CN111547751A - Method for preparing porous alumina by using solid waste - Google Patents
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- CN111547751A CN111547751A CN202010477392.6A CN202010477392A CN111547751A CN 111547751 A CN111547751 A CN 111547751A CN 202010477392 A CN202010477392 A CN 202010477392A CN 111547751 A CN111547751 A CN 111547751A
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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 50
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000002910 solid waste Substances 0.000 title claims abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 25
- 239000010902 straw Substances 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 23
- 239000000706 filtrate Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 21
- 239000002244 precipitate Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000002243 precursor Substances 0.000 abstract description 5
- 238000002386 leaching Methods 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002154 agricultural waste Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 20
- 239000011148 porous material Substances 0.000 description 15
- 239000000203 mixture Substances 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 8
- 240000008042 Zea mays Species 0.000 description 7
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 7
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 7
- 235000005822 corn Nutrition 0.000 description 7
- 238000004876 x-ray fluorescence Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000009766 low-temperature sintering Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting 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
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for preparing porous alumina by using solid waste, which comprises the following steps: washing the aluminum ash residue with water, filtering, drying the residue, leaching the residue with acid, purifying with alkali, filtering, adjusting pH of the filtrate with dilute acid to obtain Al (OH)3A precursor prepared from Al (OH)3The precursor is mixed with agricultural waste straw powder serving as a template, and porous alumina is prepared by roasting. Compared with the traditional preparation method of the porous alumina, the method provided by the invention has the advantages that industrial and agricultural solid wastes are fully utilized, the production cost is obviously reduced, the raw material source is wide, the environmental pollution is small, the process is simple, and the like.
Description
Technical Field
The invention relates to resource utilization of solid waste and preparation of a porous material, in particular to a method for preparing porous alumina by utilizing the solid waste.
Background
Alumino-ash is a solid waste generated during the production and recovery of electrolytic aluminum, cast aluminum, and other aluminum industries. The aluminum ash has more complex components, and the main components of the aluminum ash are aluminum oxide and ferric oxide (Al)2O3、Fe2O3) Silicon dioxide (SiO)2) Spinel (MgO. Al)2O3) And a small amount of meltable salt substances such as fluoride and chloride. At present, the mode of industrial treatment of aluminum ash is still stacking or landfill, which not only seriously damages the environment, but also causes a great deal of waste of aluminum resources. The crop straw is a huge and valuable biomass energy resource in an agricultural ecological systemThe source has great significance for promoting the income increase of farmers, protecting the environment, saving resources and sustainable development of agricultural economy. At present, most straws are still treated by incineration, which not only causes a great deal of waste of biomass energy resources, but also threatens the environment. Therefore, the aluminum ash and the crop straws are recycled, the problem of material shortage is solved, and the effects of protecting the environment and avoiding pollution can be achieved to a certain extent.
The porous alumina takes alumina as aggregate, and open-pore or closed-pore materials are formed inside the porous alumina through high-temperature sintering and molding processes. The porous alumina ceramic not only has the advantages of high temperature resistance and good corrosion resistance of the alumina ceramic, but also has the excellent characteristics of large specific surface area, low thermal conductivity and the like of porous materials, has selective permeability to liquid and gas media, is widely applied to the fields of aviation, surface corrosion prevention, catalysts and the like, and is also increasingly paid more attention to the application in the aspects of heat preservation and insulation, separation, sensors, filtering materials and the like. However, the alumina prepared by low-temperature sintering is easy to agglomerate, the specific surface area and the pore diameter of the product are reduced, and the performance of the alumina as a carrier is influenced.
Disclosure of Invention
The invention aims to provide a method for preparing porous alumina by using solid waste.
In order to achieve the purpose, the invention adopts the following technical scheme:
1) stirring and mixing the aluminum ash and water, filtering, and vacuum-drying the obtained filter residue;
2) adding excessive dilute acid (optional dilute sulfuric acid, dilute hydrochloric acid and the like) into the dried filter residue obtained in the step 1) so as to completely dissolve alumina in the aluminum ash, heating at constant temperature for a certain time, filtering after bubbles are not generated, and collecting filtrate;
3) adding excessive NaOH solution into the filtrate obtained in the step 2), filtering until precipitate is generated and the color of the precipitate is not changed any more, collecting the filtrate, then adjusting the pH value (the pH value is 7-9) of the filtrate with the dilute acid to generate white flocculent precipitate, and collecting the precipitate through filtering to obtain Al (OH)3；
4) Drying and crushing the straws to obtain straw powder, mixing the straw powder with the Al (OH) obtained in the step 3)3Mixing and stirring uniformly to obtain a raw material, wherein the mass fraction of straw powder in the raw material is less than or equal to 10%;
5) roasting the uniformly mixed raw materials in the step 4) at 500-900 ℃ for 2-4 h to obtain the porous alumina.
Preferably, in the step 1), the drying temperature is 80-120 ℃, and the drying time is 10-15 h.
Preferably, in the step 2), the adopted dilute acid is 1-1.8 mol/L dilute sulfuric acid, the heating temperature is 50-80 ℃, and the heating time is 0.5-5 h.
Preferably, in the step 3), the concentration of the NaOH solution is 5-8 mol/L, and the dilute acid is 1-1.8 mol/L dilute sulfuric acid.
Preferably, in the step 4), the particle size of the straw powder is 20-100 meshes, and the stirring time is 0.5-2 hours.
Preferably, in the step 5), the roasting conditions are as follows: preserving heat for 2-4 hours in a box type furnace at 700-900 ℃, and cooling to room temperature along with the furnace after preserving heat; the temperature rise rate of the box-type furnace is 5-10 ℃/min.
Preferably, the aluminum ash is selected from secondary aluminum ash of secondary aluminum.
The invention has the beneficial effects that:
the invention adopts industrial solid waste aluminum ash as raw material, the aluminum ash is washed, filtered and dried, the filter residue is leached by acid, purified by alkali and filtered, the pH value of the filtrate is adjusted by dilute acid, Al (OH) is obtained3Mixing Al (OH)3Mixing with straw powder as a template, and roasting to obtain the porous alumina. The porous alumina prepared by the method has high purity, large specific surface area and pore volume; the invention fully utilizes industrial and agricultural solid wastes, obviously reduces the production cost, has the advantages of wide raw material source, small environmental pollution, simple process and the like, and is suitable for industrial production.
Furthermore, the corn straw is an agricultural byproduct, contains a large amount of cellulose, hemicellulose and lignin, has a melting point of 700-800 ℃, is relatively consistent with the low-temperature sintering temperature of alumina, can be completely carbonized at the sintering temperature (700-900 ℃) and generates corresponding volatile hydrocarbon gas, ensures that the sintered product has porous characteristics, and avoids caking (for example, the reaction product is sintered at 500 ℃ and has a large loose blocky structure), thereby promoting the formation of high-purity porous alumina with a certain crystal form.
Drawings
FIG. 1 is a flow chart of the preparation of porous alumina using solid waste in the embodiment of the present invention.
FIG. 2 is an XRD pattern of the porous alumina prepared in example 1 of the present invention.
FIG. 3 is an SEM image of porous alumina prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. The examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
The invention provides a preparation method of a porous alumina product, which aims at solving the problems that aluminous ash (such as secondary aluminous ash of regenerated aluminum) and straws are difficult to treat and cause environmental pollution easily due to improper treatment and the problem that high-purity porous alumina is difficult to prepare (alumina prepared by low-temperature sintering is easy to agglomerate), and the preparation method utilizes the aluminous ash to purify aluminum hydroxide, simultaneously takes straw powder as a template and promotes the molding of a porous structure by mixing and roasting (see figure 1). Compared with the conventional preparation method of the porous alumina, the method has the advantages of low impurity content of the product, large specific surface area and pore volume and the like, and increases the way for efficiently utilizing agricultural and industrial waste resources.
Example 1
1. Washing and drying: adding sufficient deionized water into the aluminum ash, stirring, filtering, collecting filter residue, and drying the filter residue in a vacuum drying oven at 110 ℃ for 12 h;
2. acid leaching: weighing 20g of dried filter residue obtained in the step 1) by using an electronic balance, putting the filter residue into a beaker, introducing 1.6mol/L excess (550mL) of dilute sulfuric acid into the beaker through a glass rod, then putting the beaker into a constant-temperature water bath kettle for heating reaction at the heating temperature of 80 ℃ for 4 hours, filtering and collecting filtrate after bubbles are not generated, wherein the mass fraction of aluminum in the filtrate collected in the step is 70.7% according to the analysis result of an X-ray fluorescence spectrometer;
3. alkaline purification and pH value adjustment: to the filtrate obtained in step 2) was added an excess (550mL) of 5mol/L NaOH solution until a precipitate formed and the precipitate did not change in color. Filtering to collect filtrate, adjusting pH to 9 with 1.6mol/L dilute sulfuric acid to obtain white flocculent precipitate, filtering and collecting the white flocculent precipitate to obtain Al (OH) as precursor3According to the analysis result of an X-ray fluorescence spectrometer, the sum of the mass fractions of aluminum element and oxygen element in the white flocculent precipitate collected in the step is 99.4%;
4. mixing and stirring: drying corn straws (80-110 ℃), crushing, sieving with a 100-mesh sieve, and mixing with the Al (OH) obtained in the step 3)3Placing the mixture on a magnetic stirrer for mixing and stirring, wherein the content of the straws in the obtained mixture is 6 wt%, and the stirring time is 2 hours;
5. roasting: mixing the raw materials uniformly in the step 4 (namely the Al (OH)3The mixture of the powder and the sieved corn straw powder) is put into an alumina ceramic boat, the alumina ceramic boat is put into a high-temperature box type furnace (air atmosphere), the temperature rise rate is set to be 5 ℃/min, the heating temperature is 850 ℃, the temperature is kept for 2h, the furnace temperature is reduced to the room temperature at the speed of 10 ℃/min after the temperature keeping is finished, and the alumina ceramic boat is taken out to obtain a gray powder product;
6. the pore volume of the product was 0.34cm as determined by BET3Per g, specific surface area 261.22cm2In terms of/g, the mean pore diameter is 52.64 nm. The product was high purity gamma-alumina by X-ray diffraction analysis, containing few other impurities (see figure 2). The product was observed by scanning electron microscopy to be porous and to have a uniform distribution of pore sizes (see FIG. 3). The detection and analysis result shows that the product is high-purity porous alumina.
Example 2
1. Washing and drying: adding sufficient deionized water into the aluminum ash, stirring, filtering, collecting filter residue, and drying the filter residue in a vacuum drying oven at 80 ℃ for 10 h;
2. acid leaching: weighing 20g of dried filter residue obtained in the step 1) by using an electronic balance, putting the filter residue into a beaker, introducing excessive (550mL)1mol/L dilute sulfuric acid into the beaker through a glass rod, then putting the beaker into a constant-temperature water bath kettle for heating reaction at the heating temperature of 50 ℃ for 0.5h, filtering and collecting filtrate after bubbles are not generated any more, wherein the mass fraction of aluminum element in the filtrate collected in the step is 41.3% according to the analysis result of an X-ray fluorescence spectrometer;
3. alkaline purification and pH value adjustment: an excess (550mL) of 8mol/L NaOH solution was added to the filtrate from step 2) until a precipitate formed and no further change in color occurred. Filtering to collect filtrate, adjusting pH to 7 with 1mol/L dilute sulfuric acid to obtain white flocculent precipitate, filtering and collecting the white flocculent precipitate to obtain Al (OH) as precursor3According to the analysis result of an X-ray fluorescence spectrometer, the sum of the mass fractions of aluminum element and oxygen element in the white flocculent precipitate collected in the step is 78.5 percent;
4. mixing and stirring: drying corn straws (80-110 ℃), crushing, sieving with a 20-mesh sieve, and mixing with the Al (OH) obtained in the step 3)3Placing the mixture on a magnetic stirrer for mixing and stirring, wherein the content of the straws in the obtained mixture is 2 wt%, and the stirring time is 0.5 h;
5. roasting: mixing the raw materials uniformly in the step 4 (namely the Al (OH)3The mixture of the powder and the sieved corn straw powder) is put into an alumina ceramic boat, the alumina ceramic boat is put into a high-temperature box type furnace (air atmosphere), the temperature rise rate is set to be 8 ℃/min, the heating temperature is set to be 700 ℃, the temperature is kept for 2h, the furnace temperature is reduced to the room temperature at the speed of 10 ℃/min after the temperature keeping is finished, and the alumina ceramic boat is taken out to obtain a gray powder product;
6. the pore volume of the product was 0.22cm as shown by BET detection3Per g, specific surface area 80.06cm2In terms of/g, the mean pore diameter is 105.51 nm. By X-ray diffraction analysis, the main phase of the product is gamma-alumina and has trace amount of unknown impurities. The scanning electron microscope observes that the product is porous, namely the product is high-purity porous alumina.
Example 3
1. Washing and drying: adding sufficient deionized water into the aluminum ash, stirring, filtering, collecting filter residue, and drying the filter residue in a vacuum drying oven at 120 ℃ for 15 h;
2. acid leaching: weighing 20g of dried filter residue obtained in the step 1) by using an electronic balance, putting the filter residue into a beaker, introducing 1.8mol/L excess (550mL) of dilute sulfuric acid into the beaker through a glass rod, then putting the beaker into a constant-temperature water bath kettle for heating reaction at the heating temperature of 70 ℃ for 5 hours, filtering and collecting filtrate after bubbles are not generated, wherein the mass fraction of aluminum in the filtrate collected in the step is 69.5% according to the analysis result of an X-ray fluorescence spectrometer;
3. alkaline purification and pH value adjustment: an excess (550mL) of 8mol/L NaOH solution was added to the filtrate from step 2) until a precipitate formed and no further change in color occurred. Filtering to collect filtrate, adjusting pH to 9 with 1.8mol/L dilute sulfuric acid to obtain white flocculent precipitate, filtering and collecting the white flocculent precipitate to obtain Al (OH) as precursor3According to the analysis result of an X-ray fluorescence spectrometer, the sum of the mass fractions of aluminum and oxygen in the white flocculent precipitate collected in the step is 89.6 percent;
4. mixing and stirring: drying corn straws (80-110 ℃), crushing, sieving with a 50-mesh sieve, and mixing with the Al (OH) obtained in the step 3)3Placing the mixture on a magnetic stirrer for mixing and stirring, wherein the content of the straws in the obtained mixture is 10 wt%, and the stirring time is 2 hours;
5. roasting: mixing the raw materials uniformly in the step 4 (namely the Al (OH)3The mixture of the powder and the sieved corn straw powder) is put into an alumina ceramic boat, the alumina ceramic boat is put into a high-temperature box type furnace (air atmosphere), the temperature rise rate is 10 ℃/min, the heating temperature is 900 ℃, the temperature is kept for 2h, the furnace temperature is reduced to the room temperature at the speed of 10 ℃/min after the temperature keeping is finished, and the alumina ceramic boat is taken out to obtain a gray powder product;
6. the pore volume of the product was 0.18cm as determined by BET3Per g, specific surface area 176.92cm2In terms of/g, the mean pore diameter is 40.23 nm. By passingThe main phase of the product is gamma-alumina and has trace unknown impurities by X-ray diffraction analysis. The product is observed by a scanning electron microscope to be porous, the uniformity of the porous distribution is slightly worse than that of the product in the example 1, and the pore diameter is smaller. The detection and analysis result shows that the product is high-purity porous alumina.
Claims (7)
1. A method for preparing porous alumina by using solid waste is characterized by comprising the following steps: the method comprises the following steps:
1) stirring and mixing the aluminum ash and water, filtering, and vacuum drying the obtained filter residue;
2) adding dilute acid into the dried filter residue obtained in the step 1), then heating for a certain time at a constant temperature, filtering and collecting filtrate;
3) adding NaOH solution into the filtrate obtained in the step 2), filtering and collecting the filtrate until the precipitate is completely generated, then adjusting the pH value of the filtrate with dilute acid to generate white flocculent precipitate, and collecting the precipitate by filtering to obtain Al (OH)3；
4) Mixing the straw powder with the Al (OH) obtained in the step 3)3Mixing and stirring uniformly to obtain a raw material, wherein the mass fraction of straw powder in the raw material is less than or equal to 10%;
5) roasting the raw materials obtained in the step 4) at 500-900 ℃ for 2-4 h to obtain the porous alumina.
2. The method for preparing porous alumina by using solid waste, according to claim 1, is characterized in that: in the step 1), the drying temperature is 80-120 ℃, and the drying time is 10-15 h.
3. The method for preparing porous alumina by using solid waste, according to claim 1, is characterized in that: in the step 2), the adopted dilute acid is 1-1.8 mol/L dilute sulfuric acid, the heating temperature is 50-80 ℃, and the heating time is 0.5-5 h.
4. The method for preparing porous alumina by using solid waste, according to claim 1, is characterized in that: in the step 3), the concentration of the NaOH solution is 5-8 mol/L, and the dilute acid is 1-1.8 mol/L dilute sulfuric acid.
5. The method for preparing porous alumina by using solid waste, according to claim 1, is characterized in that: in the step 4), the particle size of the straw powder is 20-100 meshes, and the stirring time is 0.5-2 hours.
6. The method for preparing porous alumina by using solid waste, according to claim 1, is characterized in that: in the step 5), the roasting conditions are as follows: and (3) preserving the heat for 2-4 hours in a box type furnace at 700-900 ℃.
7. The method for preparing porous alumina by using solid waste, according to claim 1, is characterized in that: the aluminous ash is selected from secondary aluminous ash of secondary aluminium.
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| CN202010477392.6A CN111547751A (en) | 2020-05-29 | 2020-05-29 | Method for preparing porous alumina by using solid waste |
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| CN114032396A (en) * | 2021-11-09 | 2022-02-11 | 东北大学 | Method for treating aluminum ash by low-temperature harmless wet method |
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