CN116813374B - Ceramic manufactured by fly ash of garbage power plant - Google Patents
Ceramic manufactured by fly ash of garbage power plant Download PDFInfo
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- CN116813374B CN116813374B CN202211605146.XA CN202211605146A CN116813374B CN 116813374 B CN116813374 B CN 116813374B CN 202211605146 A CN202211605146 A CN 202211605146A CN 116813374 B CN116813374 B CN 116813374B
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- fly ash
- stirring
- power plant
- washing
- solution
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- 239000010881 fly ash Substances 0.000 title claims abstract description 103
- 239000000919 ceramic Substances 0.000 title claims abstract description 67
- 239000010813 municipal solid waste Substances 0.000 title claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 78
- 238000005406 washing Methods 0.000 claims abstract description 64
- 239000003463 adsorbent Substances 0.000 claims abstract description 52
- 229920001661 Chitosan Polymers 0.000 claims abstract description 45
- 239000002699 waste material Substances 0.000 claims abstract description 38
- 238000005245 sintering Methods 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 31
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 26
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 13
- 239000002105 nanoparticle Substances 0.000 claims abstract description 13
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 13
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 108010024636 Glutathione Proteins 0.000 claims abstract description 10
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 10
- 229960003180 glutathione Drugs 0.000 claims abstract description 10
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005266 casting Methods 0.000 claims abstract description 9
- 238000004132 cross linking Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 85
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 69
- 238000001035 drying Methods 0.000 claims description 50
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 48
- 238000002156 mixing Methods 0.000 claims description 47
- 239000008367 deionised water Substances 0.000 claims description 38
- 229910021641 deionized water Inorganic materials 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 28
- 239000008055 phosphate buffer solution Substances 0.000 claims description 28
- 229960000583 acetic acid Drugs 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 20
- 239000012154 double-distilled water Substances 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 19
- 239000002122 magnetic nanoparticle Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 239000006260 foam Substances 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 16
- 239000011268 mixed slurry Substances 0.000 claims description 15
- 239000004568 cement Substances 0.000 claims description 14
- 239000004927 clay Substances 0.000 claims description 14
- 239000010433 feldspar Substances 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims description 14
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 14
- DOBUSJIVSSJEDA-UHFFFAOYSA-L 1,3-dioxa-2$l^{6}-thia-4-mercuracyclobutane 2,2-dioxide Chemical compound [Hg+2].[O-]S([O-])(=O)=O DOBUSJIVSSJEDA-UHFFFAOYSA-L 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 12
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 12
- 229910052753 mercury Inorganic materials 0.000 claims description 12
- 238000000746 purification Methods 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 229940074994 mercuric sulfate Drugs 0.000 claims description 8
- 229910000372 mercury(II) sulfate Inorganic materials 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 8
- 229910007926 ZrCl Inorganic materials 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000001384 succinic acid Substances 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 6
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000004088 foaming agent Substances 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 238000007731 hot pressing Methods 0.000 claims description 6
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 2
- BHTJEPVNHUUIPV-UHFFFAOYSA-N pentanedial;hydrate Chemical compound O.O=CCCCC=O BHTJEPVNHUUIPV-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 238000009270 solid waste treatment Methods 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 22
- 238000012360 testing method Methods 0.000 description 18
- 229910001385 heavy metal Inorganic materials 0.000 description 17
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 12
- 229910052801 chlorine Inorganic materials 0.000 description 12
- 239000000460 chlorine Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 229910000370 mercury sulfate Inorganic materials 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000006298 dechlorination reaction Methods 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 230000000185 dioxinlike effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 229940093915 gynecological organic acid Drugs 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012633 leachable Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/10—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by using foaming agents or by using mechanical means, e.g. adding preformed foam
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/135—Combustion residues, e.g. fly ash, incineration waste
- C04B33/1352—Fuel ashes, e.g. fly ash
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3481—Alkaline earth metal alumino-silicates other than clay, e.g. cordierite, beryl, micas such as margarite, plagioclase feldspars such as anorthite, zeolites such as chabazite
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
The invention relates to the technical field of solid waste treatment and resource utilization, and discloses ceramics made of fly ash of a garbage power plant. The preparation method of the ceramic prepared from the fly ash of the garbage power plant comprises the following steps: synthesizing a modified chitosan adsorbent and magnetic ZrMOF by a chemical method, and reacting the magnetic ZrMOF with glutathione, the modified chitosan adsorbent and melamine under the crosslinking of glutaraldehyde to obtain a composite adsorbent; carrying out microwave hydrothermal treatment and adsorption by a composite adsorbent on the waste power plant fly ash pretreated by water washing to obtain purified fly ash; sintering the purified fly ash at high temperature to obtain sintered fly ash; adding the sintered fly ash and the ground waste ceramic powder into a suspension containing multi-wall carbon nanotubes and magnetic nickel nanoparticles, adding other components, casting, molding, sintering and cooling to obtain the ceramic. The invention realizes harmless treatment of fly ash and reasonable utilization of resources; the ceramic of the invention has excellent electromagnetic interference shielding capability and fracture toughness resistance.
Description
Technical Field
The invention relates to the technical field of solid waste treatment and resource utilization, in particular to ceramics made of fly ash of a garbage power plant.
Background
Among the garbage disposal methods, the incineration method has the advantages of small occupied area, good reduction and recycling effects and the like, and is attracting more and more attention in China. The fly ash generated in the garbage incineration process is rich in leachable heavy metals, dioxin and other toxic substances and is listed as solid dangerous waste, so that a novel method capable of realizing the resource utilization of the fly ash of the garbage incineration power plant and the harmless treatment of the garbage incineration fly ash is explored, and the method has obvious environmental protection benefit and economic benefit.
Disclosure of Invention
In order to solve the technical problems, the invention provides ceramics prepared from fly ash of a garbage power plant, which is prepared by the following steps:
step (1) mixing and stirring the mercury coordination solution A and the chitosan acetic acid solution B, washing, suction filtering, crosslinking in glutaraldehyde with the volume fraction of 2.5%, washing, filtering, drying and grinding the gel obtained by the reaction to obtain a modified chitosan adsorbent;
in the process, mercury in a mercury coordination solution A formed by mercury sulfate and two organic acids (citric acid and succinic acid) reacts with amino in a chitosan acetic acid solution B to obtain the modified chitosan adsorbent with a chloride ion adsorption effect.
Step (2) ZrCl 4 Adding the magnetic nano particles attached to the silicon dioxide into a mixed solution of N, N-dimethylformamide and double distilled water, and stirring to obtain a mixture; dissolving 2-amino terephthalic acid in N, N-dimethylformamide, adding the mixture into the mixture, uniformly mixing, transferring the mixture into an autoclave, heating the mixture for reaction, collecting magnetic brown particles by using a magnet, washing the magnetic brown particles, and drying the magnetic brown particles to obtain magnetic ZrMOF;
in the process, the magnetic nano particles attached to the silicon dioxide are coordinated with the ZrMOF, and the magnetic nano particles attached to the silicon dioxide are grafted on the surface of the ZrMOF.
Dispersing magnetic ZrMOF in phosphate buffer solution, adding 2.5wt% glutaraldehyde water solution, stirring, separating and washing with magnet, adding the particles into phosphate buffer solution, adding glutathione, modified chitosan adsorbent and melamine, mixing at room temperature on a shaking table, and separating with magnetSeparating the reaction product, and washing to obtain a composite adsorbent; in the process, glutaraldehyde forms a cross-linked structure by losing two carbonyl groups to react with glutathione, a modified chitosan adsorbent, melamine and amine groups in the magnetic ZrMOF, and a large amount of-NH is introduced on the surface of the magnetic ZrMOF 2 -COOH, -NH, -CO, -SH, -OH, to obtain the composite adsorbent with high porosity and high adsorption capacity.
Step (4) mixing the water-washed and pretreated fly ash of the garbage power plant with deionized water, adding sodium hydroxide, transferring to a sealed polytetrafluoroethylene reactor, performing microwave hydrothermal treatment under a nitrogen atmosphere, heating for reaction, adjusting the pH of the solution to 7.2-7.4, adding a composite adsorbent, stirring for reaction, and purifying to obtain purified fly ash;
in the process, through microwave hydrothermal treatment, water is not only a solvent but also a reactant, and is also a medium for absorbing microwave energy, organic chlorine in the fly ash is converted into inorganic chlorine, and chloride ions and leached heavy metals in the solution after the microwave treatment are adsorbed into the composite adsorbent.
Step (5) sintering the purified fly ash at a high temperature of 800-3000 ℃, cooling to room temperature, and ball-milling to 200-500 meshes to obtain sintered fly ash; ball milling waste ceramic powder, cement, feldspar and clay respectively to 200-500 meshes for later use;
in the above process, a very small amount of heavy metals in the purified fly ash is solidified by high-temperature sintering, and simultaneously, dioxin-like organic matters in the fly ash are decomposed under the high-temperature condition.
Adding the multiwall carbon nanotubes and the magnetic nickel nanoparticles into aluminum sol, stirring, dripping hydrochloric acid to adjust the pH value to 4, then adding 5wt% of sodium dodecyl sulfate aqueous solution, and continuing stirring to obtain suspension; adding sintered fly ash and ground waste ceramic powder into the suspension, stirring, adding ground cement, ground feldspar, ground clay, FS-20 Pasteur water reducer, sodium tripolyphosphate, polyvinyl alcohol and water, and stirring uniformly to obtain mixed slurry; mixing and stirring the mixed slurry and the foam, casting, forming, drying, sintering and cooling the dried sample to obtain the ceramic.
In the process, due to electrostatic repulsion caused by adsorption of sodium dodecyl sulfate on the surface of the aluminum sol, the multi-wall carbon nano tube and the magnetic nickel nano particles are uniformly dispersed in the suspension, and uniformly coated on the surfaces of the fly ash and the ceramic powder by stirring, so that a uniform conductive network is formed on the surfaces of the fly ash and the ceramic powder.
Preferably, in the step (1):
the preparation method of the mercury coordination solution A comprises the following steps: adding 2.5-5kg of citric acid, 1.5-3kg of succinic acid and 4-8kg of mercuric sulfate into 500-1000L of deionized water, adding 1-2L of 70wt% concentrated sulfuric acid, and dissolving mercuric sulfate to prepare mercuric coordination solution A;
the preparation method of the chitosan acetic acid solution B comprises the following steps: weighing 20-40kg of chitosan, dissolving in 1000-2000L of glacial acetic acid water solution with volume fraction of 2%, and stirring at a rotation speed of 200-300r/min for 5-6h until the chitosan solution is completely bubble-free, thus obtaining chitosan acetic acid solution B.
Preferably, in the step (1), mixing and stirring time is: 1.5-2.5h; washing conditions of the gel obtained by the reaction: washing with deionized water for 3-5 times; crosslinking time: 30-40min; drying conditions: drying at 50-60deg.C to constant weight
Preferably, in the step (2), the method for preparing the silica-attached magnetic nanoparticle comprises: 9-18kg of nano Fe 3 O 4 Dispersing in a mixed solution formed by mixing double distilled water and ethanol according to the volume of 1:4, adding 100-200L of ammonia water and 21-42L of tetraethoxysilane, stirring for 12-16h at 40-50 ℃, collecting solid particles by using a magnet, washing by using ethanol, and drying at 140-160 ℃ to obtain the magnetic nano particles attached to silicon dioxide.
Preferably, in the step (2), the content of each component in the mixture is: zrCl 4 3-6kg, 1.5-3kg of magnetic nano particles attached to silicon dioxide, 200-400L of N, N-dimethylformamide and 750-1500mL of double distilled water; the dosage ratio of the 2-amino terephthalic acid to the N, N-dimethylformamide is 2.35-4.7kg:100-200L; heating reaction conditions: reacting for 24-30h at 110-120 ℃; washing conditions: flushing with double distilled water3-5 times; drying temperature: 50-70 ℃.
Preferably, in the step (3), a phosphate buffer solution is used: the pH is 7.4, and the concentration is 0.1mol/L; the dosage ratio of the magnetic ZrMOF to the phosphate buffer solution is 1-2kg:100-200L; stirring time: 6-8h; washing liquid adopted in the washing is phosphate buffer solution; the dosage ratio of the phosphate buffer solution, the glutathione, the modified chitosan adsorbent and the melamine is 200-400L:5-10kg:3-6kg:0.5-2kg; mixing time on shaking table: 8-10h.
Preferably, in the step (4), the method for water washing pretreatment of the fly ash of the garbage power plant comprises the following steps: adding 100-200kg of fly ash of a garbage power plant into 1000-2000L of deionized water, stirring at a rotation speed of 400-600r/min for 2-4h, filtering, repeating the above processes for 2-3 times, and drying the filtered solid at 80-100 ℃ for 24-36h;
preferably, in the step (4), the solid-to-liquid ratio of the fly ash of the waste power plant pretreated by water washing to deionized water is 0.1-0.2kg/L; the dosage of the sodium hydroxide and the composite adsorbent is respectively 10-20wt% and 3-10wt% of the total solid-liquid mixture of the fly ash of the garbage power plant and the deionized water which are subjected to water washing pretreatment; heating reaction conditions: reacting for 1-2h at 200-220 ℃; stirring reaction time: 8-10h; the purification method comprises the following steps: firstly, separating the composite adsorbent adsorbed with other substances by using a magnet, filtering the rest mixed solution, washing filter residues by using deionized water, and then drying.
Preferably, in the step (6), the method for preparing foam comprises: mixing 0.3-1.5kg of hydroxyethyl cellulose, 0.4-2kg of foaming agent and 4-5kg of water, and stirring for 3-5min to obtain foam; the dosage ratio of the multiwall carbon nano tube, the magnetic nickel nano particles, the aluminum sol and the 5wt% sodium dodecyl sulfate aqueous solution is 1.38-2.25kg:2.25-6.75kg:30-60kg:3-8kg; the mass ratio of the sintered fly ash to the ground waste ceramic powder to the ground cement to the ground feldspar to the ground clay to the FS-20 basf water reducer to the sodium tripolyphosphate to the polyvinyl alcohol to the water is 30-50:25-40:10-15:5-20:5-10:1.5-4:1.5-4:6-15:40-60; the amount of foam is 10-30wt% of the solid content of the mixed slurry.
Preferably, in the step (6), drying conditions after casting molding are as follows: naturally drying for 12-15h, and drying at 60-90deg.C for 6-10h; sintering conditions: heating the dried sample to 1000-1200 ℃ at a heating rate of 5 ℃/min for primary sintering, and preserving heat for 1.5-2.5h; then heating to 1350-1450 ℃ at a heating rate of 5 ℃/min, hot-pressing and sintering under constant pressure of 5-50MPa, and preserving heat for 1.5-2.5h.
Compared with the prior art, the invention has the beneficial effects that:
1. the fly ash and the waste ceramic powder of the garbage power plant are used as raw materials to be processed into the ceramic, so that waste is changed into valuable, reasonable utilization of resources is realized, and simultaneously, heat and part of waste heat generated by garbage incineration in the garbage power plant can be used in high-temperature heating and sintering operations in the ceramic preparation process, so that the energy utilization rate of the garbage power plant is improved, and the production cost is reduced.
2. The pretreatment mode of the fly ash is different from the traditional fly ash treatment, the heavy metal is recycled in a solidification mode, the organic chlorine in the fly ash is converted into inorganic chlorine through a microwave hydrothermal method, and chloride ions and heavy metals are adsorbed in the magnetic composite adsorbent through the cooperation of the composite adsorbent and the microwave hydrothermal method, so that 95% of the heavy metal and total chlorine in the fly ash can be removed, and the problem of secondary pollution in the traditional hydrothermal treatment process is avoided; the subsequent high-temperature sintering is carried out, so that residual heavy metals are solidified and organic matters such as dioxin are decomposed under the high-temperature condition, the harmless treatment of the fly ash is realized, the sintering quality in the ceramic preparation process is improved, the ceramic performance is improved, meanwhile, harmful substances in the finally prepared ceramic are greatly reduced, and the application range of the ceramic is enlarged; in addition, the composite adsorbent provided by the invention is easy to separate due to magnetism, can be continuously used after desorption, and is economical and environment-friendly.
3. In the process of preparing the ceramic, the conductive network formed by the multiwall carbon nanotubes and the magnetic nickel nanoparticles not only improves the electromagnetic interference shielding performance of the ceramic, but also improves the fracture toughness of the ceramic; in addition, unlike conventional foamed ceramic sintering mode, the present invention has hot pressed sintering after one sintering, the porous wall is broken into fragments under the sintering pressure to form disordered layered structure, and the fragments constitute grains with anisotropic growth into plate grains with great diameter-thickness ratio in the hot pressed sintering process, so that the plate grains exert fiber-like toughening mechanism to further raise the fracture toughness of the ceramic.
Drawings
FIG. 1 is a flow chart of a preparation process of ceramics made of fly ash of a garbage power plant;
FIG. 2 is a flow chart of a process for preparing the composite adsorbent of the present invention;
FIG. 3 is a graph showing the comparative test of the purification effect (total chlorine purification rate and heavy metal purification rate) of fly ash of examples 1 to 4 and comparative examples 1 to 2 in the present invention;
FIG. 4 is a graph showing comparison of EMI shielding effectiveness tests for the ceramics of examples 1-4 and comparative examples 1-5 in accordance with the present invention;
FIG. 5 is a graph comparing fracture toughness tests of the ceramics of examples 1-4 and comparative examples 1-5 in the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Example 1
The embodiment discloses a preparation method of ceramic manufactured by fly ash of a garbage power plant, which comprises the following steps:
step (1), adding 2.5kg of citric acid, 1.5kg of succinic acid and 4kg of mercuric sulfate into 500L of deionized water, adding 1L of 70wt% concentrated sulfuric acid, and dissolving the mercuric sulfate to prepare a mercuric coordination solution A; weighing 20kg of chitosan, dissolving in 1000L of glacial acetic acid aqueous solution with volume fraction of 2%, and stirring at a rotating speed of 200r/min for 5h until the chitosan solution is completely bubble-free to obtain chitosan acetic acid solution B; mixing and stirring the mercury coordination solution A and the chitosan acetic acid solution B for 1.5 hours, washing gel obtained by the reaction with deionized water for 3 times, carrying out suction filtration, then placing the gel in glutaraldehyde with the volume fraction of 2.5% for crosslinking for 30 minutes, washing, filtering, drying to constant weight at 50 ℃, and grinding to obtain the modified chitosan adsorbent.
Step (2) 9kg of nano Fe 3 O 4 Dispersing in a mixed solution formed by mixing double distilled water and ethanol according to the volume of 1:4, adding 100L of ammonia water and 21L of tetraethoxysilane, stirring for 12 hours at 40 ℃, collecting solid particles by using a magnet, washing by using ethanol, and drying at 140 ℃ to obtain magnetic nano particles attached to silicon dioxide; 3kg ZrCl 4 Adding 1.5kg of the magnetic nano particles attached to the silicon dioxide into 200L of mixed solution of N, N-dimethylformamide and 750mL of double distilled water, and stirring for 15min to obtain a mixture; 2.35kg of 2-amino terephthalic acid was dissolved in 100L of N, N-dimethylformamide, added to the above mixture, transferred to an autoclave after uniform mixing, reacted at 110℃for 24 hours, collected magnetic brown particles with a magnet, washed 3 times with double distilled water, and dried at 50℃to obtain magnetic ZrMOF.
Step (3) dispersing 1kg of magnetic ZrMOF in 0.1mol/L phosphate buffer solution with the concentration of 100L, pH being 7.4, adding 250L of 2.5wt% glutaraldehyde aqueous solution, stirring for 6 hours, separating particles by using a magnet, washing 3 times by using the phosphate buffer solution, adding the particles into 200L of the phosphate buffer solution, adding 5kg of glutathione, 3kg of modified chitosan adsorbent and 0.5kg of melamine, mixing on a shaking table at room temperature for 8 hours, separating a reaction product by using a magnet, and washing 3 times by using the phosphate buffer solution to obtain the composite adsorbent.
Step (4) adding 100kg of waste power plant fly ash into 1000L of deionized water, stirring for 2 hours at a rotating speed of 400r/min, filtering, repeating the above process for 2 times, and drying the filtered solid at 80 ℃ for 24 hours to obtain waste power plant fly ash pretreated by water washing; mixing the water-washed and pretreated fly ash of the garbage power plant with deionized water at a solid-liquid ratio of 0.1kg/L, adding 10wt% sodium hydroxide into the solid-liquid mixture, transferring into a sealed polytetrafluoroethylene reactor, performing microwave hydrothermal treatment under a nitrogen atmosphere, reacting for 1h at 200 ℃, adjusting the pH of the solution to 7.2 with acetic acid, adding a composite adsorbent, stirring for 8h, firstly separating the composite adsorbent adsorbed with other substances with a magnet after the reaction is finished, filtering the rest mixed solution, washing filter residues with deionized water, and drying to obtain purified fly ash; wherein the dosage of the composite adsorbent is 3wt% of the total solid-liquid mixture of the fly ash of the garbage power plant and the deionized water which are pretreated by water washing.
Step (5) sintering the purified fly ash at a high temperature of 800 ℃, cooling to room temperature, and ball-milling to 200 meshes to obtain sintered fly ash; ball milling the waste ceramic powder, cement, feldspar and clay to 200-500 meshes respectively for standby.
Step (6), mixing 0.3kg of hydroxyethyl cellulose, 0.4kg of foaming agent and 4kg of water, and stirring for 3min to obtain foam; adding 1.38kg of multiwall carbon nanotubes and 2.25kg of magnetic nickel nano particles into 30kg of aluminum sol, stirring at the speed of 300r/min for 0.5h, dropwise adding hydrochloric acid to adjust the pH value to 4, then adding 3kg of 5wt% of sodium dodecyl sulfate aqueous solution, and continuously stirring for 0.5h to obtain a suspension; adding 30kg of sintered fly ash and 25kg of ground waste ceramic powder into the suspension, stirring at a speed of 300r/min for 1.5h, adding 10kg of ground cement, 5kg of ground feldspar, 5kg of ground clay, 1.5kg of FS-20 Pasteur water reducer, 1.5kg of sodium tripolyphosphate, 6kg of polyvinyl alcohol and 40kg of water, and stirring uniformly to obtain mixed slurry; mixing and stirring the mixed slurry and foam with the solid content of 10wt% for 1min, casting, naturally drying for 12h, drying at 60 ℃ for 6h, heating the dried sample to 1000 ℃ at a heating rate of 5 ℃/min for primary sintering, and preserving heat for 1.5h; and then heating to 1350 ℃ at a heating rate of 5 ℃/min, hot-pressing and sintering under constant pressure of 5MPa, preserving heat for 1.5h, and cooling the sintered solidified body to room temperature along with a furnace to obtain the ceramic.
Example 2
The embodiment discloses a preparation method of ceramic manufactured by fly ash of a garbage power plant, which comprises the following steps:
step (1), adding 5kg of citric acid, 3kg of succinic acid and 8kg of mercury sulfate into 1000L of deionized water, adding 2L of 70wt% concentrated sulfuric acid, and dissolving the mercury sulfate to prepare mercury coordination solution A; weighing 40kg of chitosan, dissolving in 2000L of glacial acetic acid aqueous solution with volume fraction of 2%, and stirring at a rotating speed of 300r/min for 6 hours until the chitosan solution is completely bubble-free, so as to obtain chitosan acetic acid solution B; mixing and stirring the mercury coordination solution A and the chitosan acetic acid solution B for 2.5 hours, washing gel obtained by the reaction with deionized water for 5 times, carrying out suction filtration, then placing the gel in glutaraldehyde with the volume fraction of 2.5% for crosslinking for 40 minutes, washing, filtering, drying to constant weight at 60 ℃, and grinding to obtain the modified chitosan adsorbent.
Step (2) 18kg of nano Fe 3 O 4 Dispersing in a mixed solution formed by mixing double distilled water and ethanol according to the volume of 1:4, adding 200L of ammonia water and 42L of tetraethoxysilane, stirring for 16 hours at 50 ℃, collecting solid particles by using a magnet, washing by using ethanol, and drying at 160 ℃ to obtain magnetic nano particles attached to silicon dioxide; 6kg ZrCl 4 Adding 3kg of the silicon dioxide-attached magnetic nano particles into 400L of mixed solution of N, N-dimethylformamide and 1500mL of double distilled water, and stirring for 30min to obtain a mixture; 4.7kg of 2-amino terephthalic acid is dissolved in 200L of N, N-dimethylformamide, added into the mixture, uniformly mixed and transferred into an autoclave to react for 30 hours at 120 ℃, magnetic brown particles are collected by a magnet, washed 5 times by double distilled water and dried at 70 ℃ to obtain the magnetic ZrMOF.
And (3) dispersing 2kg of magnetic ZrMOF in 0.1mol/L phosphate buffer solution with the concentration of 200L, pH being 7.4, adding 500L of 2.5wt% glutaraldehyde aqueous solution, stirring for 8 hours, separating particles by using a magnet, washing the particles with the phosphate buffer solution for 5 times, adding the particles into 400L of phosphate buffer solution, adding 10kg of glutathione, 6kg of modified chitosan adsorbent and 2kg of melamine, mixing the materials on a shaking table at room temperature for 10 hours, separating a reaction product by using the magnet, and washing the reaction product with the phosphate buffer solution for 5 times to obtain the composite adsorbent.
Step (4) adding 200kg of waste power plant fly ash into 2000L of deionized water, stirring for 4 hours at a rotating speed of 600r/min, filtering, repeating the above process for 3 times, and drying the filtered solid at 100 ℃ for 36 hours to obtain waste power plant fly ash pretreated by water washing; mixing the water-washed and pretreated fly ash of the garbage power plant with deionized water according to the solid-liquid ratio of 0.2kg/L, adding sodium hydroxide with the weight percent of the solid-liquid mixture into a sealed polytetrafluoroethylene reactor, carrying out microwave hydrothermal treatment under the nitrogen atmosphere, reacting for 2 hours at 220 ℃, adjusting the pH value of the solution to 7.4 by acetic acid, adding a composite adsorbent, stirring for 10 hours, firstly separating the composite adsorbent adsorbed with other substances by using a magnet after the reaction is finished, filtering the rest mixed solution, washing filter residues by using deionized water, and drying to obtain purified fly ash; wherein the dosage of the composite adsorbent is 10wt% of the total solid-liquid mixture of the fly ash of the garbage power plant and the deionized water which are pretreated by water washing.
Step (5) sintering the purified fly ash at a high temperature of 3000 ℃, cooling to room temperature, and ball-milling to 500 meshes to obtain sintered fly ash; and respectively ball-milling the waste ceramic powder, cement, feldspar and clay to 500 meshes for later use.
Step (6) mixing 1.5kg of hydroxyethyl cellulose, 2kg of foaming agent and 5kg of water, and stirring for 5min to obtain foam; adding 2.25kg of multiwall carbon nanotubes and 6.75kg of magnetic nickel nano particles into 60kg of aluminum sol, stirring at the speed of 400r/min for 1h, dropwise adding hydrochloric acid to adjust the pH value to 4, then adding 8kg of 5wt% sodium dodecyl sulfate aqueous solution, and continuously stirring for 1h to obtain a suspension; adding 50kg of sintered fly ash and 40kg of ground waste ceramic powder into the suspension, stirring at a speed of 400r/min for 2.5 hours, adding 15kg of ground cement, 20kg of ground feldspar, 10kg of ground clay, 4kg of FS-20 Baff water reducer, 4kg of sodium tripolyphosphate, 15kg of polyvinyl alcohol and 60kg of water, and stirring uniformly to obtain mixed slurry; mixing and stirring the mixed slurry and foam with the solid content of 30wt% of the mixed slurry for 3min, casting and molding, naturally drying for 15h, drying for 10h at 90 ℃, heating the dried sample to 1200 ℃ at a heating rate of 5 ℃/min for primary sintering, and preserving heat for 2.5h; and then heating to 1450 ℃ at a heating rate of 5 ℃/min, hot-pressing and sintering under a constant pressure of 50MPa, preserving heat for 2.5h, and cooling the sintered solidified body to room temperature along with a furnace to obtain the ceramic.
Example 3
The embodiment discloses a preparation method of ceramic manufactured by fly ash of a garbage power plant, which comprises the following steps:
step (1), adding 3kg of citric acid, 2kg of succinic acid and 5kg of mercury sulfate into 700L of deionized water, adding 1.3L of 70wt% concentrated sulfuric acid, and dissolving the mercury sulfate to prepare mercury coordination solution A; weighing 25kg of chitosan, dissolving in 1300L of glacial acetic acid aqueous solution with volume fraction of 2%, and stirring at a rotating speed of 250r/min for 5.3h until the chitosan solution is completely bubble-free to obtain chitosan acetic acid solution B; mixing and stirring the mercury coordination solution A and the chitosan acetic acid solution B for 1.8 hours, washing gel obtained by the reaction with deionized water for 3 times, carrying out suction filtration, then placing the gel in glutaraldehyde with the volume fraction of 2.5% for crosslinking for 35 minutes, washing, filtering, drying to constant weight at 55 ℃, and grinding to obtain the modified chitosan adsorbent.
Step (2) 12kg of nano Fe 3 O 4 Dispersing in a mixed solution formed by mixing double distilled water and ethanol according to the volume of 1:4, adding 130L ammonia water and 28L tetraethoxysilane, stirring for 14 hours at 44 ℃, collecting solid particles by using a magnet, washing by using ethanol, and drying at 145 ℃ to obtain magnetic nano particles attached to silicon dioxide; 4kg ZrCl 4 Adding 2kg of the silicon dioxide-attached magnetic nano particles into 250L of mixed solution of N, N-dimethylformamide and 900mL of double distilled water, and stirring for 20min to obtain a mixture; 3kg of 2-amino terephthalic acid was dissolved in 130L of N, N-dimethylformamide, added to the above mixture, transferred to an autoclave after uniform mixing, reacted at 113℃for 26 hours, collected magnetic brown particles with a magnet, washed 4 times with double distilled water, and dried at 55℃to obtain magnetic ZrMOF.
Step (3) dispersing 1.5kg of magnetic ZrMOF in 130L, pH of 7.4 0.1mol/L phosphate buffer solution, then adding 300L of 2.5wt% glutaraldehyde aqueous solution, stirring for 6.5h, separating particles by using a magnet, washing with the phosphate buffer solution for 4 times, then adding the particles into 250L of phosphate buffer solution, adding 6.5kg of glutathione, 4kg of modified chitosan adsorbent and 1kg of melamine, mixing for 8.5h on a shaking table at room temperature, separating a reaction product by using a magnet, and washing with the phosphate buffer solution for 4 times to obtain the composite adsorbent.
Step (4) adding 130kg of waste power plant fly ash into 1400L of deionized water, stirring at a rotating speed of 450r/min for 2.5h, filtering, repeating the above process for 3 times, and drying the filtered solid at 85 ℃ for 28h to obtain waste power plant fly ash pretreated by water washing; mixing the water-washed and pretreated fly ash of the garbage power plant with deionized water according to the solid-liquid ratio of 0.14kg/L, adding 13wt% of sodium hydroxide into the solid-liquid mixture, transferring into a sealed polytetrafluoroethylene reactor, carrying out microwave hydrothermal treatment under the nitrogen atmosphere, reacting for 1.3 hours at 205 ℃, regulating the pH value of the solution to 7.2 by using acetic acid, adding a composite adsorbent, stirring for 8.5 hours, firstly separating the composite adsorbent adsorbed with other substances by using a magnet after the reaction is finished, filtering the rest mixed solution, washing filter residues by using deionized water, and drying to obtain purified fly ash; wherein the dosage of the composite adsorbent is 5wt% of the total solid-liquid mixture of the fly ash of the garbage power plant and the deionized water which are pretreated by water washing.
Step (5) sintering the purified fly ash at a high temperature of 1600 ℃, cooling to room temperature, and ball-milling to 300 meshes to obtain sintered fly ash; and respectively ball-milling the waste ceramic powder, cement, feldspar and clay to 300 meshes for later use.
Step (6) mixing 0.7kg of hydroxyethyl cellulose, 0.9kg of foaming agent and 4.3kg of water, and stirring for 4min to obtain foam; adding 1.62kg of multiwall carbon nanotubes and 3.75kg of magnetic nickel nano particles into 40kg of aluminum sol, stirring at the speed of 330r/min for 0.6h, dropwise adding hydrochloric acid to adjust the pH value to 4, then adding 4.5kg of 5wt% sodium dodecyl sulfate aqueous solution, and continuously stirring for 0.6h to obtain a suspension; adding 35kg of sintered fly ash and 30kg of ground waste ceramic powder into the suspension, stirring at a speed of 330r/min for 1.8 hours, adding 11kg of ground cement, 10kg of ground feldspar, 6kg of ground clay, 2kg of FS-20 Baff water reducer, 2kg of sodium tripolyphosphate, 9kg of polyvinyl alcohol and 45kg of water, and stirring uniformly to obtain mixed slurry; mixing and stirring the mixed slurry and foam with the solid content of 15wt% for 2min, casting, naturally drying for 13h, drying for 7h at 70 ℃, heating the dried sample to 1050 ℃ at a heating rate of 5 ℃/min for primary sintering, and preserving heat for 1.8h; and then heating to 1400 ℃ at a heating rate of 5 ℃/min, hot-pressing and sintering under constant pressure of 20MPa, preserving heat for 1.8h, and cooling the sintered solidified body to room temperature along with a furnace to obtain the ceramic.
Example 4
The embodiment discloses a preparation method of ceramic manufactured by fly ash of a garbage power plant, which comprises the following steps:
step (1), adding 4kg of citric acid, 2.5kg of succinic acid and 6.5kg of mercuric sulfate into 850L of deionized water, adding 1.6L of 70wt% concentrated sulfuric acid, and dissolving the mercuric sulfate to prepare a mercuric coordination solution A; weighing 30kg of chitosan, dissolving in 1600L of glacial acetic acid aqueous solution with volume fraction of 2%, and stirring at a rotating speed of 280r/min for 5.6h until the chitosan solution is completely bubble-free to obtain chitosan acetic acid solution B; mixing and stirring the mercury coordination solution A and the chitosan acetic acid solution B for 2.1h, washing gel obtained by the reaction with deionized water for 4 times, carrying out suction filtration, then placing the gel in glutaraldehyde with the volume fraction of 2.5% for crosslinking for 35min, washing, filtering, drying to constant weight at 58 ℃, and grinding to obtain the modified chitosan adsorbent.
Step (2) 15kg of nano Fe 3 O 4 Dispersing in a mixed solution formed by mixing double distilled water and ethanol according to the volume of 1:4, then adding 160L of ammonia water and 35L of tetraethoxysilane, stirring for 15 hours at 48 ℃, collecting solid particles by using a magnet, washing by using ethanol, and drying at 150 ℃ to obtain magnetic nano particles attached to silicon dioxide; 5kg ZrCl 4 Adding 2.5kg of the magnetic nano particles attached to the silicon dioxide into 300L of mixed solution of N, N-dimethylformamide and 1200mL of double distilled water, and stirring for 25min to obtain a mixture; 3.6kg of 2-amino terephthalic acid was dissolved in 160L of N, N-dimethylformamide, added to the above mixture, transferred to an autoclave after uniform mixing, reacted at 115℃for 28 hours, collected magnetic brown particles with a magnet, washed 4 times with double distilled water, and dried at 60℃to obtain magnetic ZrMOF.
Step (3) dispersing 1.8kg of magnetic ZrMOF in 160L, pH of 7.4 0.1mol/L phosphate buffer solution, then adding 400L of 2.5wt% glutaraldehyde aqueous solution, stirring for 7h, then separating particles by using a magnet and washing for 4 times by using the phosphate buffer solution, then adding the particles into 300L of phosphate buffer solution, then adding 8kg of glutathione, 5kg of modified chitosan adsorbent and 1.5kg of melamine, mixing for 9h on a shaking table at room temperature, separating reaction products by using a magnet, and washing for 4 times by using the phosphate buffer solution to obtain the composite adsorbent.
Step (4) 160kg of waste power plant fly ash is added into 1600L of deionized water, stirred for 3 hours at a rotating speed of 500r/min, filtered, the process is repeated for 3 times, and the filtered solid is dried for 32 hours at 90 ℃ to obtain waste power plant fly ash pretreated by washing; mixing the water-washed and pretreated fly ash of the garbage power plant with deionized water according to the solid-liquid ratio of 0.18kg/L, adding 16wt% sodium hydroxide of the solid-liquid mixture, transferring into a sealed polytetrafluoroethylene reactor, performing microwave hydrothermal treatment under the nitrogen atmosphere, reacting for 1.6 hours at 210 ℃, adjusting the pH of the solution to 7.3 by acetic acid, adding a composite adsorbent, stirring for 9 hours, firstly separating the composite adsorbent adsorbed with other substances by using a magnet after the reaction is finished, filtering the residual mixed solution, washing filter residues by using deionized water, and drying to obtain purified fly ash; wherein the dosage of the composite adsorbent is 8wt% of the total solid-liquid mixture of the fly ash of the garbage power plant and the deionized water which are pretreated by water washing.
Step (5) sintering the purified fly ash at high temperature of 2400 ℃, cooling to room temperature, and ball-milling to 400 meshes to obtain sintered fly ash; and respectively ball-milling the waste ceramic powder, cement, feldspar and clay to 400 meshes for later use.
Step (6), mixing 1.1kg of hydroxyethyl cellulose, 1.5kg of foaming agent and 4.6kg of water, and stirring for 4min to obtain foam; adding 1.98kg of multiwall carbon nanotubes and 5.25kg of magnetic nickel nano particles into 50kg of aluminum sol, stirring at the speed of 350r/min for 0.8h, dropwise adding hydrochloric acid to adjust the pH value to 4, then adding 6kg of 5wt% sodium dodecyl sulfate aqueous solution, and continuously stirring for 0.8h to obtain a suspension; adding 40kg of sintered fly ash and 35kg of ground waste ceramic powder into the suspension, stirring at a speed of 360r/min for 2.1h, adding 13kg of ground cement, 15kg of ground feldspar, 8kg of ground clay, 3kg of FS-20 Baff water reducer, 3kg of sodium tripolyphosphate, 12kg of polyvinyl alcohol and 50kg of water, and stirring uniformly to obtain mixed slurry; mixing and stirring the mixed slurry and foam with the solid content of 20wt% for 2min, casting, naturally drying for 14h, drying at 80 ℃ for 8h, heating the dried sample to 1100 ℃ at a heating rate of 5 ℃/min for primary sintering, and preserving heat for 2.1h; and then heating to 1450 ℃ at a heating rate of 5 ℃/min, hot-pressing and sintering under constant pressure of 35MPa, preserving heat for 2 hours, and cooling the sintered solidified body to room temperature along with a furnace to obtain the ceramic.
Comparative example 1
Comparative example 1 compared with example 3, no microwave hydrothermal treatment was performed during the preparation of purified fly ash, and the other conditions were unchanged.
Comparative example 2
Comparative example 2 compared with example 3, no composite adsorbent was added during the preparation of the purified fly ash, and the other conditions were unchanged.
Comparative example 3
Comparative example 3 compared with example 3, the multi-walled carbon nanotubes were not added during the preparation of the ceramic, and the other conditions were unchanged.
Comparative example 4
Comparative example 4 compared with example 3, no magnetic nickel nanoparticle was added during the preparation of the ceramic, and the other conditions were unchanged.
Comparative example 5
Comparative example 5 compared with example 3, the hot press sintering was not performed during the preparation of the ceramic, and the other conditions were not changed.
Experimental example
Test one, purification Effect test of fly ash
The total chlorine content and the heavy metal content in the fly ash of the garbage power plant and the purified fly ash in examples 1 to 4 and comparative examples 1 to 2 were measured, and the total chlorine purification rate and the heavy metal purification rate of the fly ash were calculated.
The method for measuring the total chlorine content comprises the following steps: the chlorine content was measured using japanese industrial standard (JIS A1 1 54), and the specific steps were as follows: grinding the fly ash sample to below 150pm, and drying for later use: mixing 65% nitric acid and distilled water according to the volume ratio of l:6, mixing and preparing nitric acid (1+6) reagent; adding 70mL of nitric acid (1+6) reagent into the 109 samples, magnetically stirring for 30min, heating and boiling for about 5min, and cooling to normal temperature; filtering by a vacuum filtration device, and taking filtrate to fix the volume; and measuring the content of chloride ions in the filtrate after the constant volume by adopting an ion chromatograph, and obtaining the total content of chloride in the fly ash after conversion of the obtained result.
The heavy metal content determination method comprises the following steps: adopting an electric heating plate digestion method to digest a sample to be measured, and specifically comprising the following steps: the sample to be tested is at 105.C, drying in a drying oven until the weight is constant, and then sieving with a 100-target standard sieve; adding 6mL of concentrated nitric acid (65%), 2mL of hydrogen peroxide (30%) and 2mL of hydrofluoric acid (30%) into 0.1g of sieved sample, and heating and digesting on a 200 ℃ electric heating plate; after the solid is completely dissolved, adding a certain amount of distilled water, continuously heating to near dryness at 100 ℃ on an electric hot plate to volatilize HF, and transferring the digestion solution to a 50mL volumetric flask to fix the volume by dilute nitric acid with the mass fraction of 4%; and determining the heavy metal content of the digestion liquid after the constant volume by using an inductively coupled plasma emission spectrometry, and converting the heavy metal content into the solid-phase heavy metal content of the fly ash.
The test results are shown in table 1:
TABLE 1
Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | |
Total chlorine purification rate/% | 99.1 | 99.6 | 99.3 | 99.5 | 95.3 | 98.6 |
Heavy metal purification rate/% | 97.9 | 99.2 | 98.3 | 98.7 | 97.5 | 93.2 |
As can be seen from the test results in Table 1, the total chlorine and heavy metal contents in the purified fly ash obtained in examples 1 to 4 of the present invention are greatly reduced; as is clear from comparative example 1, the microwave hydrothermal dechlorination effect is superior to the traditional water washing dechlorination (dechlorination effect is 95-98%); as can be seen from comparative example 2, both microwave hydrothermal and composite adsorbents have a positive effect on the removal of heavy metals.
Testing II, ceramic performance testing: the ceramics prepared in examples 1-4 and comparative examples 1-5 were tested for EMI Shielding Effectiveness (SE), fracture toughness.
1) EMI Shielding Effectiveness (SE):
wherein X is the electric field strength, subscript 0 indicates no shield, and subscript 1 indicates shield.
The test frequency range is 130-1800MHz, and the propagation speed of electromagnetic wave in airThe rate is about 3X 10 8 m/s, the test wavelength can be obtained: testing low frequency f l Test wavelength lambda =130 MHz l =2300 mm; test high frequency f h Test wavelength λ =1800 MHz h =167mm。
2) Fracture toughness (K)
The fracture toughness of the samples was measured by a three-point bending method using a universal tester with a crosshead speed of 0.05mm/min. The samples were beam-shaped samples of 4X 2X 16mm (toughness test). Prior to testing, single side band notched beam (SENB) specimens were notched to a depth of about 2mm with a 200 μm thick diamond saw.
The test results are shown in table 2:
TABLE 2
From the test results of Table 2, it is understood that the ceramics prepared in examples 1 to 4 of the present invention have excellent electromagnetic interference shielding ability and fracture toughness; as can be seen from comparative example 5, the fracture toughness of the ceramic can be improved by performing hot press sintering after the primary sintering; as is clear from comparative examples 3 and 4, the synergistic effect of the multiwall carbon nanotubes and the magnetic nickel nanoparticles can improve the electromagnetic interference shielding capability and fracture toughness of the ceramics.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The ceramic manufactured by the fly ash of the garbage power plant is characterized by being prepared by the following steps:
step (1) mixing and stirring the mercury coordination solution A and the chitosan acetic acid solution B, washing, suction filtering, crosslinking in glutaraldehyde with the volume fraction of 2.5%, washing, filtering, drying and grinding the gel obtained by the reaction to obtain a modified chitosan adsorbent; the preparation method of the mercury coordination solution A comprises the following steps: adding 2.5-5kg of citric acid, 1.5-3kg of succinic acid and 4-8kg of mercuric sulfate into 500-1000L of deionized water, adding 1-2L of 70wt% concentrated sulfuric acid, and dissolving mercuric sulfate to prepare mercuric coordination solution A; the preparation method of the chitosan acetic acid solution B comprises the following steps: weighing 20-40kg of chitosan, dissolving in 1000-2000L of glacial acetic acid aqueous solution with volume fraction of 2%, and stirring at a rotating speed of 200-300r/min for 5-6h until the chitosan solution is completely bubble-free to obtain chitosan acetic acid solution B;
step (2) ZrCl 4 Adding the magnetic nano particles attached to the silicon dioxide into a mixed solution of N, N-dimethylformamide and double distilled water, and stirring to obtain a mixture; dissolving 2-amino terephthalic acid in N, N-dimethylformamide, adding the mixture into the mixture, uniformly mixing, transferring the mixture into an autoclave, heating the mixture for reaction, collecting magnetic brown particles by using a magnet, washing the magnetic brown particles, and drying the magnetic brown particles to obtain magnetic ZrMOF;
dispersing magnetic ZrMOF in phosphate buffer solution, adding 2.5wt% glutaraldehyde water solution, stirring, separating particles by using a magnet, washing, putting the particles into the phosphate buffer solution, adding glutathione, a modified chitosan adsorbent and melamine, mixing on a shaking table at room temperature, separating a reaction product by using the magnet, and washing to obtain a composite adsorbent;
step (4) mixing the water-washed and pretreated fly ash of the garbage power plant with deionized water, adding sodium hydroxide, transferring to a sealed polytetrafluoroethylene reactor, performing microwave hydrothermal treatment under a nitrogen atmosphere, heating for reaction, adjusting the pH of the solution to 7.2-7.4, adding a composite adsorbent, stirring for reaction, and purifying to obtain purified fly ash; wherein the dosages of the sodium hydroxide and the composite adsorbent are respectively 10-20wt% and 3-10wt% of the total solid-liquid mixture of the fly ash of the waste power plant and the deionized water which are subjected to water washing pretreatment; heating reaction conditions: reacting for 1-2h at 200-220 ℃; stirring reaction time: 8-10h;
step (5) sintering the purified fly ash at a high temperature of 800-3000 ℃, cooling to room temperature, and ball-milling to 200-500 meshes to obtain sintered fly ash; ball milling waste ceramic powder, cement, feldspar and clay respectively to 200-500 meshes for later use;
adding the multiwall carbon nanotubes and the magnetic nickel nanoparticles into aluminum sol, stirring, dripping hydrochloric acid to adjust the pH value to 4, then adding 5wt% of sodium dodecyl sulfate aqueous solution, and continuing stirring to obtain suspension; adding sintered fly ash and ground waste ceramic powder into the suspension, stirring, adding ground cement, ground feldspar, ground clay, FS-20 Pasteur water reducer, sodium tripolyphosphate, polyvinyl alcohol and water, and stirring uniformly to obtain mixed slurry; mixing and stirring the mixed slurry and the foam, casting, forming, drying, sintering and cooling the dried sample to obtain ceramic; wherein, sintering conditions are as follows: heating the dried sample to 1000-1200 ℃ at a heating rate of 5 ℃/min for primary sintering, and preserving heat for 1.5-2.5h; then heating to 1350-1450 ℃ at a heating rate of 5 ℃/min, hot-pressing and sintering under constant pressure of 5-50MPa, and preserving heat for 1.5-2.5h.
2. The ceramic produced by fly ash from a waste power plant according to claim 1, wherein in the step (1), mixing and stirring time is as follows: 1.5-2.5h; washing conditions of the gel obtained by the reaction: washing with deionized water for 3-5 times; crosslinking time: 30-40min; drying conditions: drying at 50-60deg.C to constant weight.
3. The ceramic made of fly ash of a waste power plant according to claim 1, wherein in the step (2), the preparation method of the silica-attached magnetic nanoparticles comprises: 9-18kg of nano Fe 3 O 4 Dispersing in a mixed solution formed by mixing double distilled water and ethanol according to the volume of 1:4, adding 100-200L of ammonia water and 21-42L of tetraethoxysilane, stirring for 12-16h at 40-50 ℃, collecting solid particles by using a magnet, washing by using ethanol, and drying at 140-160 ℃ to obtain the magnetic nano particles attached to silicon dioxide.
4. The ceramic produced from fly ash of a refuse-derived power plant according to claim 1, wherein in said step (2), the contents of the components in the mixture are as follows:ZrCl 4 3-6kg, 1.5-3kg of magnetic nano particles attached to silicon dioxide, 200-400L of N, N-dimethylformamide and 750-1500mL of double distilled water; the dosage ratio of the 2-amino terephthalic acid to the N, N-dimethylformamide is 2.35-4.7kg:100-200L; heating reaction conditions: reacting for 24-30h at 110-120 ℃; washing conditions: flushing with double distilled water for 3-5 times; drying temperature: 50-70 ℃.
5. The ceramic produced by fly ash from a waste power plant according to claim 1, wherein in the step (3), a phosphate buffer solution is used: the pH is 7.4, and the concentration is 0.1mol/L; the dosage ratio of the magnetic ZrMOF to the phosphate buffer solution is 1-2kg:100-200L; stirring time: 6-8h; washing liquid adopted in the washing is phosphate buffer solution; the dosage ratio of the phosphate buffer solution, the glutathione, the modified chitosan adsorbent and the melamine is 200-400L:5-10kg:3-6kg:0.5-2kg; mixing time on shaking table: 8-10h.
6. The ceramic produced by the fly ash of the waste power plant according to claim 1, wherein in the step (4), the method for water-washing pretreatment of the fly ash of the waste power plant comprises the following steps: adding 100-200kg of fly ash of a garbage power plant into 1000-2000L of deionized water, stirring at a rotation speed of 400-600r/min for 2-4h, filtering, repeating the above process for 2-3 times, and drying the filtered solid at 80-100 ℃ for 24-36h.
7. The ceramic produced by the fly ash of the waste power plant according to claim 1, wherein in the step (4), the solid-to-liquid ratio of the fly ash of the waste power plant pretreated by water washing to deionized water is 0.1-0.2kg/L; the purification method comprises the following steps: firstly, separating the composite adsorbent adsorbed with other substances by using a magnet, filtering the rest mixed solution, washing filter residues by using deionized water, and then drying.
8. The ceramic produced by the fly ash of a waste power plant according to claim 1, wherein in the step (6), the method for producing the foam comprises: mixing 0.3-1.5kg of hydroxyethyl cellulose, 0.4-2kg of foaming agent and 4-5kg of water, and stirring for 3-5min to obtain foam; the dosage ratio of the multiwall carbon nano tube, the magnetic nickel nano particles, the aluminum sol and the 5wt% sodium dodecyl sulfate aqueous solution is 1.38-2.25kg:2.25-6.75kg:30-60kg:3-8kg; the mass ratio of the sintered fly ash to the ground waste ceramic powder to the ground cement to the ground feldspar to the ground clay to the FS-20 basf water reducer to the sodium tripolyphosphate to the polyvinyl alcohol to the water is 30-50:25-40:10-15:5-20:5-10:1.5-4:1.5-4:6-15:40-60; the amount of foam is 10-30wt% of the solid content of the mixed slurry.
9. The ceramic produced by fly ash from a waste power plant according to claim 1, wherein in the step (6), the drying condition after casting molding is as follows: naturally drying for 12-15h, and drying at 60-90deg.C for 6-10h.
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