CN114956784B - Ceramic membrane and preparation method thereof - Google Patents
Ceramic membrane and preparation method thereof Download PDFInfo
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- CN114956784B CN114956784B CN202210523672.5A CN202210523672A CN114956784B CN 114956784 B CN114956784 B CN 114956784B CN 202210523672 A CN202210523672 A CN 202210523672A CN 114956784 B CN114956784 B CN 114956784B
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- ceramic membrane
- household garbage
- bottom slag
- polyvinyl alcohol
- garbage incineration
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- 239000000919 ceramic Substances 0.000 title claims abstract description 200
- 239000012528 membrane Substances 0.000 title claims abstract description 171
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 239000002893 slag Substances 0.000 claims abstract description 112
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 88
- 238000005245 sintering Methods 0.000 claims abstract description 79
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 46
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 42
- 239000010703 silicon Substances 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 238000003825 pressing Methods 0.000 claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 20
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 76
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 76
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 38
- 239000002245 particle Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 19
- 238000005303 weighing Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 229910001593 boehmite Inorganic materials 0.000 claims description 10
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 6
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims 3
- 239000002994 raw material Substances 0.000 abstract description 18
- 238000002474 experimental method Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 65
- 238000001914 filtration Methods 0.000 description 38
- 239000011148 porous material Substances 0.000 description 33
- 230000000052 comparative effect Effects 0.000 description 32
- 238000000926 separation method Methods 0.000 description 31
- 230000000694 effects Effects 0.000 description 26
- 239000011651 chromium Substances 0.000 description 19
- 229910021645 metal ion Inorganic materials 0.000 description 18
- 239000010949 copper Substances 0.000 description 17
- 230000004907 flux Effects 0.000 description 16
- 230000001070 adhesive effect Effects 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- 239000000853 adhesive Substances 0.000 description 13
- 239000011133 lead Substances 0.000 description 13
- 239000000126 substance Substances 0.000 description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 150000002500 ions Chemical class 0.000 description 9
- 230000008901 benefit Effects 0.000 description 8
- 229910001385 heavy metal Inorganic materials 0.000 description 8
- 239000010842 industrial wastewater Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 238000012216 screening Methods 0.000 description 6
- 238000004876 x-ray fluorescence Methods 0.000 description 6
- 239000011363 dried mixture Substances 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000010183 spectrum analysis Methods 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 4
- 239000010881 fly ash Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000004075 wastewater filtration Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 208000001647 Renal Insufficiency Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 208000007502 anemia Diseases 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- -1 heavy metal ions Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 201000006370 kidney failure Diseases 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 230000005976 liver dysfunction Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 231100000189 neurotoxic Toxicity 0.000 description 1
- 230000002887 neurotoxic effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 208000016261 weight loss Diseases 0.000 description 1
Classifications
-
- 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
- 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
- C04B33/1355—Incineration residues
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/1305—Organic additives
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/131—Inorganic additives
-
- 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
- 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
- C04B33/1328—Waste materials; Refuse; Residues without additional clay
-
- 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
- C04B33/00—Clay-wares
- C04B33/24—Manufacture of porcelain or white ware
-
- 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
-
- 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
- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- 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
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The invention discloses a ceramic membrane and a preparation method thereof, wherein the preparation method of the ceramic membrane comprises the following steps: mixing: incineration of household garbage with bottom slag and Al 2 O 3 Mixing and grinding an organic solvent, a binder and a pore-forming agent to form a mixture; pressing: pressing the mixture into a sheet; sintering: sintering the flake at 900-1050 ℃ to obtain the ceramic film. The preparation method of the ceramic membrane uses the life incineration bottom slag and Al 2 O 3 As a raw material, the preparation cost of the ceramic membrane is lower, and experiments prove that when the molar ratio of silicon to aluminum in the mixture is 2:1, the ratio of the household garbage incineration bottom slag in the mass of the whole ceramic membrane can reach 81%, the utilization rate of the household garbage incineration bottom slag is higher, the problem of recycling the household garbage incineration bottom slag can be effectively solved, and the production cost of the ceramic membrane is greatly reduced.
Description
Technical Field
The invention relates to the technical field of ceramic membrane preparation, in particular to a ceramic membrane and a preparation method thereof.
Background
The ceramic membrane has excellent coagulation, precipitation and entrapment capacity, has the advantages of easy cleaning, stable performance, high mechanical strength, acid and alkali corrosion resistance, strong heat resistance and the like, and is widely applied to the food and beverage industry and industrial filtration.
In the related art, pure chemical or industrial reagents are used as raw materials for preparing the ceramic membrane, but pure substances have high cost and low sintering activity, and generally require sintering temperature of more than 1500 ℃, so that the ceramic membrane has high energy consumption and high production cost.
Disclosure of Invention
The embodiment of the invention discloses a ceramic membrane and a preparation method thereof.
In order to achieve the above object, in a first aspect, an embodiment of the present invention discloses a method for preparing a ceramic film, including the steps of:
mixing: incineration of household garbage with bottom slag and Al 2 O 3 Mixing and grinding an organic solvent, a binder and a pore-forming agent to form a mixture;
pressing: pressing the mixture into a sheet;
sintering: sintering the sheet at 900-1050 ℃ to obtain the ceramic membrane.
The preparation method of the ceramic membrane provided by the embodiment of the invention comprises the steps of incinerating household garbage to bottom slag and Al 2 O 3 Mixing and grinding the organic solvent, the adhesive and the pore-forming agent, pressing to form a sheet so as to facilitate sintering, and decomposing the organic solvent, the adhesive and the pore-forming agent to generate gas in the sintering process at 900-1050 ℃ so that dense pores are generated on the surface and the inside of the sintered ceramic membrane, thereby When the method is applied to wastewater filtration, ions can be intercepted on the surface of the ceramic membrane, and meanwhile, the ceramic membrane has a certain adsorption effect on metal ions due to the effect of the surface charge of the ceramic membrane, so that the interception effect on the metal ions is further improved. Because the household garbage incineration bottom slag is used as the raw material, the preparation cost of the ceramic membrane is lower. In addition, compared with the method for preparing the ceramic membrane by using pure substances (the pure substances can comprise alumina and silica) as raw materials, when the household garbage incineration bottom slag is used as the raw materials for preparing the ceramic membrane, the sintering temperature is lower, and the ceramic membrane can be formed by sintering at the temperature below 1050 ℃, so that energy saving in the process of preparing the ceramic membrane is realized.
As the content of general silicon in the household incineration bottom slag is more and the content of aluminum is less, if the content of aluminum is less, the pore diameter of the prepared ceramic membrane is too small, and the filtration efficiency of the ceramic membrane is low, the embodiment adds Al 2 O 3 The content of silicon and aluminum is balanced, so that the pore diameter of the prepared ceramic membrane is better and proper, and the ceramic membrane has higher filtering efficiency.
As an alternative embodiment, in an embodiment of the first aspect of the present invention, before the step of mixing, the preparation method further comprises the steps of:
Component analysis: carrying out component analysis on the household garbage incineration bottom slag to obtain the molar quantity of silicon and aluminum in the household garbage incineration bottom slag;
weighing Al 2 O 3 : weighing Al 2 O 3 So that the molar quantity of silicon in the household garbage incineration bottom slag, the household garbage incineration bottom slag and the Al 2 O 3 The ratio of the sum of the molar amounts of the aluminum is 1:1 to 3:1.
The molar quantity of silicon and aluminum in the household garbage incineration bottom slag is obtained by carrying out component analysis on the household garbage incineration bottom slag, so that the added Al can be obtained by calculation 2 O 3 Such that the ratio of the molar amount of silicon to the sum of the molar amounts of aluminum is 1:1 to 3:1. The preparation method comprises the steps of controlling the ratio of the molar quantity of silicon to the molar quantity of aluminum to be 1:1-3:1, controlling the ratio of silicon to aluminum to be in a reasonable rangeThe resulting ceramic membrane can have a suitable pore size. When the ratio of the sum of the molar quantity of silicon and the molar quantity of aluminum is less than 1:1, namely the molar quantity of silicon is too small and the molar quantity of aluminum is too large, the pore diameter of the prepared ceramic membrane is smaller, the pure water flux is smaller, and the filtering efficiency is low. When the ratio of the sum of the molar quantity of silicon and the molar quantity of aluminum is more than 3:1, namely the molar quantity of silicon is too high and the molar quantity of aluminum is too low, the pore diameter of the prepared ceramic membrane is too large, and the ceramic membrane cannot effectively intercept some ions and has poor filtering effect.
As an alternative embodiment, in an embodiment of the first aspect of the present invention, before the step of mixing, the preparation method further comprises the steps of:
grinding: grinding the household garbage incineration bottom slag until the particle size of the particles of the household garbage incineration bottom slag is smaller than 325 meshes.
The household garbage incineration bottom slag is ground until the particle size of the particles of the household garbage incineration bottom slag is smaller than 325 meshes, so that the household garbage incineration bottom slag particles are fine, and the household garbage incineration bottom slag particles can be uniformly mixed with other components in the mixing step, thereby being beneficial to improving the structural uniformity of the sintered ceramic membrane.
As an alternative embodiment, in the embodiment of the first aspect of the present invention, the Al 2 O 3 Is gamma-Al 2 O 3 The mixing step is preceded by the steps of:
preparation of gamma-Al 2 O 3 : sintering boehmite in a muffle furnace at 600-650 ℃ to form gamma-Al 2 O 3 。
Due to gamma-Al 2 O 3 Has the advantages of porous property, large surface area, good adsorption performance, good thermal stability and the like, thus utilizing gamma-Al 2 O 3 The prepared ceramic membrane also has the advantages of porosity and better filtering performance.
As an alternative embodiment, in the example of the first aspect of the present invention, the organic solvent includes at least one of methanol, ethanol, formaldehyde, and acetaldehyde; or,
The adhesive comprises at least one of a polyvinyl alcohol solution, a carboxymethyl cellulose solution and a polyethylene glycol solution; or,
the pore-forming agent is calcium carbonate.
The dissolution of each component can be improved by the organic solvent, the adhesion effect is realized by the adhesive, and the prepared ceramic membrane has the porosity by the pore-forming agent so as to realize the filtration effect.
As an alternative embodiment, in the embodiment of the first aspect of the present invention, when the binder includes a polyvinyl alcohol solution, the mixing step further includes:
preparing a polyvinyl alcohol solution: adding deionized water into polyvinyl alcohol particles, and stirring at 80-100 ℃ until the polyvinyl alcohol particles are dissolved to prepare a polyvinyl alcohol solution, wherein the polyvinyl alcohol solution comprises 5-10wt% of polyvinyl alcohol.
The polyvinyl alcohol particles are dissolved at 80-100 ℃ to form a polyvinyl alcohol solution, and the polyvinyl alcohol solution can be ensured to have proper viscosity by limiting the mass percentage of the polyvinyl alcohol in the polyvinyl alcohol solution to 5-10 wt%.
In an alternative embodiment, in the embodiment of the first aspect of the present invention, the polyvinyl alcohol solution has a mass greater than that of the household garbage incineration bottom slag and the Al 2 O 3 10wt% of the sum of the masses.
By limiting the mass of the polyvinyl alcohol solution to be larger than that of the household garbage incineration bottom slag and Al 2 O 3 The adhesive effect of the polyvinyl alcohol solution can be fully realized by 10 weight percent of the sum of the mass. Illustratively, the polyvinyl alcohol solution has the mass of household garbage incineration bottom slag and Al 2 O 3 10wt%, 20wt%, 30wt% of the sum of the masses of (a) and (b), etc.
As an alternative embodiment, in an example of the first aspect of the present invention, before the step of pressing, the preparation method comprises the steps of:
and (3) drying: the mixture is dried at 60-70 ℃.
Drying the mixture at a lower temperature prior to the pressing step can remove the organic solvent from the mixture and avoid the organic solvent evaporating too fast during sintering to affect the formation of the ceramic membrane and the pore size of the ceramic membrane.
As an alternative embodiment, in the example of the first aspect of the present invention, in the step of pressing, the pressing pressure is 20MPa to 30MPa, and the holding time is 1min to 3min. By controlling the pressing pressure to be 20-30 MPa, the sheet can be pressed without cracking. When the pressure is more than 30MPa, the pressure is too high, so that the sheet is easy to crack, and when the pressure is less than 20MPa, the pressure is too low, and the press molding is difficult. By controlling the dwell time to be 1min to 3min, the pressed sheet can be ensured not to crack.
In a second aspect, the invention also discloses a ceramic membrane prepared by the preparation method of the ceramic membrane in the first aspect. The ceramic membrane has low cost and excellent filtering effect.
Compared with the prior art, the embodiment of the invention has the beneficial effects that:
the ceramic membrane and the preparation method thereof provided by the embodiment burn household garbage with bottom slag and Al 2 O 3 The organic solvent, the adhesive and the pore-forming agent are mixed and ground, and are pressed to form a sheet so as to be convenient for sintering, and in the sintering process at the temperature of 900-1050 ℃, the organic solvent, the adhesive and the pore-forming agent are decomposed to generate gas, so that dense holes are generated on the surface and inside of the sintered ceramic membrane, ions can be intercepted on the surface of the ceramic membrane when the ceramic membrane is applied to wastewater filtration, and meanwhile, the ceramic membrane has a certain adsorption effect on metal ions due to the effect of the surface charge of the ceramic membrane, so that the interception effect on the metal ions is further improved. Because the household garbage incineration bottom slag is used as the raw material, the preparation cost of the ceramic membrane is lower. In addition, compared with the method for preparing the ceramic film by adopting pure substances (the pure substances can comprise alumina and silicon oxide) as raw materials and adopting household garbage incineration bottom slag as raw materials, the sintering temperature is lower, and the ceramic film can be formed by sintering at the temperature below 1050 ℃ so as to realize the preparation Energy is saved in the process of the ceramic membrane.
As the content of general silicon in the household incineration bottom slag is more and the content of aluminum is less, if the content of aluminum is less, the pore diameter of the prepared ceramic membrane is too small, and the filtration efficiency of the ceramic membrane is low, the embodiment adds Al 2 O 3 The content of silicon and aluminum is balanced, so that the pore diameter of the prepared ceramic membrane is better and proper, and the ceramic membrane has higher filtering efficiency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, 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 microscope image of a ceramic film according to a first embodiment;
FIG. 2 is a scanning electron microscope image of a ceramic film according to a second embodiment;
FIG. 3 is a graph showing the effect of the ceramic membrane according to the second embodiment on the separation of metal ions in a single metal component solution;
fig. 4 is a graph showing the effect of the ceramic membrane provided in the second embodiment on the separation of metal ions in the mixed metal component solution;
FIG. 5 is a graph showing permeation flux and Cr-pair of six-cycle filtration of a ceramic membrane according to the second embodiment 3+ Is a graph of separation effect of (2);
FIG. 6 is a scanning electron microscope image of a ceramic film provided in the third embodiment;
FIG. 7 is a scanning electron microscope image of a ceramic film according to a fourth embodiment;
FIG. 8 is a scanning electron microscope image of the ceramic film provided in this comparative example one;
FIG. 9 shows the Cr-to-Cr ratio of the ceramic films of the first to fourth embodiments and the first comparative example 3+ Separating a result graph;
FIG. 10 shows ceramic films according to the first to fourth embodiments and the first comparative exampleFor Cu 2+ Separating a result graph;
FIG. 11 is a graph showing the pure water flux of the ceramic membranes of the second example and the first comparative example.
Detailed Description
In the present invention, the terms "upper", "lower", "left", "right", "front", "rear", "top", "bottom", "inner", "outer", "middle", "vertical", "horizontal", "lateral", "longitudinal" and the like indicate an azimuth or a positional relationship based on that shown in the drawings. These terms are only used to better describe the present invention and its embodiments and are not intended to limit the scope of the indicated devices, elements or components to the particular orientations or to configure and operate in the particular orientations.
Also, some of the terms described above may be used to indicate other meanings in addition to orientation or positional relationships, for example, the term "upper" may also be used to indicate some sort of attachment or connection in some cases. The specific meaning of these terms in the present invention will be understood by those of ordinary skill in the art according to the specific circumstances.
Furthermore, the terms "mounted," "configured," "provided," "connected," and "connected" are to be construed broadly. For example, it may be a fixed connection, a removable connection, or a unitary construction; may be a mechanical connection, or an electrical connection; may be directly connected, or indirectly connected through intervening media, or may be in internal communication between two devices, elements, or components. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
Furthermore, the terms "first," "second," and the like, are used primarily to distinguish between different devices, elements, or components (the particular species and configurations may be the same or different), and are not used to indicate or imply the relative importance and number of devices, elements, or components indicated. Unless otherwise indicated, the meaning of "a plurality" is two or more.
Current rapid industrialization and urbanization and certain offensive emissions result in the emission of wastewater containing large amounts of heavy metals (e.g., lead, chromium, nickel, copper, etc.) into the environment, posing a threat to the ecosystem and human health.
For example, the leather industry produces approximately 3 x 10 per year 8 Ton of Cr-containing 3+ Low concentration of Cr 3+ High concentrations of Cr, which can lead to diabetes or coronary artery disease 3+ Can result in weight loss, anemia, renal failure, liver dysfunction, etc. If Cr 3+ Oxidized to Cr 6+ With more serious consequences.
Waste water containing heavy metals such as copper, lead and nickel, especially Cu in large amounts, is produced in the manufacturing industries of batteries, paints, fertilizers, automobile parts and the like 2+ Copper is a neurotoxic substance, and excessive Cu 2+ The food can be taken into fish and aquatic products by bioaccumulation, and can be taken into human body if excessive Cu is taken 2+ It may lead to Alzheimer's disease, dysreading or nausea. Lead and nickel are also highly toxic at very low concentrations. Thus, there is a need for filtering industrial wastewater to separate heavy metal ions from the wastewater.
When researching the technology of filtering and separating industrial wastewater, the inventor synthesizes ceramic membranes by taking silicon oxide and aluminum oxide as raw materials to realize the separation of heavy metal ions in the industrial wastewater, however, the pure substance is adopted to synthesize the ceramic membranes, the pure substance has very high price, and the economic benefit is difficult to meet when the industrial wastewater is filtered and separated, so the inventor further considers how to filter and separate the industrial wastewater while meeting the economic benefit, namely, the economic benefit and the environmental protection are simultaneously considered. The inventors found that the household garbage is mainly treated by incineration, a large amount of household garbage incineration bottom slag is accumulated along with the gradual increase of the incineration amount of the household garbage, and found that the household garbage incineration bottom slag contains a large amount of silicon and aluminum. Therefore, the inventor explores a method for preparing a ceramic membrane by utilizing household garbage incineration bottom slag, so as to separate heavy metals in industrial wastewater through the ceramic membrane and realize both economic benefit and environmental protection.
The embodiment of the invention provides a preparation method of a ceramic membrane, which comprises the following steps:
mixing: incineration of household garbage with bottom slag and Al 2 O 3 Mixing and grinding an organic solvent, a binder and a pore-forming agent to form a mixture;
pressing: pressing the mixture into a sheet;
sintering: sintering the flake at 900-1050 ℃ to obtain the ceramic film.
The preparation method of the ceramic membrane provided by the embodiment of the invention comprises the steps of incinerating household garbage to bottom slag and Al 2 O 3 The organic solvent, the adhesive and the pore-forming agent are mixed and ground, and are pressed to form a sheet so as to be convenient for sintering, and in the sintering process at the temperature of 900-1050 ℃, the organic solvent, the adhesive and the pore-forming agent are decomposed to generate gas, so that dense holes are generated on the surface and inside of the sintered ceramic membrane, and ions, particularly heavy metal ions, in the wastewater can be efficiently filtered when the ceramic membrane is applied to the wastewater filtration. In addition, when the ceramic membrane filters wastewater, metal ions generate a bridging effect at the inlets of the holes of the ceramic membrane, so that the metal ions smaller than the aperture can be effectively separated, and the separation rate is improved. And after a period of filtration, the surface of the ceramic membrane can be polluted by the membrane due to concentration polarization, so that particles are accumulated on the surface of the ceramic membrane, and the separation rate can be improved.
Because the main component of the household incineration bottom slag is SiO 2 And Al 2 O 3 Silicate and aluminosilicate are formed after sintering, and because of the specificity of the crystal structure, cations are needed to neutralize the crystal, ion exchange can occur during filtering metal cations, the crystal structure is stabilized, and meanwhile, the separation rate of the ceramic membrane to heavy metal is improved.
In addition, the ceramic membrane surface presents electronegativity, so that the ceramic membrane has an adsorption effect on metal cations, and meanwhile, solutes in some wastewater can be deposited in pores due to electrostatic adsorption, so that the separation rate of the metal ions is further improved.
Compared with the method for preparing the ceramic membrane by using pure substances (the pure substances can comprise alumina and silica) as raw materials, when the household garbage incineration bottom slag is used as the raw materials, the household garbage incineration bottom slag also comprises various metal oxides and other substances, so that the household garbage incineration bottom slag is a mixed system of various components, the sintering temperature is lower, the ceramic membrane can be formed by sintering at the temperature below 1050 ℃, and the energy saving in the process of preparing the ceramic membrane is realized.
As the content of general silicon in the household incineration bottom slag is more and the content of aluminum is less, if the content of aluminum is less, the pore diameter of the prepared ceramic membrane is too small, and the filtration efficiency of the ceramic membrane is low, the embodiment adds Al 2 O 3 The content of silicon and aluminum is balanced, so that the pore diameter of the prepared ceramic membrane is better and proper, and the ceramic membrane has higher filtering efficiency.
Optionally, before the step of mixing, the preparation method further comprises the steps of:
component analysis: carrying out component analysis on the household garbage incineration bottom slag to obtain the molar quantity of silicon and aluminum in the household garbage incineration bottom slag;
weighing Al 2 O 3 : weighing Al 2 O 3 So that the molar quantity of silicon in the household garbage incineration bottom slag is equal to that of the household garbage incineration bottom slag and Al 2 O 3 The ratio of the sum of the molar amounts of the aluminum is 1:1 to 3:1.
The molar quantity of silicon and aluminum in the household garbage incineration bottom slag is obtained by carrying out component analysis on the household garbage incineration bottom slag, so that the added Al can be obtained by calculation 2 O 3 Such that the ratio of the molar amount of silicon to the molar amount of aluminum is 1:1 to 3:1. The ratio of the molar quantity of silicon to the molar quantity of aluminum is controlled to be 1:1-3:1, and the proportion of the silicon to the aluminum is controlled to be in a reasonable range, so that the prepared ceramic membrane can have proper pore diameter. When the ratio of the molar amount of silicon to the molar amount of aluminum is less than 1:1, i.e. siliconWhen the molar quantity of the ceramic membrane is too small and the molar quantity of the aluminum is too large, the pore diameter of the prepared ceramic membrane is smaller, the pure water flux is smaller, and the filtering efficiency is low. When the ratio of the molar quantity of silicon to the molar quantity of aluminum is more than 3:1, namely the molar quantity of silicon is too high and the molar quantity of aluminum is too low, the pore diameter of the prepared ceramic membrane is too large, and the ceramic membrane cannot effectively intercept some ions and has poor filtering effect. In addition, experiments show that when the molar ratio of silicon to aluminum in the mixture is 2:1, the ratio of the household garbage incineration bottom slag in the mass of the whole ceramic membrane can reach 81%, the utilization rate of the household garbage incineration bottom slag is high, the problem of recycling the household garbage incineration bottom slag can be effectively solved, and the production cost of the ceramic membrane is greatly reduced.
Optionally, the components of the household garbage incineration bottom slag can be analyzed by adopting an X-ray fluorescence spectrum, and of course, the components of the household garbage incineration bottom slag can also be analyzed by adopting other component analysis methods.
The ratio of the molar amount of silicon to the molar amount of aluminum is 1:1 to 3:1, inclusive of any point value within the range of the ratio, and the ratio of the molar amount of silicon to the molar amount of aluminum is 1:1, 1:1.5, 1:2, 1:2.5, 1:3, or the like, for example.
Optionally, before the step of mixing, the preparation method further comprises the steps of:
grinding: grinding the household garbage incineration bottom slag until the particle size of the household garbage incineration bottom slag particles is smaller than 325 meshes.
The household garbage incineration bottom slag is ground until the particle size of the household garbage incineration bottom slag particles is smaller than 325 meshes, and the particles of the household garbage incineration bottom slag are fine, so that the household garbage incineration bottom slag can be uniformly mixed with other components in the mixing step, and the structural uniformity of the sintered ceramic membrane is improved.
Alternatively, al 2 O 3 Is gamma-Al 2 O 3 The mixing step is preceded by the steps of:
preparation of gamma-Al 2 O 3 : sintering boehmite in a muffle furnace at 600-650 ℃ to form gamma-Al 2 O 3 . Due to gamma-Al 2 O 3 Has a porous nature, Large surface area, good adsorption performance, good thermal stability, etc., thus utilizing gamma-Al 2 O 3 The prepared ceramic membrane also has the advantages of porosity and better filtering performance.
In the preparation of gamma-Al 2 O 3 In the step (a), the temperature rising rate of the boehmite in the muffle furnace can be 5-10 ℃ per minute, and the sintering time can be 2-3 hours. The heating rate of sintering the boehmite in the muffle furnace is 5-10 ℃ per minute, including any point value within the heating rate range, for example, the heating rate can be 5-3 hours, including any point value within the time range, for example, 2 hours, 2.5 hours, 3 hours, etc., and the heating rate can be 5-6 ℃ per minute, 7 ℃/min, 8 ℃/min, 9 ℃/min, 10 ℃/min, etc.
Optionally, the organic solvent comprises at least one of methanol, ethanol, formaldehyde, and acetaldehyde; alternatively, the binder comprises at least one of a polyvinyl alcohol solution, a carboxymethyl cellulose solution and a polyethylene glycol solution; alternatively, the pore former is calcium carbonate. The dissolution of each component can be improved by the organic solvent, the adhesion effect is realized by the adhesive, and the prepared ceramic membrane has the porosity by the pore-forming agent so as to realize the filtration effect. When calcium carbonate is used as pore-forming agent, the calcium carbonate and SiO in the household garbage incineration bottom slag 2 And Al 2 O 3 The chemical reaction occurs, and the reaction formula is as follows:
2CaCO 3 +Al 2 O 3 +SiO 2 →Ca 2 Al 2 O 7 +2CO 2
wherein, calcium in the calcium carbonate can play a grafting role, and compared with the method which adopts starch as a pore-forming agent, the prepared ceramic film is not easy to crack and has better forming effect. Furthermore, caCO 3 、Al 2 O 3 、SiO 2 CO is generated when chemical reaction occurs 2 The gas can make the ceramic membrane have porosity so as to form better filtering effect. Optionally, when the binder comprises a polyvinyl alcohol solution, the mixing step may further comprise:
preparing a polyvinyl alcohol solution: deionized water is added into the polyvinyl alcohol particles, and the polyvinyl alcohol particles are stirred at the temperature of 80-100 ℃ until the polyvinyl alcohol particles are dissolved, so that a polyvinyl alcohol solution is prepared, wherein the mass percent of the polyvinyl alcohol in the polyvinyl alcohol solution is 5-10 wt%.
The polyvinyl alcohol particles are dissolved at 80-100 ℃ to form a polyvinyl alcohol solution, and the polyvinyl alcohol solution can be ensured to have proper viscosity by limiting the mass percentage of the polyvinyl alcohol in the polyvinyl alcohol solution to 5-10 wt%.
The dissolution temperature of the polyvinyl alcohol particles may be any value in the range of 80 to 100 ℃, for example, the dissolution temperature of the polyvinyl alcohol particles is 80 ℃, 90 ℃, 100 ℃, etc., and the mass percentage of the polyvinyl alcohol in the polyvinyl alcohol solution is 5 to 10wt% inclusive of any value in the range of the mass percentage, for example, the mass percentage of the polyvinyl alcohol in the polyvinyl alcohol solution is 5 to 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, etc.
Optionally, the mass of the polyvinyl alcohol solution is larger than that of the household garbage incineration bottom slag and Al 2 O 3 10wt% of the sum of the masses. By limiting the mass of the polyvinyl alcohol solution to be larger than that of the household garbage incineration bottom slag and Al 2 O 3 The adhesive effect of the polyvinyl alcohol solution can be fully realized by 10 weight percent of the sum of the mass. Illustratively, the polyvinyl alcohol solution has the mass of household garbage incineration bottom slag and Al 2 O 3 10wt%, 20wt%, 30wt% of the sum of the masses of (a) and (b), etc.
Optionally, before the step of pressing, the preparation method comprises the steps of:
and (3) drying: the mixture is dried at 60-70 ℃.
Drying the mixture at a lower temperature prior to the pressing step can remove the organic solvent from the mixture and avoid the organic solvent evaporating too fast during sintering to affect the formation of the ceramic membrane and the pore size of the ceramic membrane.
The drying of the mixture at 60 to 70 ℃ includes any point value within the drying temperature, and the drying temperature is, for example, 60 ℃, 65 ℃, 70 ℃.
Optionally, in the step of pressing, the pressing pressure is 20MPa to 30MPa, and the holding time is 1min to 3min. By controlling the pressing pressure to be 20-30 MPa, the sheet can be pressed without cracking. When the pressure is more than 30MPa, the pressure is too high, so that the sheet is easy to crack, and when the pressure is less than 20MPa, the pressure is too low, and the press molding is difficult. By controlling the dwell time to be 1min to 3min, the pressed sheet can be ensured not to crack.
The pressing pressure is 20MPa to 30MPa, including any point value within the pressure range, and the pressing pressure is, for example, 20MPa, 23MPa, 25MPa, 28MPa, 30MPa, or the like. The dwell time is 1min to 3min including any point value within the time range, illustratively, 1min, 2min, 3min, etc.
Optionally, the step of sintering comprises:
and (3) placing the sheet into a muffle furnace, and sintering at 900-1050 ℃ for 2-4 hours at a heating rate of less than 10 ℃/min to obtain the ceramic membrane. By controlling the sintering at a temperature rising rate of less than 10 ℃/min, cracking of the ceramic film due to too fast a temperature rising rate can be avoided. By controlling the sintering time to be 2-4 h, the organic solvent, the adhesive and the pore-forming agent can be fully volatilized, so that the ceramic membrane has uniform and dense pores to improve the filtering performance, and meanwhile, the forming effect of the ceramic membrane can be ensured. When the sintering time is longer than 4 hours, the ceramic membrane is easy to crack due to overlong sintering time, and when the sintering time is shorter than 2 hours, the ceramic membrane has poor forming effect.
The sintering time of 2h to 4h includes any point value in the time range, for example, the sintering time is 2h, 3h, 4h, and the like.
The embodiment of the invention also discloses a ceramic membrane, which is prepared by adopting the preparation method of the ceramic membrane. The ceramic membrane has low cost and excellent filtering effect.
The technical scheme of the invention will be further described with reference to the examples and the accompanying drawings.
Example 1
The embodiment of the invention discloses a preparation method of a ceramic membrane, which comprises the following steps:
grinding: crushing the household garbage incineration bottom slag by a crusher and grinding by a planetary grinder, and screening by a 325-mesh filter screen to obtain uniform and fine household garbage incineration bottom slag particles.
Component analysis: adopting X-ray fluorescence spectrum analysis to the household garbage incineration bottom slag to obtain the molar quantity of silicon and aluminum in the household garbage incineration bottom slag;
preparation of gamma-Al 2 O 3 : sintering boehmite in a muffle furnace at a sintering rate of 5 ℃/min for 3 hours at 650 ℃ to obtain gamma-Al 2 O 3 。
Weighing gamma-Al 2 O 3 : weighing a certain amount of gamma-Al 2 O 3 So that the molar quantity of silicon in the household garbage incineration bottom slag is equal to that of the household garbage incineration bottom slag and gamma-Al 2 O 3 The ratio of the sum of the molar amounts of aluminum in (2) to (1).
Preparing a polyvinyl alcohol solution: 5g of 1788 type polyvinyl alcohol particles are added into 95g of deionized water, and the mixture is magnetically stirred for 1h at 80 ℃ to obtain a polyvinyl alcohol solution with the mass percentage of 5 wt%.
Mixing: incineration of ground household garbage bottom slag and gamma-Al 2 O 3 Adding into a mortar, adding absolute ethyl alcohol, 5wt% polyvinyl alcohol solution and calcium carbonate, grinding and mixing uniformly to obtain a mixture. Wherein, the added polyvinyl alcohol solution with the weight percentage of 5 percent is the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the mass of the added calcium carbonate is the mass of the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the masses.
And (3) drying: the mixture is dried at 60-70 ℃.
Pressing: the dried mixture was tabletted in an electric tablet press using a die having a diameter of 22mm under a pressure of 20MPa for a dwell time of 1min to obtain a sheet.
Sintering: and sintering the sheet in a muffle furnace for 3 hours at 900 ℃ at a heating rate of 5 ℃/min to obtain the ceramic membrane.
As shown in fig. 1, this embodiment also discloses a ceramic membrane, which is prepared by using the preparation method of the ceramic membrane.
Example two
The second embodiment of the invention discloses a preparation method of a ceramic membrane, which comprises the following steps:
grinding: crushing the household garbage incineration bottom slag by a crusher and grinding by a planetary grinder, and screening by a 325-mesh filter screen to obtain uniform and fine household garbage incineration bottom slag particles.
Component analysis: adopting X-ray fluorescence spectrum analysis to the household garbage incineration bottom slag to obtain the molar quantity of silicon and aluminum in the household garbage incineration bottom slag;
preparation of gamma-Al 2 O 3 : sintering boehmite in a muffle furnace at a sintering rate of 5 ℃/min for 3 hours at 650 ℃ to obtain gamma-Al 2 O 3 。
Weighing gamma-Al 2 O 3 : weighing a certain amount of gamma-Al 2 O 3 So that the molar quantity of silicon in the household garbage incineration bottom slag is equal to that of the household garbage incineration bottom slag and gamma-Al 2 O 3 The ratio of the sum of the molar amounts of aluminum in (2) to (1).
Preparing a polyvinyl alcohol solution: 5g of 1788 type polyvinyl alcohol particles are added into 95g of deionized water, and the mixture is magnetically stirred for 1h at 80 ℃ to obtain a polyvinyl alcohol solution with the mass percentage of 5 wt%.
Mixing: incineration of ground household garbage bottom slag and gamma-Al 2 O 3 Adding into a mortar, adding absolute ethyl alcohol, 5wt% polyvinyl alcohol solution and calcium carbonate, grinding and mixing uniformly to obtain a mixture. Wherein, the added polyvinyl alcohol solution with the weight percentage of 5 percent is the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the mass of the added calcium carbonate is the mass of the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the masses.
And (3) drying: the mixture is dried at 60-70 ℃.
Pressing: the dried mixture was tabletted in an electric tablet press using a die having a diameter of 22mm under a pressure of 20MPa for a dwell time of 1min to obtain a sheet.
Sintering: and sintering the sheet in a muffle furnace for 3 hours at 950 ℃ at a heating rate of 5 ℃/min to obtain the ceramic membrane.
As shown in fig. 2, this embodiment also discloses a ceramic membrane, which is prepared by using the preparation method of the ceramic membrane.
The test shows that the pore diameter of the ceramic membrane is 0.5-1.5 mu m, the porosity is 40-50%, and the pure water flux is 215-322 kg/m under the pressure of 0.3bar 2 H. Therefore, the ceramic membrane has smaller pore diameter, can be applied to filtering heavy metal ions in wastewater, and has larger porosity, so that better separation rate and better filtering efficiency can be realized.
The ceramic membrane is used for testing the separation rate of metal ions in a single-component metal ion solution, and specifically, the ceramic membrane is used for testing Cu with initial concentration of 100mg/L 2+ Pb solution with initial concentration of 100mg/L 2+ Solution, cr with initial concentration of 100mg/L 3+ Solution, ni with initial concentration of 100mg/L 2+ Filtering the solution under a pressure of 0.3bar and Cu 2+ 、Pb 2 + 、Cr 3+ 、Ni 2+ As shown in FIG. 3, the separation rate test results of the ceramic film against Cu are shown in FIG. 3 2+ 、Pb 2+ 、Cr 3+ All have better separation rate, especially for Pb 2+ The separation rate of (2) can reach 99%.
The separation rate of metal ions in the metal ion solution of various components is tested by adopting the ceramic membrane, in particular, cu with the initial concentration of 100mg/L is adopted by adopting the ceramic membrane 2+ 、Pb 2+ 、Cr 3+ 、Ni 2+ Filtering the mixed solution of (C) at a pressure of 0.3bar and Cu 2+ 、Pb 2+ 、Cr 3+ 、Ni 2+ As shown in FIG. 4, the separation rate test results of the ceramic film against Cu are shown in FIG. 4 2 + 、Pb 2+ The separation rate of (2) can reach 100%, for Cr 3+ The separation rate of the ceramic membrane can reach 87.94 percent, and the ceramic membrane can be used for Cu 2+ 、Pb 2+ 、Cr 3+ Has very good separation effect on Ni 2+ The separation rate of (2) can also reach 67.93%. In addition, the separation rate of the ceramic membrane for metal ions in the metal ion solution with multiple components is larger than that for the metal ion solution with single component, because the multiple metal ions can have competition or competitive adsorption during filtration, and the competition between the metal ions brings synergistic effect for separation, thereby improving the separation rate.
To test the recyclability of the ceramic film, 100mg/L of Cr was passed through the ceramic film 3+ Carrying out six-round circulating filtration on the solution, wherein hydrochloric acid and ultrapure water are adopted to clean the ceramic membrane after each filtration, and Cr is subjected to six-round circulating filtration 3+ The separation rate and the pure water flux were measured, and the measurement results are shown in fig. 5.
As can be seen from FIG. 5, after six cycles of cyclic filtration, cr is recovered 3+ The separation rate can reach 97.31 percent, and the permeation flux can still reach 200L/m 2 H, therefore, the ceramic membrane still has better separation effect and permeation flux after being reused for 6 times.
Example III
The third embodiment of the invention discloses a preparation method of a ceramic membrane, which comprises the following steps:
grinding: crushing the household garbage incineration bottom slag by a crusher and grinding by a planetary grinder, and screening by a 325-mesh filter screen to obtain uniform and fine household garbage incineration bottom slag particles.
Component analysis: adopting X-ray fluorescence spectrum analysis to the household garbage incineration bottom slag to obtain the molar quantity of silicon and aluminum in the household garbage incineration bottom slag;
preparation of gamma-Al 2 O 3 : sintering boehmite in a muffle furnace at a sintering rate of 5 ℃/min for 3 hours at 650 ℃ to obtain gamma-Al 2 O 3 。
Weighing gamma-Al 2 O 3 : weighing a certain amount of gamma-Al 2 O 3 So that the household garbage burns the silicon of the bottom slagMolar mass of (2) and household garbage incineration bottom slag and gamma-Al 2 O 3 The ratio of the sum of the molar amounts of aluminum in (2) to (1).
Preparing a polyvinyl alcohol solution: 5g of 1788 type polyvinyl alcohol particles are added into 95g of deionized water, and the mixture is magnetically stirred for 1h at 80 ℃ to obtain a polyvinyl alcohol solution with the mass percentage of 5 wt%.
Mixing: incineration of ground household garbage bottom slag and gamma-Al 2 O 3 Adding into a mortar, adding absolute ethyl alcohol, 5wt% polyvinyl alcohol solution and calcium carbonate, grinding and mixing uniformly to obtain a mixture. Wherein, the added polyvinyl alcohol solution with the weight percentage of 5 percent is the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the mass of the added calcium carbonate is the mass of the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the masses.
And (3) drying: the mixture is dried at 60-70 ℃.
Pressing: the dried mixture was tabletted in an electric tablet press using a die having a diameter of 22mm under a pressure of 20MPa for a dwell time of 1min to obtain a sheet.
Sintering: and sintering the sheet in a muffle furnace for 3 hours at the temperature of 1000 ℃ at the heating rate of 5 ℃/min to obtain the ceramic membrane.
As shown in fig. 6, this embodiment also discloses a ceramic membrane, which is prepared by using the preparation method of the ceramic membrane.
Example IV
The fourth embodiment of the invention discloses a preparation method of a ceramic membrane, which comprises the following steps:
grinding: crushing the household garbage incineration bottom slag by a crusher and grinding by a planetary grinder, and screening by a 325-mesh filter screen to obtain uniform and fine household garbage incineration bottom slag particles.
Component analysis: adopting X-ray fluorescence spectrum analysis to the household garbage incineration bottom slag to obtain the molar quantity of silicon and aluminum in the household garbage incineration bottom slag;
preparation of gamma-Al 2 O 3 : boehmite in muffleSintering in a furnace at 650 ℃ for 3 hours at a sintering rate of 5 ℃/min to obtain gamma-Al 2 O 3 。
Weighing gamma-Al 2 O 3 : weighing a certain amount of gamma-Al 2 O 3 So that the molar quantity of silicon in the household garbage incineration bottom slag is equal to that of the household garbage incineration bottom slag and gamma-Al 2 O 3 The ratio of the sum of the molar amounts of aluminum in (2) to (1).
Preparing a polyvinyl alcohol solution: 5g of 1788 type polyvinyl alcohol particles are added into 95g of deionized water, and the mixture is magnetically stirred for 1h at 80 ℃ to obtain a polyvinyl alcohol solution with the mass percentage of 5 wt%.
Mixing: incineration of ground household garbage bottom slag and gamma-Al 2 O 3 Adding into a mortar, adding absolute ethyl alcohol, 5wt% polyvinyl alcohol solution and calcium carbonate, grinding and mixing uniformly to obtain a mixture. Wherein, the added polyvinyl alcohol solution with the weight percentage of 5 percent is the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the mass of the added calcium carbonate is the mass of the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the masses.
And (3) drying: the mixture is dried at 60-70 ℃.
Pressing: the dried mixture was tabletted in an electric tablet press using a die having a diameter of 22mm under a pressure of 20MPa for a dwell time of 1min to obtain a sheet.
Sintering: and sintering the sheet in a muffle furnace for 3 hours at 1050 ℃ at a heating rate of 5 ℃/min to obtain the ceramic membrane.
As shown in fig. 7, this embodiment also discloses a ceramic membrane, which is prepared by using the preparation method of the ceramic membrane.
Comparative example one
The invention discloses a preparation method of a ceramic membrane, which comprises the following steps:
grinding: crushing the household garbage incineration bottom slag by a crusher and grinding by a planetary grinder, and screening by a 325-mesh filter screen to obtain uniform and fine household garbage incineration bottom slag particles.
Component analysis: adopting X-ray fluorescence spectrum analysis to the household garbage incineration bottom slag to obtain the molar quantity of silicon and aluminum in the household garbage incineration bottom slag;
preparation of gamma-Al 2 O 3 : sintering boehmite in a muffle furnace at a sintering rate of 5 ℃/min for 3 hours at 650 ℃ to obtain gamma-Al 2 O 3 。
Weighing gamma-Al 2 O 3 : weighing a certain amount of gamma-Al 2 O 3 So that the molar quantity of silicon in the household garbage incineration bottom slag is equal to that of the household garbage incineration bottom slag and gamma-Al 2 O 3 The ratio of the sum of the molar amounts of aluminum in (2) to (1).
Preparing a polyvinyl alcohol solution: 5g of 1788 type polyvinyl alcohol particles are added into 95g of deionized water, and the mixture is magnetically stirred for 1h at 80 ℃ to obtain a polyvinyl alcohol solution with the mass percentage of 5 wt%.
Mixing: incineration of ground household garbage bottom slag and gamma-Al 2 O 3 Adding into a mortar, adding absolute ethyl alcohol, 5wt% polyvinyl alcohol solution and calcium carbonate, grinding and mixing uniformly to obtain a mixture. Wherein, the added polyvinyl alcohol solution with the weight percentage of 5 percent is the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the mass of the added calcium carbonate is the mass of the household garbage incineration bottom slag and gamma-Al 2 O 3 10wt% of the sum of the masses.
And (3) drying: the mixture is dried at 60-70 ℃.
Pressing: the dried mixture was tabletted in an electric tablet press using a die having a diameter of 22mm under a pressure of 20MPa for a dwell time of 1min to obtain a sheet.
Sintering: and sintering the sheet in a muffle furnace for 3 hours at 1100 ℃ at a heating rate of 5 ℃/min to obtain the ceramic membrane.
As shown in fig. 7, this comparative example also discloses a ceramic membrane prepared by the above-mentioned ceramic membrane preparation method.
As shown in fig. 1, 2, and 6 to 8, scanning electron microscope images of the ceramic films of example one to example four and comparative example 1 are respectively shown, the sintering temperature of example one to example four is gradually increased from 900 ℃ to 1050 ℃, the pore diameter of the pores of the surface of the prepared ceramic film is gradually increased, and the number of pores is also gradually increased, that is, the larger the pore diameter of the prepared ceramic film is and the larger the number of pores is with the increase of the sintering temperature. Wherein the pore diameter of the pores of the surface of the ceramic membrane shown in fig. 2 is relatively uniform and the number of pores is reasonable, i.e., the pore diameter of the pores of the surface of the ceramic membrane formed by sintering at 950 ℃ is relatively uniform and the number of pores is reasonable. As can be seen from fig. 6, the ceramic film prepared in comparative example one had holes that melted, i.e., when the sintering temperature reached 1100 ℃, the inside of the ceramic film began to melt.
The ceramic membranes of the first to fourth examples were used to obtain a Cr concentration of 100mg/L at the initial concentration 3+ Solution and Cu with initial concentration of 100mg/L 2+ The solution was filtered to test the ceramic membranes of examples one to four for Cr 3+ And Cu 2+ Separation rate of Cr 3+ And Cu 2+ The separation rate test results of (a) are shown in fig. 9 and 10, respectively. As shown in FIGS. 9 and 10, the ceramic film of the second embodiment is composed of Cr 3+ The separation rate of the ceramic membrane in the first embodiment reaches 84.22%, and the ceramic membrane in the first embodiment has a Cu concentration of 2+ The separation rate of (2) reaches 98.5 percent.
The ceramic films of the above examples one to comparative example one were subjected to mechanical strength test, and the test results are shown in table 2 below.
Table 2 results of mechanical strength test of ceramic films of examples one to five
As can be seen from Table 2, the ceramic films of examples one to four have a good mechanical strength, and in particular, the mechanical strength of the ceramic film obtained by sintering at 950℃in example two can reach 9.9MPa. Whereas the ceramic film of comparative example one has a smaller mechanical strength.
Comparative example two
Comparative example two discloses a preparation method of a ceramic membrane, which comprises the following steps:
the natural phosphate is used as a raw material, and after grinding and screening, a die with the diameter of 40mm is used for pressing to prepare the ceramic membrane, the sintering temperature is controlled to be 1000 ℃, the sintering speed is controlled to be 5 ℃/min, and the sintering time is controlled to be 3 hours.
Comparative example three
Comparative example three discloses a method for preparing a ceramic membrane, comprising the steps of:
mineral fly ash is used as raw material, and carboxymethyl cellulose and starch are added into the raw material to respectively serve as an adhesive and a pore-forming agent. The tubular ceramic membrane is prepared by an extrusion process, the sintering temperature is 1125 ℃, the sintering rate is 5 ℃/min, and the sintering time is 2 hours.
Comparative example four
Comparative example four discloses a method for preparing a ceramic membrane, comprising the steps of:
loess and fly ash are used as raw materials, and carboxymethyl cellulose and methyl methacrylate are added into the raw materials to respectively serve as an adhesive and a pore-forming agent. The ceramic membrane is prepared by roll forming, the sintering temperature is 1130 ℃, the sintering speed is 7 ℃/min, and the sintering time is 2.5h.
Comparative example five
Comparative example five discloses a preparation method of a ceramic membrane, comprising the following steps:
by alpha-Al 2 O 3 As raw materials, carboxymethyl cellulose and glycerol are added thereto as binders and plasticizers. The ceramic membrane is prepared by an extrusion molding method, the sintering temperature is 1300 ℃, the sintering speed is 10 ℃/min, and the sintering time is 2 hours.
Comparative example six
Comparative example six discloses a preparation method of a ceramic membrane, comprising the steps of:
Fly ash is used as raw material, and polyvinyl alcohol solution is added into the fly ash as adhesive. The ceramic membrane is prepared by using a grouting method, the sintering temperature is 800 ℃, the sintering speed is 2 ℃/min, and the sintering time is 2h.
The ceramic membranes of the above examples and comparative examples were subjected to a pure water flux test at a pressure of 0.3bar, and the test results are shown in table 3 below.
TABLE 3 pure water flux test results of ceramic membranes of the above examples and comparative examples
As is clear from Table 3, the pure water flux of the ceramic membrane prepared in this example was 220kg/m 2 H to 600kg/m 2 Between h, the ceramic membrane has both a faster filtration efficiency and a better separation rate, as can be seen from the pure water flux range. The ceramic membrane of the first comparative example has too high pure water flux, but has a low separation rate although the filtration efficiency is high, and the pure water fluxes of the second comparative example, the third comparative example, the fourth comparative example, the fifth comparative example and the sixth comparative example are all low, so that the filtration efficiency is low, and the requirement of the industrial wastewater filtration efficiency is difficult to meet.
Comparative example seven
Comparative example seven discloses a method for preparing a ceramic membrane, which is different from example two in that calcium carbonate is not used as a pore-forming agent in the preparation of the ceramic membrane.
The ceramic membranes of example two and comparative example seven were tested for pure water flux and the test structure is shown in fig. 11. As can be seen from fig. 11, the pure water flux of the ceramic membrane of example two is significantly greater than that of the ceramic membrane of comparative example seven. From this, it is known that the addition of calcium carbonate as a pore-forming agent can significantly improve the filtration efficiency of the ceramic membrane, because a large amount of gas can be generated at the time of sintering by adding calcium carbonate to increase the amount of pores and the pore diameter of the ceramic membrane, thereby improving the filtration efficiency of the ceramic membrane.
The ceramic membrane and the preparation method thereof disclosed in the embodiments of the present invention are described in detail, and specific examples are applied to illustrate the principles and embodiments of the present invention, and the description of the above examples is only for helping to understand the ceramic membrane and the preparation method and core idea thereof; meanwhile, as those skilled in the art will vary in the specific embodiments and application scope according to the idea of the present invention, the present disclosure should not be construed as limiting the present invention in summary.
Claims (9)
1. A method for preparing a ceramic membrane, comprising the steps of:
Mixing: incineration of household garbage with bottom slag and Al 2 O 3 Mixing and grinding an organic solvent, a binder and a pore-forming agent to form a mixture, said Al 2 O 3 Is gamma-Al 2 O 3 ；
Pressing: pressing the mixture into a sheet;
sintering: sintering the sheet at 950 ℃ for 2-4 hours to obtain a ceramic membrane;
before the step of mixing, the preparation method further comprises the steps of:
grinding: grinding the household garbage incineration bottom slag until the particle size of the particles of the household garbage incineration bottom slag is smaller than 325 meshes;
the organic solvent comprises at least one of methanol, ethanol, formaldehyde and acetaldehyde.
2. The method of preparing a ceramic membrane according to claim 1, wherein prior to the step of mixing, the method further comprises the steps of:
component analysis: carrying out component analysis on the household garbage incineration bottom slag to obtain the molar quantity of silicon and aluminum in the household garbage incineration bottom slag;
weighing Al 2 O 3 : weighing Al 2 O 3 So that the molar quantity of silicon in the household garbage incineration bottom slag, the household garbage incineration bottom slag and the Al 2 O 3 The ratio of the sum of the molar amounts of the aluminum is 1:1 to 3:1.
3. The method of preparing a ceramic membrane according to claim 1, wherein the mixing step is preceded by the step of:
Preparation of gamma-Al 2 O 3 : sintering boehmite in a muffle furnace at 600-650 ℃ to form gamma-Al 2 O 3 。
4. The method of producing a ceramic membrane according to claim 1, wherein the binder comprises at least one of a polyvinyl alcohol solution, a carboxymethyl cellulose solution, and a polyethylene glycol solution;
the pore-forming agent is calcium carbonate.
5. The method of claim 4, wherein when the binder comprises a polyvinyl alcohol solution, the mixing step is preceded by:
preparing a polyvinyl alcohol solution: adding deionized water into polyvinyl alcohol particles, and stirring at 80-100 ℃ until the polyvinyl alcohol particles are dissolved to prepare a polyvinyl alcohol solution, wherein the polyvinyl alcohol solution comprises 5-10wt% of polyvinyl alcohol.
6. The method for producing a ceramic membrane according to claim 5, wherein the mass of the polyvinyl alcohol solution is larger than the mass of the household garbage incineration bottom slag and the mass of the Al 2 O 3 10wt% of the sum of the masses.
7. The method of producing a ceramic membrane according to claim 1, characterized in that before the step of pressing, the method of producing comprises the steps of:
and (3) drying: the mixture is dried at 60-70 ℃.
8. The method of producing a ceramic film according to claim 1, wherein in the step of pressing, the pressing pressure is 20MPa to 30MPa and the holding time is 1min to 3min.
9. A ceramic membrane prepared by the method of any one of claims 1-8.
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