CN114506850A - Method for preparing aminated mesoporous silica material by using high-alumina fly ash - Google Patents
Method for preparing aminated mesoporous silica material by using high-alumina fly ash Download PDFInfo
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- CN114506850A CN114506850A CN202210321763.0A CN202210321763A CN114506850A CN 114506850 A CN114506850 A CN 114506850A CN 202210321763 A CN202210321763 A CN 202210321763A CN 114506850 A CN114506850 A CN 114506850A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 54
- 239000010881 fly ash Substances 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 47
- 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 42
- 238000000034 method Methods 0.000 title description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002386 leaching Methods 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000005576 amination reaction Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 238000001816 cooling Methods 0.000 claims description 30
- 238000005406 washing Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 230000003213 activating effect Effects 0.000 claims description 7
- 239000002736 nonionic surfactant Substances 0.000 claims description 7
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- -1 polyethylene Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920000428 triblock copolymer Polymers 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 230000004913 activation Effects 0.000 abstract 1
- 238000007792 addition Methods 0.000 abstract 1
- 238000010979 pH adjustment Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000005211 surface analysis Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 239000003245 coal Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000003828 vacuum filtration Methods 0.000 description 4
- 238000002329 infrared spectrum Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000013335 mesoporous material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 241001428800 Cell fusing agent virus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 208000036971 interstitial lung disease 2 Diseases 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- 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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
-
- 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
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for producing an aminated mesoporous silica material by using high-alumina fly ash, which comprises the steps of high-alumina fly ash activation, acid leaching, alkaline leaching, template agent addition, pH adjustment, high-temperature calcination and the like to prepare the mesoporous silica material, wherein the mesoporous silica material has the characteristics of high specific surface area, controllable aperture, narrow aperture distribution and the like, so that the application range of the silica material in many chemical fields is expanded; adding ethanol and an amination agent into the prepared mesoporous silica material to prepare an aminated mesoporous silica material; the mesoporous silica material is successfully prepared by using the high-alumina fly ash and is successfully aminated, so that a new direction is provided for resource utilization of the high-alumina fly ash.
Description
Technical Field
The invention relates to the technical field of preparation of aminated mesoporous silica, and particularly relates to a method for producing an aminated mesoporous silica material by using high-alumina fly ash.
Background
Fly ash is a byproduct of coal combustion in thermal power plants and is one of the most complex and abundant materials for human activities. It is estimated that in a coal fired power plant, 1 ton of fly ash is produced per 2 tons of coal fired. Whereas thermal power plants worldwide generate more than 8 million tons of fly ash from coal combustion each year. Currently, fly ash is stored in landfills, single landfills (landfills where only CFAs are placed) and ponds, or is disposed of by simple stacking. However, these treatment methods cause water and soil pollution, cause ecological damage and environmental damage, and therefore must be disposed of or recycled.
The mesoporous material has the characteristics of large specific surface area, large porosity, strong mechanical stability and continuous modulation of application performance along with structure control, so that the mesoporous material has wide application prospect in the separation field. The selective adsorption system constructed by introducing specific functional components is an important research direction of the mesoporous silicon material in the field of heavy metal wastewater treatment. Because the highly ordered mesoporous silica has the advantages of regular pore structure and the like, the highly ordered mesoporous silica has great potential application value in the aspects of macromolecule catalysis, adsorption separation, chemical assembly preparation of advanced functional materials, optical devices and the like. However, most of the currently synthesized aminated mesoporous silica materials use organic silicon sources, which are expensive and toxic, thereby restricting large-scale production. Therefore, the development of aminated silica with a low silicon source is one of the problems to be solved in practical production applications.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the method for preparing the aminated mesoporous silica material adsorbent with low cost and low energy consumption by using the high-alumina fly ash as the raw material.
The method for producing the aminated mesoporous silica material by using the high-alumina fly ash comprises the following steps:
(1) activating the high-alumina fly ash: mixing the high-alumina fly ash and an activating agent, roasting at the temperature of 700-900 ℃ for 60-180min, cooling to room temperature after roasting is finished, and grinding into uniform powder to obtain activated high-alumina fly ash;
the activating agent is sodium carbonate, and the mass ratio of the high-alumina fly ash to the activating agent is 1: 0.5-2;
(2) acid leaching: mixing the activated high-alumina fly ash obtained in the step (1) with 3-6mol/L of leaching agent, stirring the mixture in a water bath at 40-90 ℃ for 2-6 hours, cooling the mixture to room temperature, washing the mixture with distilled water, carrying out vacuum filtration, collecting filter residue, drying the filter residue at 90 ℃, and grinding the filter residue into fine powder;
the leaching agent is a nitric acid solution, and the solid-liquid ratio g of the activated fly ash to the leaching agent is mL =1: 5-20;
(3) alkaline leaching: mixing the filter residue ground in the step (2) with 5-10mol/L of leaching solution, stirring in water bath at 40-90 ℃ for 12-48h, cooling to room temperature, washing with distilled water, vacuum filtering, and collecting filtrate;
the leachate is a sodium hydroxide solution, and the solid-to-liquid ratio g of the ground filter residue to the leachate is mL =1: 5-20;
(4) adding a template agent: mixing a nonionic surfactant with the filtrate obtained in the step (3) by using the nonionic surfactant as a template agent, and stirring in a water bath at 40-90 ℃ until the solution is clear;
the nonionic surfactant is a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123), and the solid-to-liquid ratio g: mL of the nonionic surfactant to the filtrate is 1: 80-120.
(5) Adjusting the pH value: dropwise adding 5-10mol/L acid solution into the solution in the step (4) under stirring of water bath at 40-90 ℃, adjusting the pH to 0-1, stopping stirring, standing and aging for 24-48h, cooling to room temperature, washing with distilled water, vacuum filtering, collecting filter residue, drying the filter residue at 90 ℃, and grinding into fine powder;
the acid solution is hydrochloric acid solution;
(6) high-temperature calcination: placing the filter residue ground in the step (5) in a muffle furnace, heating to 500-600 ℃ at the heating rate of 1 ℃/min, preserving the heat for 4-6h, and cooling to room temperature at the cooling rate of 1 ℃/min to obtain the mesoporous silica material;
(7) and (4) adding ethanol and an amination agent into the mesoporous silica material obtained in the step (6), performing ultrasonic treatment for 10-60min, performing centrifugal washing, taking a solid precipitate, and drying at 60 ℃ to obtain the aminated mesoporous silica material.
The ethanol is absolute ethanol, the amination agent is Aminopropyltriethoxysilane (APTES), the mass volume ratio g: mL of the mesoporous silica material to the amination agent is 1-5:1-2, the ultrasonic power is 5kHz, the temperature is 25 ℃, and the centrifugal washing is repeated centrifugal washing by using ethanol.
The method has the advantages and the technical effects that:
the raw materials used by the invention are high-alumina fly ash solid wastes, so that the production cost is low; the production process does not need an impurity removal process; the mesoporous silica prepared by the method has high specific surface area and ordered pore diameter, and the aminated mesoporous silica material has good application prospect in the aspect of sulfur dioxide adsorption.
Drawings
FIG. 1 is a graph showing a pore size distribution (A) and a nitrogen adsorption/desorption curve (B) of mesoporous silica and aminated mesoporous material in example 1;
FIG. 2 is a Fourier infrared spectrum of mesoporous silica and aminated mesoporous silica of example 1.
Detailed Description
The present invention is further illustrated by the following examples, without limiting the scope of the invention thereto; the high-alumina fly ash used in the following examples was derived from a thermal power plant of inner Mongolia, and the chemical composition and the main phase composition thereof are shown in Table 1;
TABLE 1 high-alumina fly ash ingredient table
Example 1:
1. uniformly mixing 10g of high-alumina fly ash and 5g of sodium carbonate according to the mass ratio of 1:0.5 of the high-alumina fly ash to the activator, roasting at 750 ℃ for 150min, cooling to room temperature after roasting is finished, and grinding into uniform powder to obtain activated high-alumina fly ash;
2. according to the solid-liquid ratio g: mL =1:5 of activated high-alumina fly ash and leaching agent, 10g of activated high-alumina fly ash and 50mL of HNO3(4 mol/L) mixing the components,stirring in water bath at 80 deg.C for 4 hr, cooling to room temperature, washing with distilled water, vacuum filtering, collecting residue, oven drying at 90 deg.C, and grinding into fine powder;
3. weighing 10g of ground filter residue and a sodium hydroxide solution (5 mol/L) according to the solid-to-liquid ratio g: mL =1:5 of the ground filter residue to the leachate, mixing the mixture at 80 ℃ in a water bath for 12 hours, cooling to room temperature, washing with distilled water, carrying out vacuum filtration, and collecting filtrate;
4. weighing 3g P123 according to the solid-liquid ratio g: mL of the P123 to the filtrate being 1:100, mixing with the filtrate, and stirring in a water bath at 40 ℃ until the solution is clear;
5. dropwise pumping 5mol/L hydrochloric acid solution into the solution in the step 4 under the water bath stirring at 40 ℃, adjusting the pH value to 0, stopping stirring, standing and aging for 24 hours, cooling to room temperature, washing with distilled water, vacuum filtering, collecting filter residues, drying the filter residues at 90 ℃, and grinding into fine powder;
6. placing the ground filter residue in a muffle furnace, heating to 500 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 6h, and then cooling to room temperature at the cooling rate of 1 ℃/min to obtain the mesoporous silica material; the specific surface area of the mesoporous silica material obtained by the determination of a full-automatic BET specific surface analysis tester is 513.216m2The pore diameter distribution diagram and the nitrogen absorption and desorption curve of the mesoporous silica material are shown in figure 1, and the Fourier infrared spectrum is shown in figure 2;
7. weighing 0.5g of mesoporous silica material, adding 100mL of absolute ethanol and 0.1mL of aminopropyltriethoxysilane, carrying out ultrasonic treatment at 25 ℃ and 5kHz for 10min, carrying out centrifugal washing with ethanol at 1000r for 3min, carrying out centrifugal washing for 5 times, and drying solid precipitate at 60 ℃ for 12h to obtain an aminated mesoporous silica material; the specific surface area of the aminated mesoporous silica material is 415.103m by the measurement of a full-automatic BET specific surface analysis tester2The/g shows that the pore diameter distribution diagram and the nitrogen adsorption and desorption curve of the aminated mesoporous silica material are shown in figure 1, the Fourier infrared spectrum is shown in figure 2, and the aminated mesoporous silica can be seen to have an ammonium peak, which indicates that the amination is successful.
Example 2:
1. uniformly mixing 10g of high-alumina fly ash and 10g of sodium carbonate according to the mass ratio of 1:1, roasting at 800 ℃ for 90min, cooling to room temperature after roasting is finished, and grinding into uniform powder to obtain activated high-alumina fly ash;
2. according to the solid-liquid ratio g: mL =1:10 of activated high-alumina fly ash and leaching agent, 10g of activated high-alumina fly ash and 100mL of HNO3(5 mol/L), stirring in water bath at 90 ℃ for 2h, cooling to room temperature, washing with distilled water, vacuum filtering, collecting filter residue, drying the filter residue at 90 ℃, and grinding into fine powder;
3. weighing 20g of ground filter residue and a sodium hydroxide solution (5 mol/L) according to the solid-to-liquid ratio g: mL =1:10 of the ground filter residue to the leachate, mixing the mixture at 80 ℃ in a water bath for 24 hours, cooling to room temperature, washing with distilled water, carrying out vacuum filtration, and collecting filtrate;
4. weighing 6g P123 according to the solid-liquid ratio g: mL =1:120 of the P123 and the filtrate, mixing with the filtrate, and stirring in a water bath at 40 ℃ until the solution is clear;
5. dropwise pumping 5mol/L hydrochloric acid solution into the solution in the step 4 under stirring of water bath at 40 ℃, adjusting the pH to 0.48, stopping stirring, standing and aging for 36 hours, cooling to room temperature, washing with distilled water, vacuum filtering, collecting filter residue, drying the filter residue at 90 ℃, and grinding into fine powder;
6. placing the ground filter residue in a muffle furnace, heating to 550 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 5h, and then cooling to room temperature at the cooling rate of 1 ℃/min to obtain the mesoporous silica material; the specific surface area of the mesoporous silica material is 452.356m through the measurement of a full-automatic BET specific surface analysis tester2/g；
7. Adding 100mL of absolute ethanol and 0.5mL of aminopropyltriethoxysilane into 0.5g of mesoporous silica material, carrying out ultrasonic treatment at 5kHz and 25 ℃ for 30min, carrying out centrifugal washing with ethanol at 1000r for 5min, carrying out centrifugal washing for 6 times, taking solid precipitate, and drying at 60 ℃ for 12h to obtain an aminated mesoporous silica material; the specific surface area of the aminated mesoporous silica material is 398.549m by the measurement of a full-automatic BET specific surface analysis tester2/g。
Example 3:
1. uniformly mixing 10g of high-alumina fly ash and 20g of sodium carbonate according to the mass ratio of 1:2, roasting at 900 ℃ for 60min, cooling to room temperature after roasting is finished, and grinding into uniform powder to obtain activated high-alumina fly ash;
2. according to the solid-liquid ratio g: mL =1:20 of activated high-alumina fly ash and leaching agent, 10g of activated high-alumina fly ash and 200mL of HNO3(6 mol/L), stirring in water bath at 40 ℃ for 6 hours, cooling to room temperature, washing with distilled water, vacuum filtering, collecting filter residue, drying the filter residue at 90 ℃, and grinding into fine powder;
3. weighing 30g of ground filter residue and a sodium hydroxide solution (5 mol/L) according to the solid-to-liquid ratio g: mL =1:20 of the ground filter residue to the leachate, mixing the mixture at 80 ℃ in a water bath for 36h, cooling to room temperature, washing with distilled water, carrying out vacuum filtration, and collecting filtrate;
4. weighing 9g of P123 and the filtrate according to the solid-liquid ratio g: mL =1:80, mixing the P123 and the filtrate, and stirring in a water bath at 40 ℃ until the solution is clear;
5. dropwise pumping 5mol/L hydrochloric acid solution into the solution in the step 4 under stirring of water bath at 40 ℃, adjusting the pH value to 1, stopping stirring, standing and aging for 48 hours, cooling to room temperature, washing with distilled water, vacuum filtering, collecting filter residue, drying the filter residue at 90 ℃, and grinding into fine powder;
6. placing the ground filter residue in a muffle furnace, heating to 600 ℃ at the heating rate of 1 ℃/min, preserving the temperature for 6h, and then cooling to room temperature at the cooling rate of 1 ℃/min to obtain the mesoporous silica material; the specific surface area of the mesoporous silica material obtained by the determination of a full-automatic BET specific surface analysis tester is 485.265m2/g；
7. Weighing 0.5g of mesoporous silica material, adding 100mL of absolute ethanol and 1mL of aminopropyltriethoxysilane, and carrying out 5kHz ultrasonic treatment at 25 ℃ for 60 min; centrifuging and washing with ethanol at 1000r for 10min, centrifuging and washing for 4 times, drying the solid precipitate at 60 deg.C for 12h to obtain aminated mesoporous silica material, and determining with a full-automatic BET specific surface analysis tester to obtain aminated mesoporous silica material with specific surface area of 378.245m2/g。
Claims (7)
1. A method for producing an aminated mesoporous silica material by using high-alumina fly ash is characterized by comprising the following steps:
(1) mixing the high-alumina fly ash and an activating agent, roasting at the temperature of 700-900 ℃ for 60-180min, cooling to room temperature after roasting is finished, and grinding into uniform powder to obtain activated high-alumina fly ash;
(2) mixing the activated high-alumina fly ash obtained in the step (1) with 3-6mol/L of leaching agent, stirring in water bath at 40-90 ℃ for 2-6h, cooling to room temperature, washing with distilled water, vacuum filtering, collecting filter residue, drying and grinding into fine powder;
(3) mixing the filter residue ground in the step (2) with 5-10mol/L of leaching solution, stirring in water bath at 40-90 ℃ for 12-48h, cooling to room temperature, washing with distilled water, vacuum filtering, and collecting filtrate;
(4) mixing a nonionic surfactant with the filtrate obtained in the step (3), and stirring in a water bath at 40-90 ℃ until the solution is clear;
(5) dropwise adding 5-10mol/L acid solution into the solution in the step (4) under stirring of water bath at 40-90 ℃, adjusting the pH to 0-1, stopping stirring, standing and aging for 24-48h, cooling to room temperature, washing with distilled water, vacuum filtering, collecting filter residue, drying and grinding into fine powder;
(6) placing the filter residue after grinding in the step (5) in a muffle furnace, heating to 500-600 ℃ at the heating rate of 1 ℃/min, preserving the heat for 4-6h, and cooling to room temperature at the cooling rate of 1 ℃/min to obtain a mesoporous silica material;
(7) and (4) adding ethanol and an amination agent into the mesoporous silica material obtained in the step (6), performing ultrasonic treatment for 10-60min, performing centrifugal washing, and drying solid precipitates to obtain the aminated mesoporous silica material.
2. The method for producing the aminated mesoporous silica material by using the high-alumina fly ash according to claim 1, is characterized in that: the activating agent is sodium carbonate, and the mass ratio of the high-alumina fly ash to the activating agent is 1: 0.5-2.
3. The method for producing the aminated mesoporous silica material by using the high-alumina fly ash according to claim 1 is characterized by comprising the following steps: in the step (2), the leaching agent is a nitric acid solution, and the solid-to-liquid ratio g: mL of the activated high-alumina fly ash to the leaching agent is 1: 5-20.
4. The method for producing the aminated mesoporous silica material by using the high-alumina fly ash according to claim 1, is characterized in that: and (4) in the step (3), the leaching solution is a sodium hydroxide solution, and the solid-to-liquid ratio g/mL of the ground filter residue to the leaching solution is 1: 5-20.
5. The method for producing the aminated mesoporous silica material by using the high-alumina fly ash according to claim 1, is characterized in that: the nonionic surfactant is a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, and the solid-to-liquid ratio g: mL of the nonionic surfactant to the filtrate is 1: 80-120.
6. The method for producing the aminated mesoporous silica material by using the high-alumina fly ash according to claim 1, is characterized in that: and (5) the acid solution is hydrochloric acid solution.
7. The method for producing the aminated mesoporous silica material by using the high-alumina fly ash according to claim 1, is characterized in that: the ethanol is absolute ethanol, the amination agent is aminopropyltriethoxysilane, and the mass volume ratio g: mL of the mesoporous silica material to the amination agent is 1-5: 1-2.
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| CN112938995A (en) * | 2021-04-08 | 2021-06-11 | 昆明理工大学 | Method for preparing spherical silicon dioxide |
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| CN115231597A (en) * | 2022-07-08 | 2022-10-25 | 太原理工大学 | Fly ash-based mesoporous silicon-aluminum composite oxide material and preparation method thereof |
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