in the S10 is controlled to be 1250-1400 ℃, and the calcination time is 1-1.5 h.
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