CN116651390A - Meta-aluminate modified fly ash and preparation method and application thereof - Google Patents
Meta-aluminate modified fly ash and preparation method and application thereof Download PDFInfo
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- CN116651390A CN116651390A CN202310841708.9A CN202310841708A CN116651390A CN 116651390 A CN116651390 A CN 116651390A CN 202310841708 A CN202310841708 A CN 202310841708A CN 116651390 A CN116651390 A CN 116651390A
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- 239000010881 fly ash Substances 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 239000013078 crystal Substances 0.000 claims description 19
- YAIQCYZCSGLAAN-UHFFFAOYSA-N [Si+4].[O-2].[Al+3] Chemical compound [Si+4].[O-2].[Al+3] YAIQCYZCSGLAAN-UHFFFAOYSA-N 0.000 claims description 18
- 239000004005 microsphere Substances 0.000 claims description 14
- 239000003463 adsorbent Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- WPUINVXKIPAAHK-UHFFFAOYSA-N aluminum;potassium;oxygen(2-) Chemical compound [O-2].[O-2].[Al+3].[K+] WPUINVXKIPAAHK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052730 francium Inorganic materials 0.000 claims description 3
- KLMCZVJOEAUDNE-UHFFFAOYSA-N francium atom Chemical compound [Fr] KLMCZVJOEAUDNE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052705 radium Inorganic materials 0.000 claims description 3
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052701 rubidium Inorganic materials 0.000 claims description 3
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 30
- 239000002351 wastewater Substances 0.000 abstract description 16
- 238000012986 modification Methods 0.000 abstract description 13
- 230000004048 modification Effects 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 230000002378 acidificating effect Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 239000002910 solid waste Substances 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000007500 overflow downdraw method Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000010883 coal ash Substances 0.000 description 6
- 238000011049 filling Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 239000011325 microbead Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- 238000013494 PH determination Methods 0.000 description 1
- 239000011959 amorphous silica alumina Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 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 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 150000003385 sodium Chemical class 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/06—Combustion residues, e.g. purification products of smoke, fumes or exhaust gases
- C04B18/10—Burned or pyrolised refuse
- C04B18/105—Gaseous combustion products or dusts collected from waste incineration, e.g. sludge resulting from the purification of gaseous combustion products of waste incineration
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- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
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- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
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Abstract
The invention belongs to the technical field of comprehensive utilization of solid wastes, and particularly relates to meta-aluminate modified fly ash and a preparation method and application thereof. The method for modifying the fly ash by microwave-meta-aluminate has the advantages of mild preparation conditions, low energy consumption, simple steps, no need of heating in the preparation process, convenient operation and control, and excellent adsorption performance of the obtained product, and good hydrothermal stability and adsorption stability. The preparation method provided by the invention is rapid and efficient in modification, free of pollution, and excellent in adsorption effect, and realizes high-quality utilization of the fly ash. Compared with the traditional alkali fusion method, the preparation method provided by the invention reduces energy consumption; compared with the traditional hydrothermal method, the method shortens the synthesis time, improves the production efficiency and also has the effect of reducing the energy consumption. The meta-aluminate modified fly ash prepared by the invention can neutralize the acidity of acidic pit wastewater and can adsorb various heavy metal ions in water.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of solid wastes, and particularly relates to meta-aluminate modified fly ash and a preparation method and application thereof.
Background
The adsorbent is a material capable of adsorbing one or more substances in gas or liquid on the surface thereof, thereby achieving a separation effect, and can be used for purifying waste water and waste gas. Currently, commonly used adsorbents are zeolite, molecular sieve, various activated carbon, and the like.
Fly ash is fine-grained dispersed industrial solid waste generated by coal combustion of a thermal power plant, and the main component of the fly ash is SiO 2 And Al 2 O 3 The total content of the two is more than 70 percent. The fly ash has volcanic ash characteristics, and the synthetic zeolite of the fly ash is an effective way for changing fly ash into valuables and obtaining products with high added value. Researchers use fly ash to prepare zeolite or molecular sieve as adsorbent for treating waste water or waste gas, but the synthesis conditions are harsh and the energy consumption is high.
Disclosure of Invention
The invention aims to provide meta-aluminate modified fly ash, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of meta-aluminate modified fly ash, which comprises the following steps:
mixing fly ash, meta-aluminate and water, and performing microwave irradiation to obtain meta-aluminate modified fly ash;
the microwave power of the microwave irradiation is 500-800W, and the irradiation time is 15-30 min.
Preferably, the meta-aluminate comprises one or more of sodium meta-aluminate, potassium meta-aluminate, rubidium meta-aluminate, cesium meta-aluminate, francium meta-aluminate, calcium meta-aluminate, strontium meta-aluminate, barium meta-aluminate and radium meta-aluminate.
Preferably, siO in the fly ash 2 、Al 2 O 3 And Fe (Fe) 2 O 3 The total content of the three oxides is not less than 60wt%.
Preferably, the mass ratio of the meta-aluminate to the water is 10-20:80-90; the ratio of the mass of the fly ash to the total volume of the meta-aluminate and the water is 0.5-1.5 g/6-15 mL.
Preferably, the fly ash has a particle size of no greater than 630 microns.
Preferably, the microwave irradiation further comprises: the resulting product was washed and dried sequentially.
Preferably, the temperature of the drying is 105-110 ℃, and the drying is to constant weight.
The invention also provides the meta-aluminate modified fly ash obtained by the preparation method of the scheme, which comprises silicon-aluminum oxide crystals and silicon-aluminum oxide crystal hollow microspheres; the mass ratio of the silicon aluminum oxide crystal to the silicon aluminum oxide crystal hollow microsphere is 0.2-0.5:0.5-0.8.
Preferably, the particle size of the meta-aluminate modified fly ash is 550-4000 microns.
The invention also provides application of the meta-aluminate modified fly ash as an adsorbent or a filling material.
The invention provides a preparation method of meta-aluminate modified fly ash. The preparation method disclosed by the invention has the advantages that the microwave-meta-aluminate modification is carried out on the fly ash, the preparation condition is mild, the energy consumption is lower, the steps are simple, the heating is not needed in the preparation process, the operation and control are convenient, the adsorption performance of the obtained product are excellent, all silicon-aluminum effective components including quartz and mullite in the fly ash can be fully activated, the silicon-aluminum components can be converted into silicon-aluminum oxide crystals with higher crystallinity and higher purity in the crystallization process, and the hollow microspheres are converted into silicon-aluminum oxide crystal hollow microspheres, so that the silicon-aluminum oxide crystal hollow microspheres have good hydrothermal stability and adsorption stability. The preparation method provided by the invention is rapid and efficient in modification, free of pollution, and excellent in adsorption effect, and realizes high-quality utilization of the fly ash. Compared with the traditional alkali fusion method, the preparation method provided by the invention reduces energy consumption; compared with the traditional hydrothermal method, the method shortens the synthesis time, improves the production efficiency and also has the effect of reducing the energy consumption.
The invention also provides the meta-aluminate modified fly ash obtained by the preparation method. In the meta-aluminate modified fly ash provided by the invention, the meta-aluminate is hydrolyzed to generate AlO 2- Amorphous SiO desorbed from fly ash 2 The reaction is carried out to form new silicon-aluminum oxide crystals, the hollow microspheres are converted into silicon-aluminum oxide crystal hollow microspheres, and heavy metals enter the crystal lattice of the silicon-aluminum oxide crystals through isomorphous substitution, so that the immobilized heavy metals are not easy to release. The meta-aluminate modified fly ash prepared by the invention can neutralize the acidity of acidic pit wastewater and can adsorb various heavy metal ions in water.
The invention also provides application of the meta-aluminate modified fly ash as an adsorbent or a filling material. The meta-aluminate modified fly ash can be used as a filling material of a precipitation reaction tank and an underground water permeation reaction grid, has good treatment effect, can be used for treating heavy metal wastewater with various purposes, including but not limited to acid pit wastewater, and has the characteristics of high efficiency, low cost and no secondary pollution when being used for the acid pit wastewater. The invention obviously reduces the synthesis cost of the modified fly ash, obviously improves the adsorption performance, and solves the problems of high modification cost and poor adsorption performance of the existing fly ash serving as an adsorbent.
The meta-aluminate modified fly ash prepared by the invention can neutralize the acidity of acidic pit wastewater and can be used for adsorbing various heavy metals in waterIons, e.g. Fe 3+ 、Cd 2+ Mn and 2+ etc., wherein, for Cd 2+ The maximum adsorption capacity of the catalyst can be increased from 34.48mg/g (fly ash before modification) to 59.94mg/g, and the catalyst can be used for Mn 2+ The maximum adsorption capacity of (3) can be increased from 23.70mg/g (fly ash before modification) to 25.04mg/g.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron micrograph of fly ash before and after modification of example 1;
FIG. 2 shows the reaction time of test example 2 for adsorbing Cd in fly ash before and after modification 2+ Is a function of (a) and (b).
FIG. 3 shows Mn adsorption by fly ash before and after modification by reaction time in test example 3 2+ Is a function of (a) and (b).
Detailed Description
The invention provides a preparation method of meta-aluminate modified fly ash, which comprises the following steps:
mixing fly ash, meta-aluminate and water, and performing microwave irradiation to obtain meta-aluminate modified fly ash;
the microwave power of the microwave irradiation is 500-800W, and the irradiation time is 15-30 min.
In the invention, siO in the fly ash 2 、Al 2 O 3 And Fe (Fe) 2 O 3 The total content of the three oxides is preferably not less than 60wt%, more preferably not less than 65wt%, further preferably not less than 70wt%; the particle size of the fly ash is preferably not greater than 630 microns, more preferably not greater than 600 microns, and even more preferably not greater than 550 microns.
In the invention, the fly ash is preferably pretreated before being mixed; the pretreatment is preferably: grinding the fly ash, sequentially sieving and washing; the fly ash with the target particle size is obtained through grinding and sieving; the water for washing is preferably deionized water; the number of times of the washing is preferably 2 to 5 times, more preferably 3 to 4 times; the solid-to-liquid ratio of the water washing is preferably 0.4 to 1g:10 to 20mL, more preferably 0.5 to 0.8g:15 to 16mL.
In the present invention, the meta-aluminate preferably includes one or more of sodium meta-aluminate, potassium meta-aluminate, rubidium meta-aluminate, cesium meta-aluminate, francium meta-aluminate, calcium meta-aluminate, strontium meta-aluminate, barium meta-aluminate and radium meta-aluminate, and more preferably sodium meta-aluminate.
In the invention, the mass ratio of the meta-aluminate to the water is preferably 10-20:80-90, more preferably 12-17:83-88, and even more preferably 15:85; the ratio of the mass of the fly ash to the total volume of meta-aluminate and water is preferably 0.5-1.5 g:6-15 mL, more preferably 0.5-1 g:8-10 mL, and even more preferably 1g:10mL.
In the invention, the mixing mode of the fly ash, the meta-aluminate and the water is preferably stirring; the rotation speed of stirring is preferably 100-300 r/min, more preferably 150-200 r/min, and the stirring time is preferably 5-20 min, more preferably 10-15 min; the mixing of the fly ash, meta-aluminate and water is preferably as follows: pre-mixing meta-aluminate and water to obtain meta-aluminate solution, and then mixing the meta-aluminate solution with fly ash.
In the present invention, the microwave power of the microwave irradiation is preferably 540 to 700W, more preferably 580 to 650W, further preferably 600W, and the irradiation time is preferably 15 to 30min, more preferably 18 to 25min, further preferably 20 to 22min.
In the present invention, the microwave irradiation preferably further comprises: washing and drying the obtained product in sequence; the washing is preferably water washing; the water for washing is preferably deionized water; the number of times of the washing is preferably 3 to 6 times, more preferably 4 to 5 times; the solid-liquid ratio of the washing is preferably 0.5-1.5 g:5-10 mL, more preferably 0.5-1 g:5-8 mL; the temperature of the drying is preferably 105 to 110 ℃, more preferably 105 to 108 ℃, and the drying is preferably to constant weight.
The invention also provides the meta-aluminate modified fly ash obtained by the preparation method of the scheme, which comprises silicon-aluminum oxide crystals and silicon-aluminum oxide crystal hollow microspheres; the mass ratio of the silicon aluminum oxide crystal to the silicon aluminum oxide crystal hollow microsphere is 0.2-0.5:0.5-0.8.
In the present invention, the particle size of the meta-aluminate-modified fly ash is preferably 550 to 4000. Mu.m, more preferably 830 to 1700. Mu.m, still more preferably 1000 to 1400. Mu.m.
The invention also provides application of the meta-aluminate modified fly ash as an adsorbent or a filling material.
In the present invention, the application of the meta-aluminate modified fly ash as an adsorbent preferably comprises the following steps:
and (3) throwing the meta-aluminate modified fly ash into the water body to be treated to finish adsorption, and taking out.
In the present invention, the addition amount of the meta-aluminate-modified fly ash is preferably 5 to 50g/L, more preferably 10 to 30g/L.
In the present invention, the time of the adsorption is preferably 20 to 90 minutes, more preferably 30 to 60 minutes.
The method for applying the meta-aluminate modified fly ash as the filling material has no special requirement, and the filling material can be obtained by adopting a conventional method in the field.
The following detailed description of the embodiments of the invention is provided in connection with the accompanying drawings and examples to further illustrate the invention, but should not be construed as limiting the scope of the invention.
Example 1
The preparation method of the meta-aluminate modified fly ash comprises the following steps:
and (3) soaking the fly ash with the particle size not more than 630 microns in a sodium metaaluminate solution with the mass concentration of 15%, uniformly mixing according to the solid-to-liquid ratio (W/v) of 1:15, carrying out microwave irradiation for 15min under the condition of 600W microwave power, washing with deionized water after the solution is cooled, and drying at 105 ℃ to constant weight to obtain the metaaluminate modified fly ash.
Test example 1
Surface morphology and specific surface area comparison of fly ash before and after modification in example 1:
specific surface areas and scanning electron microscope analyses were performed on the meta-aluminate modified fly ash and the unmodified fly ash respectively to verify the modification effect of the microwave-sodium meta-aluminate on the fly ash, and the results are shown in figure 1. As can be seen from FIG. 1, the unmodified fly ash has a certain amount of hollow microspheres with special structures, the number of the hollow microspheres is small, the sizes of the hollow microspheres are different, and the surface is smooth; after being modified by the microwave-sodium metaaluminate, the number of the microbeads on the surface of the fly ash is increased, the morphology is changed, and the surface of the microbeads is smoother and brighter; compared with unmodified fly ash, the specific surface area of the meta-aluminate modified fly ash is 7.27m 2 Reduced/g to 5.00m 2 Per g, the average pore diameter is reduced from 19.98nm to 16.18nm, but for Cd 2+ And Mn of 2+ The adsorption effect of the modified sodium metaaluminate is higher than that of unmodified coal ash, and the adsorption effect is probably due to the fact that the salt solution erodes the surface of the coal ash in the modification process of the sodium metaaluminate, so that the internal amorphous silica-alumina structure is exposed, metaaluminate enters pores and cracks of the coal ash, the eroded pore canal of the salt solution is blocked, the specific surface area of the coal ash is relatively reduced, but the adsorption active sites of the coal ash are increased due to the amorphous structure, and the adsorption performance of the coal ash is enhanced.
Test example 2
EXAMPLE 1 meta-aluminate modified fly ash and unmodified fly ash to remove Cd in Water 2+ Comparison:
taking two groups of analog Cd 2+ 50mL of wastewater (800 mg/L) was placed in 5 150mL beakers and simulated Cd was adjusted with NaOH and HCl solutions of different concentration gradients 2+ The pH of the polluted wastewater is adjusted to 6.5, 0.5g of meta-aluminate modified fly ash and 0.5g of unmodified fly ash are respectively added, the mixture is put into a constant temperature reaction shaking table (25 ℃ C., rotating speed is 175 r/min), sampling is carried out at adsorption time of 5min, 10min, 15min, 30min, 1h, 2h, 4h, 6h, 8h, 12h, 24h and 36h, the supernatant is filtered by a filter membrane of 0.45 mu m, and Cd in the filtrate is measured by ICP-MS 2+ Concentration.
Compared with unmodified fly ash (36 h), the meta-aluminate modified fly ash of the invention has the following characteristics of Cd 2+ The adsorption capacity of (2) is improved by 62%. By usingThe quasi-second-level kinetic model fits the adsorption results of meta-aluminate modified fly ash and unmodified fly ash, the fitting correlation coefficient is 0.9953 and 0.9998 respectively, the fitting effect is good, the fitting equilibrium adsorption amounts of the two fly ash are 60.50mg/g and 34.82mg/g respectively, and the fitting equilibrium adsorption amounts are similar to 59.94mg/kg and 34.48mg/kg obtained by experiments. It can be seen that the meta-aluminate modified fly ash of the invention is specific to Cd 2+ Has excellent adsorption capacity.
Test example 3
EXAMPLE 1 meta-aluminate modified fly ash and unmodified fly ash to remove Mn from Water 2+ Comparison:
taking two groups of simulation Mn 2+ 50mL of wastewater (880 mg/L) was placed in 5 150mL beakers and the simulated Mn was adjusted with NaOH and HCl solutions of different concentration gradients 2+ The pH of the polluted wastewater is adjusted to 6.5, 0.5g of meta-aluminate modified fly ash and 0.5g of unmodified fly ash are respectively added, the mixture is put into a constant temperature reaction shaking table (25 ℃ C., rotating speed is 175 r/min), sampling is carried out at adsorption time of 5min, 10min, 15min, 30min, 1h, 2h, 4h, 6h, 8h, 12h, 24h and 36h, supernatant is filtered by a filter membrane of 0.45 mu m, and Mn in filtrate is measured by ICP-MS 2+ Concentration.
Initial concentration of meta-aluminate modified fly ash and unmodified fly ash is 880mg/LMn by using quasi-second-level kinetic model 2+ The adsorption results of the solutions were fitted and the correlation coefficients (R 2 ) The theoretical saturated adsorption amounts after fitting the quasi-secondary adsorption kinetic equation are respectively 26.25mg/g and 25.83mg/g, which are respectively 0.990 and 0.973, and are more similar to the saturated adsorption amounts obtained by experiments in practical use, namely 25.04mg/g and 23.70 mg/g. It can be seen that the meta-aluminate modified fly ash of the invention has a specific Mn value 2+ The adsorption capacity of (a) is improved.
Test example 4
Example 1 static simulation experiment of meta-aluminate modified fly ash to remove acidic pit wastewater:
placing 300mL of spring acid pit wastewater into a 500mL beaker, respectively weighing 8g of fly ash, uniformly stirring at constant temperature (15 ℃) and constant speed (400 r/min) with a stirrer at constant temperature water bath, standing for 30min after stirring, filtering supernatant with a 0.45 μm filter membrane,determination of pH, total Fe concentration, total Cd concentration, total Mn concentration and SO 4 2- And (5) the concentration and the pollutant removal rate of the treated water sample are calculated. Ph=7.04, cd of the treated wastewater 2+ The concentration is 0.14mg/L, mn 2+ The concentration is 0.66mg/L, the total iron concentration is 0.03mg/L, and the requirements in the integrated wastewater discharge Standard (GB 8978-1996) are met: the total Cd standard limit value is 0.15mg/L, the total Mn standard limit value is 5mg/L, and the total Fe standard limit value is 6mg/L.
According to the embodiment, the method provided by the invention obviously reduces the synthesis cost of the modified fly ash, has mild synthesis conditions, solves the problems of high modification cost and poor adsorption performance of the existing fly ash serving as an adsorbent, and has obvious ecological benefit because the prepared meta-aluminate modified fly ash can adsorb various heavy metal ions in water.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (10)
1. A preparation method of meta-aluminate modified fly ash comprises the following steps:
mixing fly ash, meta-aluminate and water, and performing microwave irradiation to obtain meta-aluminate modified fly ash;
the microwave power of the microwave irradiation is 500-800W, and the irradiation time is 15-30 min.
2. The method of claim 1, wherein the meta-aluminate comprises one or more of sodium meta-aluminate, potassium meta-aluminate, rubidium meta-aluminate, cesium meta-aluminate, francium meta-aluminate, calcium meta-aluminate, strontium meta-aluminate, barium meta-aluminate, and radium meta-aluminate.
3. The method according to claim 1, wherein the fly ash contains SiO 2 、Al 2 O 3 And Fe (Fe) 2 O 3 Three oxidesNot less than 60% by weight in total.
4. The preparation method according to claim 1 or 2, wherein the mass ratio of meta-aluminate to water is 10-20:80-90;
the ratio of the mass of the fly ash to the total volume of the meta-aluminate and the water is 0.5-1.5 g/6-15 mL.
5. A method of making according to claim 1 or claim 3 wherein the fly ash has a particle size of no greater than 630 microns.
6. The method according to claim 1, wherein the microwave irradiation further comprises: the resulting product was washed and dried sequentially.
7. The method according to claim 6, wherein the drying is carried out at a temperature of 105 to 110 ℃ and the drying is carried out to a constant weight.
8. The meta-aluminate modified fly ash obtained by the preparation method according to any one of claims 1 to 7, comprising silicon-aluminum oxide crystals and silicon-aluminum oxide crystal hollow microspheres; the mass ratio of the silicon aluminum oxide crystal to the silicon aluminum oxide crystal hollow microsphere is 0.2-0.5:0.5-0.8.
9. The meta-aluminate modified fly ash according to claim 8, wherein the particle size of the meta-aluminate modified fly ash is 550 to 4000 microns.
10. Use of the meta-aluminate modified fly ash according to any of claims 8 to 9 as an adsorbent or filler material.
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