CN114606571A - Alumina whisker prepared from blast furnace slag and preparation method thereof - Google Patents
Alumina whisker prepared from blast furnace slag and preparation method thereof Download PDFInfo
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- CN114606571A CN114606571A CN202210350782.6A CN202210350782A CN114606571A CN 114606571 A CN114606571 A CN 114606571A CN 202210350782 A CN202210350782 A CN 202210350782A CN 114606571 A CN114606571 A CN 114606571A
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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 86
- 239000002893 slag Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 131
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000002253 acid Substances 0.000 claims abstract description 67
- 238000005406 washing Methods 0.000 claims abstract description 64
- 229910052742 iron Inorganic materials 0.000 claims abstract description 50
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 239000002243 precursor Substances 0.000 claims description 28
- 239000012065 filter cake Substances 0.000 claims description 27
- 239000012286 potassium permanganate Substances 0.000 claims description 20
- 238000005554 pickling Methods 0.000 claims description 19
- 238000001704 evaporation Methods 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 230000008020 evaporation Effects 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 150000004676 glycans Chemical class 0.000 claims description 6
- 229920001282 polysaccharide Polymers 0.000 claims description 6
- 239000005017 polysaccharide Substances 0.000 claims description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 6
- 150000002772 monosaccharides Chemical class 0.000 claims description 5
- 239000003599 detergent Substances 0.000 claims description 3
- 238000005649 metathesis reaction Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 abstract description 18
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 11
- 229940118662 aluminum carbonate Drugs 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000000377 silicon dioxide Substances 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005507 spraying Methods 0.000 description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 30
- 230000007480 spreading Effects 0.000 description 19
- 239000002245 particle Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000006386 neutralization reaction Methods 0.000 description 8
- 229930091371 Fructose Natural products 0.000 description 7
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 7
- 239000005715 Fructose Substances 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 229910000805 Pig iron Inorganic materials 0.000 description 5
- 229920002472 Starch Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 5
- 239000008107 starch Substances 0.000 description 5
- 235000019698 starch Nutrition 0.000 description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229940103272 aluminum potassium sulfate Drugs 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000007716 flux method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 description 2
- 235000011151 potassium sulphates Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B3/00—General features in the manufacture of pig-iron
- C21B3/04—Recovery of by-products, e.g. slag
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to the technical field of alumina whisker materials, and provides a method for preparing alumina whiskers by using blast furnace slag, which comprises the steps of using the blast furnace slag as a main raw material, dissolving alumina and impurities in the blast furnace slag by acid washing, recovering silicon dioxide, adjusting the pH value of acid washing filtrate to facilitate subsequent iron removal treatment, adding an iron remover to remove iron, and eliminating the interference of iron elements on double decomposition reaction; then adding a carbon source to perform double decomposition reaction with the aluminum element in the filtrate to generate aluminum carbonate, and finally calcining to decompose the aluminum carbonate to obtain the aluminum oxide whisker. The embodiment result shows that the diameter of the alumina whisker prepared by the preparation method provided by the invention is 280-392 nm, the radial dimension error is 18-23 nm, the length is 33-51 mu m, the length-diameter ratio is 86-176, the purity of the alumina phase is more than or equal to 98.4%, the elastic modulus is 385-397 GPa, and the room temperature hardness is 71-75 GPa.
Description
Technical Field
The invention relates to the technical field of alumina whisker materials, in particular to an alumina whisker prepared by using blast furnace slag and a preparation method thereof.
Background
Blast furnace slag is waste slag generated in pig iron smelting, and during the pig iron smelting, raw materials of a blast furnace are added, and besides iron ore and fuel, limestone and dolomite are also added to serve as fluxing agents. When the furnace temperature reaches 1400-1600 ℃, the fluxing agent and the iron ore react at high temperature to generate pig iron and blast furnace slag. Blast furnace slag is a fusible material consisting of gangue, ash, flux and other impurities that cannot enter pig iron. With the development of the steel industry in China, the discharge amount of blast furnace slag is increased day by day, and the environmental pollution caused by the huge industrial solid waste is obvious.
The alumina whisker has high specific strength, high specific modulus and excellent high temperature oxidation resistance, and is an important reinforcing material for high temperature composite materials, especially high temperature ceramic materials. The commonly used synthesis method of the alumina whisker mainly comprises Al-SiO2Methods, flux methods, and the like. Wherein, Al-SiO2The method is the method which is adopted most in the preparation of the aluminum oxide whisker at present and adopts metal Al and SiO2And after the powder is uniformly mixed, reacting under the Ar gas condition to obtain the alumina whisker. However, the method requires introducing protective gas in the preparation process, which limits the industrial application, and the raw materials are mostly pure substances, which increases the preparation cost. The flux method is characterized in that aluminum potassium sulfate is used as a raw material, potassium sulfate is used as a flux, the aluminum potassium sulfate and the potassium sulfate are mixed and ground uniformly according to a certain proportion, roasting is carried out, and after cooling, leaching treatment is carried out on a product to obtain the aluminum oxide whisker. However, the raw materials used in the method are mostly pure substances, and the cost is high. Therefore, how to prepare the alumina whisker with high specific strength and high specific modulus by using the blast furnace slag becomes a problem to be solved in the field.
Disclosure of Invention
The invention aims to provide an alumina whisker prepared from blast furnace slag and a preparation method thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a method for preparing alumina whiskers by using blast furnace slag, which comprises the following steps:
(1) carrying out acid pickling on blast furnace slag to obtain acid pickling filtrate;
(2) adding a pH regulator into the acid-washing filtrate obtained in the step (1) to obtain a neutralized filtrate;
(3) adding an iron remover into the neutralized filtrate obtained in the step (2) to remove iron, and then adding a carbon source to perform double decomposition reaction to obtain an alumina whisker precursor;
(4) and (4) calcining the alumina whisker precursor obtained in the step (3) under a vacuum condition to obtain the alumina whisker.
Preferably, the pickling solution used for pickling in the step (1) is a hydrochloric acid solution; the concentration of the hydrochloric acid solution is 8-10 mol/L.
Preferably, the pH value of the neutralization filtrate in the step (2) is 5.5-6.
Preferably, the iron remover in the step (3) comprises potassium permanganate or potassium dichromate; and taking the volume of the neutralized filtrate as a reference, wherein the dosage of the iron removing agent is 0.45-0.64 g/L.
Preferably, the carbon source in step (3) comprises a monosaccharide or a polysaccharide; and taking the volume of the neutralized filtrate as a reference, wherein the dosage of the carbon source is 110-140 g/L.
Preferably, the calcining temperature in the step (4) is 970-1020 ℃, and the vacuum degree under the vacuum condition is 4 x 10-3～6×10-3Pa。
Preferably, the metathesis reaction in the step (3) further comprises post-treatment after completion; the post-treatment comprises filtration, evaporation, washing and water removal treatment which are sequentially carried out.
Preferably, the temperature of the evaporation is 150-175 ℃; the detergent used for washing is absolute ethyl alcohol; the temperature of the dewatering treatment is 210-230 ℃, and the dewatering treatment time is 23-26 min per kilogram of filter cake obtained by filtering.
The invention also provides the alumina whisker prepared by the preparation method in the technical scheme.
Preferably, the diameter of the alumina whisker is 280-392 nm, the length of the alumina whisker is 33-51 μm, the length-diameter ratio of the alumina whisker is 86-176, the purity of an alumina phase is more than or equal to 98.4%, the elastic modulus of the alumina phase is 385-397 GPa, and the room-temperature hardness of the alumina whisker is 71-75 GPa.
The invention provides a method for preparing alumina whiskers by using blast furnace slag, which comprises the following steps:
(1) carrying out acid pickling on blast furnace slag to obtain acid pickling filtrate; (2) adding a pH regulator into the acid-washing filtrate obtained in the step (1) to obtain a neutralized filtrate; (3) adding an iron remover into the neutralized filtrate obtained in the step (2) to remove iron, and then adding a carbon source to perform double decomposition reaction to obtain an alumina whisker precursor; (4) and (4) calcining the precursor of the alumina whisker obtained in the step (3) under a vacuum condition to obtain the alumina whisker. The method takes the blast furnace slag as a main raw material, dissolves alumina and impurities in the blast furnace slag through acid washing, recovers silicon dioxide, adjusts the pH value of acid washing filtrate to facilitate subsequent iron removal treatment, and then adds an iron remover to remove iron so as to eliminate the interference of iron elements on double decomposition reaction; then adding a carbon source to perform double decomposition reaction with the aluminum element in the filtrate to generate aluminum carbonate, and finally calcining to decompose the aluminum carbonate to obtain the aluminum oxide whisker. The embodiment result shows that the diameter of the alumina whisker prepared by the preparation method provided by the invention is 280-392 nm, the radial dimension error is 18-23 nm, the length is 33-51 mu m, the length-diameter ratio is 86-176, the purity of the alumina phase is more than or equal to 98.4%, the elastic modulus is 385-397 GPa, and the room temperature hardness is 71-75 GPa.
Detailed Description
The invention provides a method for preparing alumina whiskers by using blast furnace slag, which comprises the following steps:
(1) carrying out acid pickling on blast furnace slag to obtain acid pickling filtrate;
(2) adding a pH regulator into the acid-washing filtrate obtained in the step (1) to obtain a neutralized filtrate;
(3) adding an iron remover into the neutralized filtrate obtained in the step (2) to remove iron, and then adding a carbon source to perform double decomposition reaction to obtain an alumina whisker precursor;
(4) and (4) calcining the precursor of the alumina whisker obtained in the step (3) under a vacuum condition to obtain the alumina whisker.
The invention carries out acid cleaning on blast furnace slag to obtain acid cleaning filtrate. The invention dissolves alumina and impurities in blast furnace slag by acid washing and recovers silicon dioxide.
The source of the blast furnace slag is not particularly limited in the present invention, and it is sufficient to use waste slag generated in pig iron smelting, which is well known to those skilled in the art. In the present invention, the average particle size of the blast furnace slag is preferably 60 to 90 μm, and more preferably 75 to 85 μm. The present invention preferably controls the average particle size of the blast furnace slag within the above range, which is advantageous in accelerating the dissolution of alumina and other components in the blast furnace slag during the pickling process.
In the present invention, the acid washing solution used for the acid washing is preferably a hydrochloric acid solution. In the invention, the concentration of the hydrochloric acid solution is preferably 8-10 mol/L, and more preferably 8-9 mol/L.
In the present invention, the acid washing is specifically preferably: spreading blast furnace slag on a screen, spraying a hydrochloric acid solution to the surface of the blast furnace slag, stopping spraying acid and feeding after a period of time, circularly spraying the filtrate filtered by the screen to the blast furnace slag, and carrying out circular pickling to obtain pickling filtrate and residues. According to the method, the hydrochloric acid solution is preferably sprayed while the blast furnace slag is spread to initially dissolve the alumina in the blast furnace slag, and the filtrate filtered by the screen is used for circularly pickling the blast furnace slag, so that the alumina in the blast furnace slag is further dissolved, the acid liquor consumption is saved, and the acid liquor pollution is prevented.
In the invention, the spreading speed of the blast furnace slag is preferably 180-260 g/s; the spreading thickness of the blast furnace slag is preferably 1.4-1.9 mm; the sieve mesh size of the sieve mesh is preferably 230-270 meshes; the acid feeding speed of the hydrochloric acid solution is preferably 140-190 mL/s; the spraying speed of the hydrochloric acid solution is preferably 54-66 m/s; the time for stopping spraying the acid and feeding is preferably 23-28 s.
In the invention, the ejection amount of the filtrate filtered by the screen is preferably 190-240 mL/s; the spraying speed of the filtrate filtered by the screen is preferably 67-73 m/s; the time of the circulating acid washing is preferably 7-10 s.
After the acid washing filtrate is obtained, the pH regulator is added into the acid washing filtrate to obtain the neutralized filtrate. The pH value of the acid washing filtrate is adjusted by adding the pH regulator, so that the subsequent iron removal treatment can be smoothly carried out.
In the present invention, the pH adjuster preferably includes sodium hydroxide, potassium hydroxide, or aqueous ammonia, more preferably sodium hydroxide or potassium hydroxide. In the invention, the pH value of the neutralization filtrate is preferably 5.5-6, and more preferably 5.6-5.9.
After the neutralized filtrate is obtained, adding an iron removing agent into the neutralized filtrate for iron removal, and then adding a carbon source for double decomposition reaction to obtain an alumina whisker precursor. The iron is removed by adding the iron remover so as to eliminate the interference of iron elements on the double decomposition reaction; then adding a carbon source to perform double decomposition reaction with the aluminum hydroxide in the filtrate to generate aluminum carbonate.
In the present invention, the iron remover preferably comprises potassium permanganate or potassium dichromate, more preferably potassium permanganate. In the invention, the dosage of the iron removing agent is preferably 0.45-0.64 g/L and more preferably 0.48-0.62 g/L based on the volume of the neutralized filtrate. The invention preferably controls the dosage of the iron remover in the range, realizes iron removal without wasting raw materials, and is beneficial to obtaining high-purity alumina whisker materials. The method changes the iron simple substance into iron ions by adding the iron remover to perform redox reaction with iron in the neutralized filtrate so as to eliminate the interference of iron elements on double decomposition reaction.
In the present invention, the carbon source preferably includes monosaccharide or polysaccharide, more preferably polysaccharide. In the present invention, the monosaccharide preferably includes glucose or fructose; the polysaccharide preferably comprises starch or cellulose. The invention preferably adopts monosaccharide or polysaccharide as the carbon source, thereby ensuring the environmental protection and resource sufficiency of the carbon source, preventing the hydrolysis of aluminum carbonate and ensuring the stability of the formation reaction of the carbonate.
In the invention, the dosage of the carbon source is preferably 110-140 g/L, and more preferably 120-135 g/L based on the volume of the neutralized filtrate. The invention preferably controls the dosage of the carbon source within the range, which is favorable for obtaining the alumina whisker material with high purity.
After the double decomposition reaction is finished, the product obtained by the double decomposition reaction is preferably subjected to post-treatment to obtain the precursor of the aluminum oxide whisker. In the present invention, the post-treatment preferably includes filtration, evaporation, washing and water removal treatment, which are sequentially performed.
The operation of filtration and evaporation is not particularly limited in the present invention, and the technical scheme of filtration and evaporation known to those skilled in the art can be adopted. In the invention, the evaporation temperature is preferably 150-175 ℃, and more preferably 160-175 ℃. The present invention preferably removes the solvent water from the metathesis reaction product by evaporation.
The washing operation is not particularly limited in the present invention, and a washing method known to those skilled in the art may be employed. In the present invention, the detergent used for the washing is preferably anhydrous ethanol. The present invention preferably removes iron-containing complexes and other soluble materials by washing.
In the invention, the temperature of the water removal treatment is preferably 210-230 ℃, and more preferably 220-230 ℃; the time of the dewatering treatment is preferably 23-26 min per kilogram of filter cake obtained by filtering, and more preferably 24-25 min. The present invention preferably removes crystal water in the alumina whisker precursor by a water removal treatment.
After the precursor of the alumina whisker is obtained, the precursor of the alumina whisker is calcined to obtain the alumina whisker. The aluminum carbonate is decomposed by calcination, and the alumina whisker is obtained.
In the invention, the calcination temperature is preferably 970-1020 ℃, and more preferably 980-1010 ℃; the calcination time is preferably 1.2-1.9 h, and more preferably 1.4-1.7 h. In the present inventionThe degree of vacuum of the vacuum condition is preferably 4X 10-3～6×10-3Pa, more preferably 4X 10-3Pa。
The method takes the blast furnace slag as a main raw material, dissolves alumina and impurities in the blast furnace slag through acid washing, recovers silicon dioxide, adjusts the pH value of acid washing filtrate to facilitate subsequent iron removal treatment, and then adds an iron remover to remove iron so as to eliminate the interference of iron elements on double decomposition reaction; then adding a carbon source to perform double decomposition reaction with the aluminum element in the filtrate to generate aluminum carbonate, and finally calcining to decompose the aluminum carbonate to obtain the aluminum oxide whisker.
The invention also provides the alumina whisker prepared by the preparation method in the technical scheme. The alumina whisker provided by the invention has uniform size and excellent mechanical property.
In the invention, the diameter of the alumina whisker is preferably 280-392 nm, the length is preferably 33-51 μm, the length-diameter ratio is preferably 86-176, the purity of the alumina phase is preferably equal to or more than 98.4%, the elastic modulus is preferably 385-397 GPa, and the room-temperature hardness is preferably 71-75 GPa.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Spreading blast furnace slag with the average particle size of 75 mu m on a screen mesh with the mesh size of 230 meshes at the speed of 180g/s, spreading to the thickness of 1.4mm, spraying hydrochloric acid solution with the concentration of 8mol/L onto the surface of the blast furnace slag at the acid feeding speed of 140mL/s and the spraying speed of 54m/s, stopping spraying the acid and feeding after 23s, placing filtrate filtered by the screen mesh in a circulating device for circular acid washing, wherein the spraying amount of the filtrate is 190mL/s, the spraying speed of the filtrate is 67m/s, finishing the circular acid washing after 7s, removing the filtrate out of the circulating device, recovering residual residues on the screen mesh, and repeating for 6 times in this way to obtain acid washing filtrate;
(2) adding sodium hydroxide into the acid-washing filtrate obtained in the step (1) to adjust the pH value of the filtrate to 5.5 to obtain neutralized filtrate, then adding potassium permanganate into the neutralized filtrate to remove iron, then adding glucose to perform double decomposition reaction, filtering after the reaction is finished, evaporating a filter cake at 150 ℃, washing the filter cake with absolute ethyl alcohol, and performing water removal treatment at 210 ℃ for 23min per kilogram of filter cake to obtain an aluminum oxide whisker precursor; wherein the dosage of potassium permanganate is 0.45g/L and the dosage of glucose is 110g/L on the basis of the volume of the neutralization filtrate;
(3) under vacuum degree of 4X 10-3And (3) calcining the precursor of the alumina whisker obtained in the step (2) at Pa and at 970 ℃, and obtaining the alumina whisker after 1.3 h.
Example 2
(1) Spreading blast furnace slag with the average particle size of 77 mu m on a screen mesh with the mesh size of 240 meshes at the speed of 190g/s, wherein the spreading thickness is 1.4mm, spraying hydrochloric acid solution with the concentration of 9mol/L onto the surface of the blast furnace slag at the acid supply speed of 150mL/s and the spraying speed of 56m/s, stopping spraying acid and feeding after 25s, placing filtrate filtered by the screen mesh in a circulating device for circulating acid washing, wherein the spraying amount of the filtrate is 200mL/s, the spraying speed of the filtrate is 69m/s, finishing the circulating acid washing after 8s, removing the filtrate from the circulating device, recovering residual residues on the screen mesh, and repeating for 8 times to obtain the filtrate, namely acid washing filtrate;
(2) adding sodium hydroxide into the acid-washing filtrate obtained in the step (1) to adjust the pH value of the filtrate to 5.6 to obtain neutralized filtrate, then adding potassium permanganate into the neutralized filtrate to remove iron, then adding fructose to perform double decomposition reaction, filtering after the reaction is finished, evaporating a filter cake at 160 ℃, washing the filter cake with absolute ethyl alcohol, and then performing water removal treatment at 220 ℃ for 24min per kilogram of filter cake to obtain an aluminum oxide whisker precursor; wherein the dosage of potassium permanganate is 0.48g/L and the dosage of fructose is 120g/L on the basis of the volume of the neutralization filtrate;
(3) under vacuum degree of 4X 10-3Pa, temperature of 980 DEG CCalcining the precursor of the alumina whisker obtained in the step (2) under the condition of (1.7) h to obtain the alumina whisker.
Example 3
(1) Spreading blast furnace slag with the average particle size of 79 mu m on a screen mesh with the mesh size of 250 meshes at the speed of 200g/s, wherein the spreading thickness is 1.4mm, spraying hydrochloric acid solution with the concentration of 10mol/L onto the surface of the blast furnace slag at the acid feeding speed of 160mL/s and the spraying speed of 58m/s, stopping spraying acid and feeding after 28s, placing filtrate filtered by the screen mesh in a circulating device for circulating acid washing, wherein the spraying amount of the filtrate is 240mL/s, the spraying speed of the filtrate is 73m/s, finishing the circulating acid washing after 10s, removing the filtrate from the circulating device, recovering residual residues on the screen mesh, and repeating for 9 times to obtain the filtrate, namely acid washing filtrate;
(2) adding sodium hydroxide into the acid-washing filtrate obtained in the step (1) to adjust the pH value of the filtrate to 6 to obtain neutralized filtrate, then adding potassium permanganate into the neutralized filtrate to remove iron, then adding starch to perform double decomposition reaction, filtering after the reaction is finished, evaporating a filter cake at 175 ℃, washing the filter cake with absolute ethyl alcohol, and performing water removal treatment at 230 ℃ for 26min per kilogram of filter cake to obtain an aluminum oxide whisker precursor; wherein the dosage of potassium permanganate is 0.64g/L and the dosage of starch is 140g/L on the basis of the volume of the neutralization filtrate;
(3) under vacuum degree of 4X 10-3And (3) calcining the precursor of the alumina whisker obtained in the step (2) under the conditions of Pa and the temperature of 1020 ℃, and obtaining the alumina whisker after 1.6 h.
Example 4
(1) Spreading blast furnace slag with the average particle size of 85 mu m on a screen mesh with the mesh size of 270 meshes at the speed of 260g/s, wherein the spreading thickness is 1.4mm, spraying hydrochloric acid solution with the concentration of 10mol/L onto the surface of the slag at the acid supply speed of 190mL/s and the spraying speed of 66m/s, stopping spraying acid and feeding after 28s, placing filtrate filtered by the screen mesh in a circulating device for circular pickling, wherein the spraying amount of the filtrate is 240mL/s, the spraying speed of the filtrate is 73m/s, finishing the circular pickling after 10s, removing the filtrate from the circulating device, recovering residual residues on the screen mesh, and repeating for 7 times to obtain the filtrate, namely pickling filtrate;
(2) adding sodium hydroxide into the acid-washing filtrate obtained in the step (1) to adjust the pH value of the filtrate to 6 to obtain neutralized filtrate, then adding potassium permanganate into the neutralized filtrate to remove iron, then adding starch to perform double decomposition reaction, filtering after the reaction is finished, evaporating a filter cake at 175 ℃, washing the filter cake with absolute ethyl alcohol, and performing water removal treatment at 230 ℃ for 26min per kilogram of filter cake to obtain an aluminum oxide whisker precursor; wherein the dosage of potassium permanganate is 0.64g/L and the dosage of starch is 140g/L on the basis of the volume of the neutralization filtrate;
(3) under vacuum degree of 4X 10-3And (3) calcining the precursor of the alumina whisker obtained in the step (2) under the conditions of Pa and the temperature of 1020 ℃, and obtaining the alumina whisker after 1.7 h.
Example 5
(1) Spreading blast furnace slag with the average particle size of 80 mu m on a screen mesh with the mesh size of 260 meshes at the speed of 210g/s, wherein the spreading thickness is 1.4mm, spraying hydrochloric acid solution with the concentration of 10mol/L onto the surface of the blast furnace slag at the acid feeding speed of 180mL/s and the spraying speed of 62m/s, stopping spraying acid and feeding after 27s, placing filtrate filtered by the screen mesh in a circulating device for circulating acid washing, wherein the spraying amount of the filtrate is 230mL/s, the spraying speed of the filtrate is 73m/s, finishing the circulating acid washing after 7s, removing the filtrate from the circulating device, recovering residual residues on the screen mesh, and repeating for 8 times in this way to obtain filtrate, namely acid washing filtrate;
(2) adding sodium hydroxide into the acid-washing filtrate obtained in the step (1) to adjust the pH value of the filtrate to 5.8 to obtain neutralized filtrate, then adding potassium permanganate into the neutralized filtrate to remove iron, then adding cellulose to perform double decomposition reaction, filtering after the reaction is finished, evaporating a filter cake at 165 ℃, washing the filter cake with absolute ethyl alcohol, and performing water removal treatment at 230 ℃ for 26min per kilogram of filter cake to obtain an aluminum oxide whisker precursor; wherein the dosage of potassium permanganate is 0.54g/L and the dosage of cellulose is 130g/L on the basis of the volume of the neutralization filtrate;
(3) under vacuum degree of 4X 10-3Calcining step at the temperature of 980 ℃ under Pa(2) And obtaining the alumina whisker after 1.4 h.
Example 6
(1) Spreading blast furnace slag with the average particle size of 81 mu m on a screen mesh with the mesh size of 240 meshes at the speed of 235g/s, spreading the blast furnace slag with the thickness of 1.4mm, spraying a hydrochloric acid solution with the concentration of 9mol/L onto the surface of the blast furnace slag at the acid feeding speed of 150mL/s and the spraying speed of 58m/s, stopping spraying the acid and feeding after 27s, placing filtrate filtered by the screen mesh in a circulating device for circular acid washing, wherein the spraying amount of the filtrate is 220mL/s, the spraying speed of the filtrate is 73m/s, finishing the circular acid washing after 8s, removing the filtrate from the circulating device, recovering residual residues on the screen mesh, and repeating for 6 times in this way to obtain acid washing filtrate;
(2) adding sodium hydroxide into the acid-washing filtrate obtained in the step (1) to adjust the pH value of the filtrate to 5.9 to obtain neutralized filtrate, then adding potassium permanganate into the neutralized filtrate to remove iron, then adding cellulose to perform double decomposition reaction, filtering after the reaction is finished, evaporating a filter cake at 155 ℃, washing the filter cake with absolute ethyl alcohol, and performing water removal treatment at 230 ℃ for 26min per kilogram of filter cake to obtain an aluminum oxide whisker precursor; wherein the dosage of potassium permanganate is 0.62g/L and the dosage of cellulose is 135g/L on the basis of the volume of the neutralized filtrate;
(3) under vacuum degree of 4X 10-3And (3) calcining the precursor of the alumina whisker obtained in the step (2) at Pa and at 970 ℃, and obtaining the alumina whisker after 1.5 h.
Example 7
(1) Spreading blast furnace slag with the average particle size of 84 mu m on a screen mesh with the mesh size of 270 meshes at the speed of 245g/s, wherein the spreading thickness is 1.4mm, spraying hydrochloric acid solution with the concentration of 8mol/L onto the surface of the blast furnace slag at the acid feeding speed of 140mL/s and the spraying speed of 54m/s, stopping spraying acid and feeding after 28s, placing filtrate filtered by the screen mesh in a circulating device for circulating acid washing, wherein the spraying amount of the filtrate is 190mL/s, the spraying speed of the filtrate is 67m/s, finishing the circulating acid washing after 10s, removing the filtrate from the circulating device, recovering residual residues on the screen mesh, and repeating for 8 times in this way to obtain filtrate, namely acid washing filtrate;
(2) adding sodium hydroxide into the acid-washing filtrate obtained in the step (1) to adjust the pH value of the filtrate to 5.5 to obtain neutralized filtrate, then adding potassium permanganate into the neutralized filtrate to remove iron, then adding fructose to perform double decomposition reaction, filtering after the reaction is finished, evaporating a filter cake at 150 ℃, washing the filter cake with absolute ethyl alcohol, and performing water removal treatment at 210 ℃ for 23min per kilogram of filter cake to obtain an aluminum oxide whisker precursor; wherein the dosage of potassium permanganate is 0.64g/L and the dosage of fructose is 110g/L on the basis of the volume of the neutralization filtrate;
(3) under vacuum degree of 4X 10-3And (3) calcining the precursor of the alumina whisker obtained in the step (2) under the conditions of Pa and the temperature of 1020 ℃, and obtaining the alumina whisker after 1.7 h.
Example 8
(1) Firstly, spreading blast furnace slag with the average particle size of 80 mu m on a screen mesh with the mesh size of 245 meshes at the speed of 255g/s, wherein the spreading thickness is 1.4mm, simultaneously spraying hydrochloric acid solution with the concentration of 10mol/L onto the surface of the slag at the acid supply speed of 175mL/s and the spraying speed of 60m/s, stopping spraying acid and feeding after 23s, placing filtrate filtered by the screen mesh in a circulating device for circulating acid washing, wherein the spraying amount of the filtrate is 240mL/s, the spraying speed of the filtrate is 73m/s, finishing the circulating acid washing after 7s, removing the filtrate from the circulating device, recovering residual residues on the screen mesh, and repeating for 6 times to obtain the filtrate, namely acid washing filtrate;
(2) adding sodium hydroxide into the acid-washing filtrate obtained in the step (1) to adjust the pH value of the filtrate to 6 to obtain neutralized filtrate, then adding potassium permanganate into the neutralized filtrate to remove iron, then adding fructose to perform double decomposition reaction, filtering after the reaction is finished, evaporating a filter cake at 175 ℃, washing the filter cake with absolute ethyl alcohol, and then performing water removal treatment at 230 ℃ for 24min per kg of filter cake to obtain an aluminum oxide whisker precursor; wherein the dosage of potassium permanganate is 0.64g/L and the dosage of fructose is 110g/L on the basis of the volume of the neutralized filtrate;
(3) under vacuum degree of 4X 10-3Calcining the alumina obtained in the step (2) under the conditions of Pa and the temperature of 990 DEG CAnd (5) obtaining the alumina whisker after 1.9h of the whisker precursor.
TABLE 1 Properties of alumina whiskers prepared in examples 1 to 8
The embodiment shows that the alumina whisker prepared by the preparation method provided by the invention has the advantages of high hardness, high modulus and large length-diameter ratio, and the obtained alumina whisker has high purity and uniform size, the diameter of the alumina whisker is 280-392 nm, the radial dimension error of the alumina whisker is 18-23 nm, the length of the alumina whisker is 33-51 mu m, the length-diameter ratio of the alumina whisker is 86-176, the purity of an alumina phase is more than or equal to 98.4%, the elastic modulus of the alumina whisker is 385-397 GPa, and the room-temperature hardness of the alumina whisker is 71-75 GPa.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for preparing alumina whiskers by using blast furnace slag comprises the following steps:
(1) carrying out acid pickling on blast furnace slag to obtain acid pickling filtrate;
(2) adding a pH regulator into the acid washing filtrate obtained in the step (1) to obtain a neutralized filtrate;
(3) adding an iron remover into the neutralized filtrate obtained in the step (2) to remove iron, and then adding a carbon source to perform double decomposition reaction to obtain an alumina whisker precursor;
(4) and (4) calcining the alumina whisker precursor obtained in the step (3) under a vacuum condition to obtain the alumina whisker.
2. The method according to claim 1, wherein the pickling solution used in the pickling in the step (1) is a hydrochloric acid solution; the concentration of the hydrochloric acid solution is 8-10 mol/L.
3. The preparation method according to claim 1, wherein the pH value of the neutralized filtrate in the step (2) is 5.5 to 6.
4. The method according to claim 1, wherein the iron removing agent in the step (3) comprises potassium permanganate or potassium dichromate; and taking the volume of the neutralized filtrate as a reference, wherein the dosage of the iron removing agent is 0.45-0.64 g/L.
5. The method according to claim 1, wherein the carbon source in the step (3) comprises a monosaccharide or a polysaccharide; and taking the volume of the neutralized filtrate as a reference, wherein the dosage of the carbon source is 110-140 g/L.
6. The method according to claim 1, wherein the calcination in step (4) is carried out at 970-1020 ℃ under a vacuum degree of 4 x 10-3～6×10-3Pa。
7. The method according to claim 1, wherein the metathesis reaction in the step (3) is completed and then a post-treatment is further included; the post-treatment comprises filtration, evaporation, washing and water removal treatment which are sequentially carried out.
8. The preparation method according to claim 7, wherein the temperature of the evaporation is 150-175 ℃; the detergent used for washing is absolute ethyl alcohol; the temperature of the dewatering treatment is 210-230 ℃, and the dewatering treatment time is 23-26 min per kilogram of filter cake obtained by filtering.
9. Alumina whiskers produced by the production method according to any one of claims 1 to 8.
10. The alumina whisker according to claim 9, wherein the alumina whisker has a diameter of 280 to 392nm, a length of 33 to 51 μm, an aspect ratio of 86 to 176, a purity of an alumina phase of 98.4% or more, an elastic modulus of 385 to 397GPa, and a room-temperature hardness of 71 to 75 GPa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1489346A (en) * | 1974-03-18 | 1977-10-19 | Hepworth & Grandage Ltd | Production of a form of alumina whiskers |
| CN101974782A (en) * | 2010-11-19 | 2011-02-16 | 昆明理工大学 | Method of preparing alpha-Al2O3 crystal whisker by carbothermal reduction |
| CN106319627A (en) * | 2015-06-16 | 2017-01-11 | 北京交泰科技有限公司 | Alumina whisker preparation method |
| RU2732661C1 (en) * | 2019-12-10 | 2020-09-22 | Федеральное государственное бюджетное научное учреждение "Федеральный исследовательский центр "Красноярский научный центр Сибирского отделения Российской академии наук" (ФИЦ КНЦ СО РАН, КНЦ СО РАН) | METHOD OF PRODUCING POROUS WHISKERS α-Al2O3 USING LEAD-ZINC PRODUCTION WASTES |
-
2022
- 2022-04-02 CN CN202210350782.6A patent/CN114606571A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1489346A (en) * | 1974-03-18 | 1977-10-19 | Hepworth & Grandage Ltd | Production of a form of alumina whiskers |
| CN101974782A (en) * | 2010-11-19 | 2011-02-16 | 昆明理工大学 | Method of preparing alpha-Al2O3 crystal whisker by carbothermal reduction |
| CN106319627A (en) * | 2015-06-16 | 2017-01-11 | 北京交泰科技有限公司 | Alumina whisker preparation method |
| RU2732661C1 (en) * | 2019-12-10 | 2020-09-22 | Федеральное государственное бюджетное научное учреждение "Федеральный исследовательский центр "Красноярский научный центр Сибирского отделения Российской академии наук" (ФИЦ КНЦ СО РАН, КНЦ СО РАН) | METHOD OF PRODUCING POROUS WHISKERS α-Al2O3 USING LEAD-ZINC PRODUCTION WASTES |
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