CN118184386A - Complex-phase porous ceramic prepared from aluminum ash and method thereof - Google Patents
Complex-phase porous ceramic prepared from aluminum ash and method thereof Download PDFInfo
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- CN118184386A CN118184386A CN202410296993.5A CN202410296993A CN118184386A CN 118184386 A CN118184386 A CN 118184386A CN 202410296993 A CN202410296993 A CN 202410296993A CN 118184386 A CN118184386 A CN 118184386A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 134
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 34
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 30
- 239000011777 magnesium Substances 0.000 claims abstract description 30
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 30
- 239000010703 silicon Substances 0.000 claims abstract description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 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 claims abstract description 19
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 15
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 14
- 239000011029 spinel Substances 0.000 claims abstract description 14
- 238000011033 desalting Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002956 ash Substances 0.000 claims description 122
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 54
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 27
- 238000002386 leaching Methods 0.000 claims description 25
- 235000012245 magnesium oxide Nutrition 0.000 claims description 25
- 239000000377 silicon dioxide Substances 0.000 claims description 25
- 239000000395 magnesium oxide Substances 0.000 claims description 23
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000001095 magnesium carbonate Substances 0.000 claims description 7
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 7
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 7
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 7
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 241000537371 Fraxinus caroliniana Species 0.000 claims description 4
- 235000010891 Ptelea trifoliata Nutrition 0.000 claims description 4
- 238000010612 desalination reaction Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 239000013535 sea water Substances 0.000 claims description 4
- 239000002918 waste heat Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005273 aeration Methods 0.000 claims description 3
- 239000010881 fly ash Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 239000010431 corundum Substances 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 12
- 239000002910 solid waste Substances 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 231100001261 hazardous Toxicity 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 238000000748 compression moulding Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 12
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 9
- 239000007791 liquid phase Substances 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 8
- 238000004064 recycling Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000012774 insulation material Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HXELGNKCCDGMMN-UHFFFAOYSA-N [F].[Cl] Chemical compound [F].[Cl] HXELGNKCCDGMMN-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical class [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to the technical field of harmless treatment and resource utilization of hazardous solid wastes, in particular to a method for preparing complex-phase porous ceramic by utilizing aluminum ash. The method comprises the steps of firstly carrying out desalting treatment on aluminum ash, then mixing the aluminum ash with a silicon source and a magnesium source, and carrying out ball milling to obtain a mixture; dry-pressing the mixture to obtain a blank; sintering the blank to obtain the complex phase porous ceramic material. According to the preparation method provided by the invention, the aluminum ash, the silicon source and the magnesium source are directly mixed, the mixture is ball-milled and mixed by regulating and controlling the mass ratio of the desalted aluminum ash, silicon source and magnesium source, and the porous ceramic taking cordierite as a main phase and at least one of mullite and magnesia-alumina spinel as a complex phase can be obtained after compression molding and sintering. The method provided by the invention realizes harmless treatment and resource utilization of the aluminum ash.
Description
Technical Field
The invention relates to the technical field of harmless treatment and resource utilization of hazardous solid wastes, in particular to a method for preparing complex-phase porous ceramic by utilizing aluminum ash and a method thereof.
Background
Aluminum ash is a dangerous solid waste generated after aluminum is smelted, and because the aluminum ash contains aluminum nitride and fluorine chlorine salt, certain reactivity and leaching toxicity exist, and the code HW48 is dangerous to waste. At present, the treatment of the aluminum ash is mainly harmless treatment, and the method for recycling the aluminum ash is relatively deficient, so that the realization of recycling the aluminum ash is urgent.
The cordierite porous ceramic material has good thermal stability, high mechanical strength, large specific surface area and low thermal expansion coefficient, and is widely used as a refractory material and a catalyst carrier. The traditional cordierite material is mainly prepared by sintering alumina, magnesia and silica at high temperature, and pore-forming agents are additionally added to the cordierite porous ceramic to be fired, and the prepared cordierite porous ceramic has low strength and poor processability, so that the application of the cordierite porous ceramic is limited. The chemical composition of mullite is 3Al 2O3·2SiO2, the chemical composition of magnesia-alumina spinel is Al 2O3. MgO, and they have similar sintering temperatures. Alumina, magnesia and silica contained in the alumina ash can form mullite and magnesia-alumina spinel under certain reaction conditions. Mullite has a higher melting point, a lower coefficient of thermal expansion, good high temperature strength, thermal shock resistance and creep resistance; the magnesia-alumina spinel has good corrosion resistance, high melting point and good chemical stability, but has high expansion coefficient and weaker thermal shock resistance. Therefore, a plurality of porous ceramic materials which take cordierite as a main phase and at least one of mullite and magnesia-alumina spinel as a composite phase are prepared by adjusting the proportion and the reaction condition of the materials and become the direction of recycling the aluminum ash.
Disclosure of Invention
The invention aims to realize harmless treatment of aluminum ash, and utilizes valuable components such as alumina, magnesia, silica and the like in the aluminum ash to the greatest extent.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a method for preparing complex phase porous ceramics by utilizing aluminum ash, which comprises the following preparation steps:
Step 1) desalting the aluminum ash by adopting a low-temperature rapid leaching method or a low-temperature roasting method to obtain desalted aluminum ash;
low temperature rapid leaching method: placing the aluminum ash into a leaching kettle, leaching for 4-5 minutes with water temperature lower than 25 ℃ and water-ash ratio of 6:1, press-filtering, and drying to obtain desalted aluminum ash;
Low temperature roasting process: placing the aluminum ash into a high-temperature furnace, heating to 700 ℃ at 10 ℃/min, preserving heat for 6 hours, and cooling to room temperature along with the furnace to obtain desalted aluminum ash;
The total amount of K, na, cl and F in the desalted aluminum ash is less than or equal to 9% of the mass of the aluminum ash powder;
Step 2) mixing desalted aluminum ash, a silicon source and a magnesium source, and then performing ball milling to obtain a mixture;
step 3) dry-pressing the mixture to form a blank;
and 4) baking the green body to obtain the complex-phase porous ceramic material.
Preferably, the silicon source in the step 2) is a silicon-containing material or silicon dioxide; the silicon-containing material comprises silica, quartz or fly ash; the silicon dioxide content of the silicon-containing material is greater than 50%; the magnesium source comprises a magnesium-containing material or magnesium oxide; the magnesium-containing material comprises one or more of seawater magnesite and light burned magnesite; the magnesium oxide content of the magnesium-containing material is more than 70 percent.
Preferably, the particle size of the desalted aluminum ash slag powder particles in the step 2) is less than or equal to 75 mu m.
Preferably, the mass of the silicon source in the step 2) is calculated as mass converted into silicon dioxide, and the mass of the magnesium source is calculated as mass converted into magnesium oxide; the silicon source accounts for 40-100% of the desalted aluminum ash, and the magnesium source accounts for 5-20% of the desalted aluminum ash.
Preferably, in the step 2), corundum grinding balls are adopted for ball milling, the ball mass ratio is 1:1-5, the rotating speed of the ball mill is 100-500 r/min, the ball milling is alternately carried out by adopting forward/reverse rotation, the frequency is 10-50 min/time, and the ball milling time is 3-10 h.
Preferably, in the step 4), the blank is heated to a first temperature from room temperature and then to a second temperature, and the heat is preserved to obtain a sintered body; cooling the sintered body to room temperature to obtain a complex-phase porous ceramic material; ventilation is needed to keep air flowing in the roasting process; the aeration rate was 0.2L/min.
Preferably, the temperature rising rate of the first temperature is 10 ℃/min, the first temperature is 700 ℃, the temperature rising rate of the second temperature is 5 ℃/min, the second temperature is 1250 ℃, and the heat preservation time is 2h.
Preferably, step 1) uses the waste heat after roasting to carry out low-temperature desalination or to dry the material after low-temperature rapid leaching.
The invention also provides the complex-phase porous ceramic, which takes cordierite as a main phase and at least one of mullite and magnesia-alumina spinel as a complex phase.
Compared with the prior art, the invention has the following beneficial effects:
Firstly, aluminum ash is composed of oxides of aluminum, silicon and magnesium, aluminum nitride and salt, and the traditional aluminum ash treatment method is to prepare high-alumina materials, only uses alumina components in the high-alumina materials, and does not completely realize the recycling of the aluminum ash; the main component of cordierite is 2MgO.2Al 2O3·5SiO2, and the component for preparing the ceramic taking cordierite as a main phase is obtained by adding a silicon source and a magnesium source while removing salt and aluminum nitride in aluminum ash, so that aluminum, magnesium, silicon oxides and aluminum nitride in the aluminum ash are utilized to the greatest extent, and harmless treatment and recycling of the aluminum ash are realized.
Secondly, the desalted aluminum ash is mixed with a silicon source and a magnesium source, and the mixture is ball-milled, mixed, pressed and formed and then baked to obtain porous ceramic taking cordierite as a main phase and at least one of mullite and magnesia-alumina spinel as a complex phase by regulating and controlling the mass ratio of the aluminum ash to the silicon source and the magnesium source. Aluminum nitride in the aluminum ash is oxidized to generate aluminum oxide and nitrogen under the condition of 700-1300 ℃ oxygen, so that the pore-forming effect can be achieved, no pore-forming agent is required to be added, the cost for preparing the complex-phase porous ceramic is reduced, the processing steps of the aluminum ash are simplified, and the harmless treatment and the recycling of the aluminum ash are realized.
Third, the traditional aluminum ash is not desalted in the pyrogenic process, when the salt content in the aluminum ash is higher, the melting point of the aluminum ash is obviously reduced, so that a large amount of liquid phases (figures 6 and 7) are generated in the roasting process, and the product (figure 5) and equipment are greatly influenced.
Fourth, the invention can use the waste heat to carry out low-temperature desalination or dry the material which is leached out at low temperature rapidly, thus playing the roles of energy conservation and emission reduction.
Fifth, the complex phase porous ceramic material prepared by the invention can be used as catalyst carriers, heat insulation materials, sound insulation materials and the like, and is more beneficial to the resource utilization of aluminum ash.
Drawings
FIG. 1 shows the morphology of green bodies before and after baking in comparative example 1 of the present invention;
FIG. 2 is a microstructure of a cordierite/mullite porous ceramic prepared in example 1 of the invention;
FIG. 3 is a microstructure of a cordierite/magnesia-alumina spinel porous ceramic prepared in example 2 of the present invention;
FIG. 4 is an industrial CT photograph of cordierite/mullite porous ceramic prepared in example 3 of the present invention;
FIG. 5 is a macroscopic structure diagram of the complex phase porous ceramics prepared in example 1 (left) and comparative example 2 (right) of the present invention;
FIG. 6 is a graph showing the change of the liquid phase amount of the material in the baking process of the high salt aluminum ash (1) in comparative example 2 according to the present invention with the change of temperature;
FIG. 7 is a graph showing the variation of the liquid phase amount of the low-salt aluminum ash in comparative example 3 according to the temperature.
FIG. 8 is an XRD pattern of the cordierite composite porous ceramics prepared in example 1 and example 2 according to the present invention.
Detailed Description
The invention provides a method for preparing complex phase porous ceramics by utilizing aluminum ash, which comprises the following preparation steps:
Step 1) desalting the aluminum ash by adopting a low-temperature rapid leaching method or a low-temperature roasting method to obtain desalted aluminum ash;
low temperature rapid leaching method: placing the aluminum ash into a leaching kettle, leaching for 4-5 minutes with water temperature lower than 25 ℃ and water-ash ratio of 6:1, press-filtering, and drying to obtain desalted aluminum ash;
Low temperature roasting process: placing the aluminum ash into a high-temperature furnace, heating to 700 ℃ at 10 ℃/min, preserving heat for 6 hours, and cooling to room temperature along with the furnace to obtain desalted aluminum ash;
The total amount of K, na, cl and F in the desalted aluminum ash is less than or equal to 9% of the mass of the aluminum ash powder;
Step 2) mixing desalted aluminum ash, a silicon source and a magnesium source, and then performing ball milling to obtain a mixture;
step 3) dry-pressing the mixture to form a blank;
and 4) baking the green body to obtain the complex-phase porous ceramic material.
In the invention, the specific operation steps of the step 1) are as follows: firstly, detecting chemical components of aluminum ash, and directly performing the step 2) when the total amount of K, na, cl and F in the aluminum ash is less than or equal to 9% of the mass of the aluminum ash powder; if the total amount of K, na, cl and F in the aluminum ash is more than 9% of the mass of the aluminum ash powder, desalting treatment by a rapid leaching method or a low-temperature roasting method is needed.
In the present invention, the silicon source in step 2) is a silicon-containing material or silicon dioxide, preferably silicon dioxide; the siliceous material comprises silica, quartz or fly ash, preferably silica or quartz, further preferably silica; the silicon-containing material has a silicon dioxide content of greater than 50%, preferably greater than 55%, further preferably greater than 60%;
The magnesium source comprises a magnesium-containing material or magnesium oxide, preferably magnesium oxide; the magnesium-containing material comprises one or more of seawater magnesite and light burned magnesite, preferably seawater magnesite; the magnesium oxide content of the magnesium-containing material is more than 70%, more preferably more than 80%, still more preferably more than 90%.
In the present invention, the particle diameter of the desalted aluminum ash powder particles in the step 2) is 75 μm or less (200 mesh sieve), preferably 63 μm or less, more preferably 53 μm or less, still more preferably 47 μm or less.
In the present invention, the mass of the silicon source in the step 2) is calculated as the mass converted into silicon dioxide, and the mass of the magnesium source is calculated as the mass converted into magnesium oxide;
The silicon source accounts for 40-100%, preferably 45-90%, more preferably 50-80%, still more preferably 60-70% of the mass of the desalted aluminum ash; the magnesium source accounts for 5 to 20 percent, preferably 6 to 15 percent, more preferably 7 to 12 percent, even more preferably 8 to 10 percent of the mass of the desalted aluminum ash.
In the invention, corundum-alumina grinding balls are adopted for ball milling in the step 2), and the mass ratio of the balls is 1:1-5, preferably 1:2-4, and more preferably 1:3; the rotation speed of the ball mill is 100-500 rpm, preferably 150-450 rpm, more preferably 200-400 rpm, still more preferably 250-350 rpm; ball milling is carried out alternately by adopting forward and reverse rotation, wherein the frequency is 10-50 min/time, preferably 15-45 min/time, more preferably 20-40 min/time, still more preferably 25-35 min/time; the ball milling time is 3 to 10 hours, preferably 4 to 9 hours, more preferably 5 to 8 hours, still more preferably 6 to 7 hours.
In the present invention, after the mixture is obtained, before the calcination, the method further comprises: dry-pressing the mixture to obtain a blank; and drying the blank body and roasting to obtain the complex-phase porous ceramic. The invention carries out dry pressing molding on the mixture before the roasting, which is beneficial to obtaining the compact-structure complex-phase porous ceramic molded body through one-step roasting.
In the present invention, the pressure of the dry press molding in the step 3) is 5 to 200MPa, preferably 20 to 180MPa, more preferably 50 to 150MPa, still more preferably 80 to 120MPa; the time is 1 to 360 minutes, preferably 10 to 300 minutes, more preferably 100 to 250 minutes, still more preferably 150 to 200 minutes.
In the invention, in the step 4), the green body is heated to a first temperature from room temperature and then to a second temperature, and the heat preservation is carried out to obtain a sintered body; cooling the sintered body to room temperature to obtain a complex-phase porous ceramic material; ventilation is needed to keep air flowing in the roasting process; the aeration rate was 0.2L/min.
In the invention, the temperature rising rate of the first temperature is 10 ℃/min, the first temperature is 700 ℃, the temperature rising rate of the second temperature is5 ℃/min, the second temperature is 1250 ℃, and the heat preservation time is 2h. In the invention, step 1) uses the waste heat after roasting to carry out low-temperature desalination or dry the material after low-temperature rapid leaching.
The invention also provides the complex phase porous ceramic, which takes cordierite as a main phase and at least one of mullite and magnesia-alumina spinel as a complex phase.
In the present invention, cordierite porous ceramic materials may be used as catalyst carriers; the cordierite/mullite complex-phase porous ceramic can be used as a filter plate of a metal melt; the cordierite/magnesia-alumina spinel composite porous ceramic material can be used as a light heat insulation material.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Preparation example 1
The chemical composition of the aluminum ash is detected, the total amount of K, na, cl and F in the aluminum ash is less than or equal to 9% of the mass of the aluminum ash powder, the aluminum ash is marked as low-salt aluminum ash, the powder composition of the low-salt aluminum ash is shown in table 1, and the aluminum nitride content of the low-salt aluminum ash powder is shown in table 2.
Preparation example 2
Desalting the high-salt aluminum ash (1) by a low-temperature rapid leaching method: placing the aluminum ash into a leaching kettle, leaching for 4-5 minutes with water-ash ratio of 6:1 at water temperature lower than 25 ℃, and press-filtering and drying to obtain fast leached desalted aluminum ash (1);
The compositions of the high salt aluminum ash (1) and the flash leaching desalted aluminum ash (1) are shown in Table 1, and the aluminum nitride contents are shown in Table 2.
Preparation example 3
Desalting the high-salt aluminum ash (2) by a low-temperature roasting method: placing the aluminum ash into a high-temperature furnace, heating to 700 ℃ at 10 ℃/min, preserving heat for 6 hours, and cooling to room temperature along with the furnace to obtain roasting desalted aluminum ash (2);
The compositions of the high-salt aluminum ash (2) and the calcined desalted aluminum ash (2) are shown in Table 1, and the aluminum nitride contents are shown in Table 2.
TABLE 1 composition of aluminum ash powder (in mass% based on oxide)
TABLE 2 aluminium nitride content of aluminium ash powder (mass percent)
| Total nitrogen content/% | Converted into aluminum nitride content/% | |
| Low-salt aluminum ash | 3.2745 | 9.586 |
| High salt aluminum ash (1) | 2.2531 | 6.592 |
| Rapid leaching desalted aluminum ash (1) | 2.1608 | 6.322 |
| High-salt aluminum ash (2) | 2.6165 | 7.655 |
| Roasting desalted aluminum ash (2) | 0.2420 | 0.708 |
Example 1
(1) And (3) batching: according to the mass of aluminum, silicon and magnesium oxides contained in the fast leaching desalted aluminum ash (1) and the proportion of each component in the molecular formulas of cordierite and mullite (2MgO.2Al 2O3·5SiO2 and 3Al 2O3·2SiO2), the ingredients are mixed according to the theoretical cordierite/mullite molar mass ratio of 9:1, the analytically pure magnesium oxide accounts for 7.2% of the mass of the aluminum ash, and the silicon dioxide accounts for 42.2% of the mass of the aluminum ash.
(2) Mixing powder: ball milling is carried out on the proportioned raw materials, the ball mass ratio is 1:2, the rotating speed of the ball mill is 300 revolutions per minute, ball milling is carried out alternately by adopting forward rotation and reverse rotation, the time interval between the forward rotation and the reverse rotation is 15 minutes, the ball milling time is 6 hours, and absolute ethyl alcohol with the mass ratio of 1:1 with the raw materials is added and mixed uniformly.
(3) Compacting: and (3) forming by adopting a dry pressing method, wherein the forming pressure is 30MPa, the diameter of a sample is 26mm, and the height of the sample is 12mm, so as to obtain a blank.
(4) And (3) drying: the green body is put into a drying box and dried for 8 hours at 75 ℃.
(5) Sintering: sintering the green body in a high-temperature furnace under the condition of: heating the high-temperature furnace to 700 ℃ at a speed of 10 ℃/min; and then heating to 1250 ℃ at 5 ℃/min, preserving heat for 2 hours, and cooling to room temperature along with a furnace to obtain the cordierite/mullite composite porous ceramic material.
FIG. 2 is a microstructure of the composite porous ceramic, and the composite porous ceramic is successfully prepared by sintering at 1250 ℃ for 2 hours, wherein a large number of acicular mullite phases exist in holes of a sample and are mutually interweaved and attached on a matrix cordierite phase.
Example 2
The difference from example 1 is that: according to the mass of aluminum, silicon and magnesium oxides contained in the fast leaching desalted aluminum ash (1) and the proportion of each component in the molecular formulas (2MgO.2Al 2O3·5SiO2 and Al 2O3.MgO) of cordierite and magnesia-alumina spinel, the ingredients are prepared according to the theoretical cordierite/spinel generation molar ratio of 9:1, the analytically pure magnesia accounts for 8.6 percent of the mass of the aluminum ash, and the silicon dioxide accounts for 42.7 percent of the mass of the aluminum ash.
FIG. 3 is a microstructure of the composite porous ceramic, in which a large number of octahedral magnesia-alumina spinel phases and bulk cordierite precipitated phases are adhered to a cordierite matrix, and the composite porous material is prepared by sintering at 1250 ℃ for 2 hours.
Example 3
The difference from example 1 is that the calcined desalted aluminum ash (2), analytically pure magnesium oxide, and silica were dosed at a theoretical cordierite/mullite molar mass ratio of 9:1, with analytically pure magnesium oxide accounting for 12.1% of the aluminum ash mass and silica accounting for 47.3% of the aluminum ash mass.
FIG. 4 is an industrial CT photograph of the cordierite/mullite porous ceramic prepared in example 3.
Comparative example 1
The only difference from example 1 is that: the proportions of the components are calculated according to the mass of oxides containing aluminum, silicon and magnesium in the fast leaching desalted aluminum ash (1) and the cordierite molecular formula 2MgO.2Al 2O3·5SiO2, the ingredients are prepared according to the theoretical cordierite component, the analytically pure magnesium oxide accounts for 8.4% of the mass of the aluminum ash, and the silicon dioxide accounts for 43.9% of the mass of the aluminum ash.
Comparative example 2
The difference from example 1 is that the high-salt aluminum ash (1) was not desalted.
FIG. 5 shows the effect of desalting on the structural properties of cordierite porous ceramic, and FIG. 5 shows the porous ceramic material obtained by sintering the desalted aluminum chloride slag in example 2, which has a stable shape and a uniform pore distribution, and FIG. 5 shows the ceramic material obtained by sintering the undesalted aluminum chloride slag in comparative example 1, which has an unstable shape and coarse pore size. FIG. 6 is a graph showing the variation of the liquid phase amount of the high-salt aluminum ash (1) in comparative example 2 with the variation of temperature. With the increase of the roasting temperature, the total amount of liquid phase components of NaF, naCl, KF, KCl and other molten salts is sharply increased after the temperature is higher than 600 ℃, so that a large amount of liquid phase is generated in the sintering process, and the sintering of the complex phase porous ceramic is failed, as shown in figure 6.
Comparative example 3
The difference from example 1 is that low-salt aluminum ash, analytically pure magnesium oxide, and silica were dosed at a theoretical cordierite/mullite molar mass ratio of 9:1, the analytically pure magnesium oxide accounting for 8.7% of the mass of the aluminum ash, the silica accounting for 43.3% of the mass of the aluminum ash, and a high-temperature furnace was warmed to 700 ℃ at 10 ℃/min, and incubated for 6 hours.
FIG. 7 is a graph showing the variation of the liquid phase amount of the low-salt aluminum ash in comparative example 3 with the variation of temperature. As the roasting temperature increases, the total amount of liquid phase components of NaF, naCl, KF, KCl and other molten salts is sharply increased after the temperature is higher than 700 ℃, so that the heat preservation at 700 ℃ can be effectively desalted, as shown in figure 7.
TABLE 3 Properties of porous ceramics prepared from aluminum ash
| Bulk Density/g/ml | Porosity/% | Compressive Strength/MPa | |
| Example 1 | 0.7714 | 68.32 | 12 |
| Example 2 | 0.8509 | 63.25 | 8 |
| Example 3 | 1.0770 | 59.26 | 10 |
| Comparative example 1 | 1.4036 | 45.46 | 2.8 |
| Comparative example 3 | 1.3254 | 50.78 | 9 |
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
1. The method for preparing the complex-phase porous ceramic by using the aluminum ash is characterized by comprising the following preparation steps:
Step 1) desalting the aluminum ash by adopting a low-temperature rapid leaching method or a low-temperature roasting method to obtain desalted aluminum ash;
low temperature rapid leaching method: placing the aluminum ash into a leaching kettle, leaching for 4-5 minutes with water temperature lower than 25 ℃ and water-ash ratio of 6:1, press-filtering, and drying to obtain desalted aluminum ash;
Low temperature roasting process: placing the aluminum ash into a high-temperature furnace, heating to 700 ℃ at 10 ℃/min, preserving heat for 6 hours, and cooling to room temperature along with the furnace to obtain desalted aluminum ash;
The total amount of K, na, cl and F in the desalted aluminum ash is less than or equal to 9% of the mass of the aluminum ash powder;
Step 2) mixing desalted aluminum ash, a silicon source and a magnesium source, and then performing ball milling to obtain a mixture;
step 3) dry-pressing the mixture to form a blank;
and 4) baking the green body to obtain the complex-phase porous ceramic material.
2. The method for preparing complex phase porous ceramic by using aluminum ash according to claim 1, wherein the silicon source in the step 2) is silicon-containing material or silicon dioxide; the silicon-containing material comprises silica, quartz or fly ash; the silicon dioxide content of the silicon-containing material is greater than 50%; the magnesium source comprises a magnesium-containing material or magnesium oxide; the magnesium-containing material comprises one or more of seawater magnesite and light burned magnesite; the magnesium oxide content of the magnesium-containing material is more than 70 percent.
3. The method for preparing complex phase porous ceramics by utilizing aluminum ash according to claim 2, wherein the particle size of the desalted aluminum ash powder particles in the step 2) is less than or equal to 75 μm.
4. The method for preparing complex phase porous ceramic by using aluminum ash according to claim 1, wherein the mass of the silicon source in the step 2) is calculated as mass converted into silicon dioxide, and the mass of the magnesium source is calculated as mass converted into magnesium oxide; the silicon source accounts for 40-100% of the desalted aluminum ash, and the magnesium source accounts for 5-20% of the desalted aluminum ash.
5. The method for preparing complex phase porous ceramic by using aluminum ash as claimed in claim 4, wherein in the step 2), corundum grinding balls are adopted for ball milling, the ball mass ratio is 1:1-5, the rotation speed of the ball mill is 100-500 rpm, the ball milling is alternately carried out by adopting forward/reverse rotation, the frequency is 10-50 min/time, and the ball milling time is 3-10 h.
6. The method for preparing complex phase porous ceramic by using aluminum ash as claimed in claim 1, wherein the firing in the step 4) is to heat up the green body from room temperature to a first temperature and then to a second temperature, and then to heat up the green body to obtain a sintered body; cooling the sintered body to room temperature to obtain a complex-phase porous ceramic material; ventilation is needed to keep air flowing in the roasting process; the aeration rate was 0.2L/min.
7. The method for preparing complex phase porous ceramic from aluminum ash according to claim 6, wherein the temperature rising rate of the first temperature is 10 ℃/min, the first temperature is 700 ℃, the temperature rising rate of the second temperature is 5 ℃/min, the second temperature is 1250 ℃, and the heat preservation time is 2h.
8. The method for preparing complex phase porous ceramics by using aluminum ash according to claim 1, wherein step 1) uses waste heat after roasting to carry out low temperature desalination or to dry the material after low temperature rapid leaching.
9. A composite porous ceramic according to any one of claims 1 to 8, wherein the composite porous ceramic comprises cordierite as a main phase and at least one of mullite and magnesia alumina spinel as a composite phase.
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