CN111056858A - Preparation method of flat ceramic membrane support and ceramic pug thereof - Google Patents
Preparation method of flat ceramic membrane support and ceramic pug thereof Download PDFInfo
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- CN111056858A CN111056858A CN201911328280.8A CN201911328280A CN111056858A CN 111056858 A CN111056858 A CN 111056858A CN 201911328280 A CN201911328280 A CN 201911328280A CN 111056858 A CN111056858 A CN 111056858A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000012528 membrane Substances 0.000 title abstract description 45
- 239000002994 raw material Substances 0.000 claims abstract description 57
- 235000015895 biscuits Nutrition 0.000 claims abstract description 54
- 238000001125 extrusion Methods 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 239000007787 solid Substances 0.000 claims abstract description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 239000000314 lubricant Substances 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 5
- 238000007602 hot air drying Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000010445 mica Substances 0.000 claims description 4
- 229910052618 mica group Inorganic materials 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 3
- 235000005822 corn Nutrition 0.000 claims description 3
- 235000013312 flour Nutrition 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 235000010981 methylcellulose Nutrition 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 240000008042 Zea mays Species 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 238000012797 qualification Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000004907 flux Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 241000209149 Zea Species 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000011800 void material Substances 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/20—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein the material is extruded
- B28B3/22—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein the material is extruded by screw or worm
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/64—Burning or sintering processes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3418—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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
- C04B2235/3445—Magnesium silicates, e.g. forsterite
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- 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
- C04B2235/34—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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- Manufacturing & Machinery (AREA)
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a ceramic pug of a thin-wall flat plate ceramic support, which comprises the following raw materials: (1) the solid raw materials comprise the following raw materials in percentage by mass: alumina powder: 60% -80%, sintering aid: 10-30%, pore-forming agent: 10% -30%; (2) the liquid raw materials comprise the following raw materials in percentage by mass: dispersing agent: 15% -25%, lubricant: 5% -15%, pure water: 60% -80%; the weight ratio of the solid raw materials to the liquid raw materials is (5-7.5): 1; the thin-wall flat ceramic support body can be prepared by adopting the ceramic pug. By adopting the method, the reject ratio of the flat-plate membrane biscuit in the processes of extrusion, drying and sintering can be reduced to a greater extent, and the qualification rate of the flat-plate ceramic membrane support body is improved; the prepared flat membrane support body has the advantages of greatly reduced sintering temperature, reduced production energy consumption, high chemical composition purity of the support body and strong corrosion resistance.
Description
Technical Field
The invention belongs to the field of water purification, and particularly relates to a preparation method of a flat ceramic membrane support and ceramic pug thereof.
Background
A Membrane Bioreactor (MBR) is a high-efficiency sewage treatment device integrating membrane separation technology and microbial technology. The most core component in the membrane bioreactor is the membrane element, and the membrane element is mainly divided into an organic membrane and a ceramic membrane according to the material at present. Compared with organic membranes, ceramic membranes have the characteristics of high temperature resistance, acid and alkali corrosion resistance, solvent resistance and the like, and have been widely applied to the engineering fields of chemical engineering, food, water treatment and the like.
Among ceramic membranes, plate-type ceramic membranes have the characteristics of convenience in installation, small filtration resistance, low running cost and the like compared with tubular ceramic membranes, and in recent years, attention is increasingly paid at home and abroad. The prior patents and literature researches on plate-type ceramic membranes mainly focus on the aspects of optimization of preparation process, cost reduction, equipment screening and the like, such as: chinese patent document CN105000871A discloses a multifunctional flat ceramic membrane and a preparation process thereof, which not only has a filtration function, but also has other functions such as catalysis and oxidation, but also has a problem that how to control deformation in the preparation process of the flat ceramic membrane is not clear; chinese patent document CN 104258737A discloses a preparation method of a large-size thin-wall hollow flat ceramic membrane, which explains the problem that the firing temperature of a thin-wall flat membrane support is low, the energy consumption is low, but the strength is low; paper literature [ guo rui song, yandean, chenyue ] metal support plate ceramic membrane preparation and performance [ J ] silicate advisory, 1999, (5): 55-57 research the preparation technology and performance of a novel membrane-metal supporting flat ceramic membrane, and try to develop the application of the novel membrane-metal supporting flat ceramic membrane in the fields of chemical industry, food, pharmacy and the like, but the product prepared under the optimal condition has the problem of low void ratio.
However, no effective control measure has been proposed in the prior art for the problem that the thin-walled flat membrane support is easily deformed during extrusion, drying and sintering processes.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength ultrathin thin-wall flat ceramic membrane support and ceramic pug thereof, which are used for solving the problems of low strength, low pure water flux and the like of a flat ceramic membrane in the prior art.
The purpose of the invention is realized by the following technical scheme:
the ceramic pug of the thin-wall flat ceramic support is characterized by comprising the following raw materials:
(1) the solid raw materials comprise the following raw materials in percentage by mass: alumina powder: 60% -80%, sintering aid: 10-30%, pore-forming agent: 10% -30%;
(2) the liquid raw materials comprise the following raw materials in percentage by mass: dispersing agent: 15% -25%, lubricant: 5% -15%, pure water: 60% -80%;
the weight ratio of the solid raw materials to the liquid raw materials is (5-7.5): 1;
the alumina is an alumina mixture with the particle size of 25-35 mu m and the particle size of 3-7 mu m, and the proportion of the alumina mixture to the alumina mixture is (4-7): 1; the pore-forming agent is one or more of starch, methyl cellulose or corn flour, and the average particle size of the pore-forming agent is 60 mu m; the sintering aid is one or more of talcum powder, mica powder or quartz stone, and the average particle size of the sintering aid is 700 nm;
the dispersing agent is one or more of polyethylene glycol or polyacrylic acid; the lubricant is one or more of glycerol, silicone oil or polyester.
The preparation method for preparing the thin-wall flat plate ceramic support body by adopting the ceramic pug is characterized by comprising the following steps of:
(1) preparing ceramic pug: respectively and uniformly mixing the solid raw material and the liquid raw material, adding the liquid raw material into the solid raw material which is continuously stirred, uniformly stirring, and putting into a closed box for ageing for 12-24 hours to obtain pug;
(2) preparing a biscuit: a two-section screw extrusion molding method is adopted, the pug is put into a screw extruder for vacuum pugging and extrusion molding, the extrusion speed is 0.5-2 m/min, the extrusion temperature is 15-30 ℃, and the extrusion pressure is 2-4 MPa; cutting to obtain a biscuit, wherein the wall thickness of the biscuit is 1.2-2.0 mm;
(3) drying the biscuit: airing the biscuit at normal temperature for 12-24 h, and then conveying the biscuit into a hot air drying kiln for drying, wherein the drying temperature is 30-70 ℃, and the drying time is 6-10 h;
(4) and (3) sintering of the biscuit: and (3) conveying the dried biscuit into a kiln for sintering, wherein the heating rate is 1-4 ℃/h, the sintering highest temperature is 1200-1300 ℃, the heat preservation time is 1.5-4 h, then slowly cooling is carried out, the cooling rate is 2-5 ℃/h, and the thin-wall flat plate ceramic support body can be obtained after cooling.
Preferably, in the step (2), the liquid raw material is added to the solid raw material which is continuously stirred in a spraying manner.
Preferably, in the step (2), the biscuit is cut by infrared rays, so that the problems of deformation and green mud accumulation during the extrusion process of the biscuit of the thin-wall flat ceramic membrane support are avoided.
Preferably, in the step (3), a vacuum chuck is adopted to convey the cut biscuit to a porous stainless steel plate with a porous sponge spread on the surface for airing.
Preferably, in the step (3), in the drying process, the temperature rise rate of the drying temperature is 1-3 ℃/h, and the problem of cracking or deformation of the biscuit caused by too fast evaporation of water is avoided through gentle temperature rise.
Compared with the prior art, the invention has the following advantages:
by adopting the method, the reject ratio of the flat-plate membrane biscuit in the processes of extrusion, drying and sintering can be reduced to a greater extent, and the qualification rate of the flat-plate ceramic membrane support body is improved; because the nano-scale talcum powder, mica powder or quartz stone is used as the sintering aid, the sintering temperature of the flat membrane support body is greatly reduced, the production energy consumption is reduced, the chemical composition purity of the support body is high, and the corrosion resistance of the support body is strong.
Detailed Description
It should be understood by those skilled in the art that the present embodiment is only for illustrating the present invention and is not to be used as a limitation of the present invention, and changes and modifications of the embodiment can be made within the scope of the claims of the present invention.
Example 1
The ceramic pug of the thin-wall flat ceramic membrane support body is as follows:
(1) solid raw materials: 70wt% of alumina powder with the average grain diameter of 25 mu m, 10wt% of alumina powder with the average grain diameter of 3 mu m, 10wt% of starch and 10wt% of talcum powder, and the total mass is 100 kg;
(2) liquid raw materials: 22wt% of polyethylene glycol with the average molecular weight of 400, 8wt% of glycerol and 70wt% of pure water, and the total mass is 20 kg;
the weight ratio of the solid raw material to the liquid raw material is 5: 1.
preparing a thin-wall flat ceramic membrane support:
(1) preparing ceramic pug: respectively and uniformly mixing the solid raw material and the liquid raw material, adding the liquid raw material into the continuously stirred solid raw material in a spraying mode, uniformly stirring, and then putting into a closed box for ageing for 12 hours to obtain pug;
(2) preparing a biscuit: adopting a two-section screw extrusion molding method, putting the pug into a screw extruder for vacuum pugging and extrusion molding, wherein the extrusion speed is 1m/min, the extrusion temperature is 20 ℃, and the extrusion pressure is 2 MPa; cutting by adopting infrared rays to obtain a biscuit, wherein the wall thickness of the biscuit is 1.5mm, and the speed of a biscuit connecting belt is consistent with that of extrusion;
(3) drying the biscuit: conveying the biscuit to a porous stainless steel plate with porous sponge spread on the surface by using a vacuum chuck, airing the biscuit for 24 hours at normal temperature, then conveying the biscuit into a hot air drying kiln for drying, slowly heating at the speed of 2 ℃/h, wherein the maximum drying temperature is 70 ℃, and the drying time is 10 hours;
(4) and (3) sintering of the biscuit: and (2) sintering the dried biscuit in a shuttle kiln at a heating rate of 2 ℃/h and a highest sintering temperature of 1250 ℃, cooling after the heat preservation time is 3h and at a cooling rate of 3 ℃/h, and cooling to obtain the thin-wall flat ceramic support body, wherein the slow heating rate and the slow cooling rate are strictly controlled, so that the rapid sintering is avoided, and the green body is cracked.
The obtained thin-wall flat ceramic membrane support has porosity of 38%, average pore diameter of 2 μm, and strength of 40%MPa, pure water flux 9m3/h/m2And the qualification rate of each batch of thin-wall flat membrane is 88 percent.
Example 2
The ceramic pug of the thin-wall flat ceramic membrane support body is as follows:
(1) solid raw materials: 65wt% of alumina powder with the average particle size of 30 mu m, 15wt% of alumina powder with the average particle size of 7 mu m, 10wt% of methyl cellulose and 10wt% of talcum powder, and the total mass is 120 kg;
(2) liquid raw materials: 25wt% of polyacrylic acid with the average molecular weight of 72, 10wt% of glycerol and 65wt% of pure water, wherein the total mass is 20 kg;
the weight ratio of the solid raw material to the liquid raw material is 6: 1.
preparing a thin-wall flat ceramic membrane support:
(1) preparing ceramic pug: respectively and uniformly mixing the solid raw material and the liquid raw material, adding the liquid raw material into the continuously stirred solid raw material in a spray drying mode, uniformly stirring, and putting into a closed box for ageing for 18 hours to obtain pug;
(2) preparing a biscuit: adopting a two-section screw extrusion molding method, putting the pug into a screw extruder for vacuum pugging and extrusion molding, wherein the extrusion speed is 0.8m/min, the extrusion temperature is 22 ℃, and the extrusion pressure is 3 MPa; cutting by adopting infrared rays to obtain a biscuit, wherein the wall thickness of the biscuit is 1.6mm, and the speed of a biscuit connecting belt is consistent with that of extrusion;
(3) drying the biscuit: conveying the biscuit to a porous stainless steel plate with porous sponge spread on the surface by using a vacuum chuck, airing the biscuit for 20 hours at normal temperature, then conveying the biscuit into a hot air drying kiln for drying, slowly heating at the speed of 2.5 ℃/h, wherein the maximum drying temperature is 70 ℃, and the drying time is 8 hours;
(4) and (3) sintering of the biscuit: and (2) sintering the dried biscuit in a shuttle kiln at a heating rate of 1.5 ℃/h and a highest sintering temperature of 1200 ℃, keeping the temperature for 2h, cooling at a cooling rate of 4 ℃/h to obtain the thin-wall flat ceramic support body, and strictly controlling the slow heating and cooling rates to avoid quick sintering and blank cracking.
The obtained thin-wall flat ceramic membrane support has a porosity of 40%, an average pore diameter of 2.2 μm, a strength of 45MPa, and a pure water flux of 10m3/h/m2And the qualification rate of preparing each batch of thin-wall flat membrane is 92 percent.
Example 3
The ceramic pug of the thin-wall flat ceramic membrane support body is as follows:
(1) solid raw materials: 55wt% of alumina powder with the average particle size of 35 mu m, 15wt% of alumina powder with the average particle size of 5 mu m, 15wt% of corn flour, 15wt% of mica powder and 140kg of total mass;
(2) liquid raw materials: 20wt% of polyethylene glycol with molecular weight of 400, 5wt% of polyester with molecular weight of 85 and 75wt% of pure water, wherein the total mass is 20 kg;
the weight ratio of the solid raw material to the liquid raw material is 7: 1.
preparing a thin-wall flat ceramic membrane support:
(1) preparing ceramic pug: respectively and uniformly mixing the solid raw material and the liquid raw material, adding the liquid raw material into the continuously stirred solid raw material in a spraying mode, uniformly stirring, and then putting into a closed box for ageing for 24 hours to obtain pug;
(2) preparing a biscuit: adopting a two-section screw extrusion molding method, putting the pug into a screw extruder for vacuum pugging and extrusion molding, wherein the extrusion speed is 1.5m/min, the extrusion temperature is 25 ℃, and the extrusion pressure is 4 MPa; cutting by adopting infrared rays to obtain a biscuit, wherein the wall thickness of the biscuit is 1.2mm, and the speed of a biscuit connecting belt is consistent with that of extrusion;
(3) drying the biscuit: conveying the biscuit to a porous stainless steel plate with porous sponge spread on the surface by using a vacuum chuck, airing the biscuit for 24 hours at normal temperature, then conveying the biscuit into a hot air drying kiln for drying, slowly heating at the speed of 2 ℃/h, wherein the maximum drying temperature is 60 ℃, and the drying time is 6 hours;
(4) and (3) sintering of the biscuit: and (2) conveying the dried biscuit into a shuttle kiln for sintering, wherein the heating rate is 2.5 ℃/h, the highest sintering temperature is 1290 ℃, the temperature is kept for 4h, then the temperature is reduced, the temperature reduction rate is 2.5 ℃/h, and the thin-wall flat plate ceramic support body can be obtained after cooling, the slow heating rate and the temperature reduction rate are strictly controlled, so that the rapid sintering is avoided, and the blank body is cracked.
The obtained thin-wall flat ceramic membrane support has porosity of 42%, average pore diameter of 2.5 μm, strength of 35MPa, and pure water flux m3/h/m2And the qualification rate of preparing each batch of thin-wall flat membrane is 90 percent.
Claims (8)
1. The ceramic pug of the thin-wall flat ceramic support is characterized by comprising the following raw materials:
(1) the solid raw materials comprise the following raw materials in percentage by mass: alumina powder: 60% -80%, sintering aid: 10-30%, pore-forming agent: 10% -30%;
(2) the liquid raw materials comprise the following raw materials in percentage by mass: dispersing agent: 15% -25%, lubricant: 5% -15%, pure water: 60% -80%;
the weight ratio of the solid raw materials to the liquid raw materials is (5-7.5): 1.
2. the ceramic slurry for a thin-walled flat ceramic support according to claim 1, wherein the alumina is a mixture of alumina having a particle size of 25 to 35 μm and a particle size of 3 to 7 μm, and the ratio of the two is (4 to 7): 1; the pore-forming agent is one or more of starch, methyl cellulose or corn flour, and the average particle size of the pore-forming agent is 60 mu m; the sintering aid is one or more of talcum powder, mica powder or quartz stone, and the average particle size of the sintering aid is 700 nm.
3. The ceramic mud of thin-walled flat ceramic support according to claim 1, wherein the dispersant is one or more of polyethylene glycol or polyacrylic acid; the lubricant is one or more of glycerol, silicone oil or polyester.
4. A method for preparing a thin-wall flat plate ceramic support body by using the ceramic mud material as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps:
(1) preparing ceramic pug: respectively and uniformly mixing the solid raw material and the liquid raw material, adding the liquid raw material into the solid raw material which is continuously stirred, uniformly stirring, and putting into a closed box for ageing for 12-24 hours to obtain pug;
(2) preparing a biscuit: a two-section screw extrusion molding method is adopted, the pug is put into a screw extruder for vacuum pugging and extrusion molding, the extrusion speed is 0.5-2 m/min, the extrusion temperature is 15-30 ℃, and the extrusion pressure is 2-4 MPa; cutting to obtain a biscuit, wherein the wall thickness of the biscuit is 1.2-2.0 mm;
(3) drying the biscuit: airing the biscuit at normal temperature for 12-24 h, and then conveying the biscuit into a hot air drying kiln for drying, wherein the drying temperature is 30-70 ℃, and the drying time is 6-10 h;
(4) and (3) sintering of the biscuit: and (3) conveying the dried biscuit into a kiln for sintering, wherein the heating rate is 1-4 ℃/h, the sintering highest temperature is 1200-1300 ℃, the heat preservation time is 1.5-4 h, then slowly cooling is carried out, the cooling rate is 2-5 ℃/h, and the thin-wall flat plate ceramic support body can be obtained after cooling.
5. The production method according to claim 4, wherein in the step (2), the liquid raw material is added in a spraying manner to the solid raw material which is continuously stirred.
6. The method according to claim 4, wherein in the step (2), the biscuit is cut with infrared rays.
7. The method according to claim 4, wherein in the step (3), the cut biscuit is conveyed to a porous stainless steel plate with a porous sponge spread on the surface thereof by using a vacuum chuck for airing.
8. The preparation method according to claim 4, wherein in the step (3), the temperature rise rate of the drying temperature in the drying process is 1-3 ℃/h.
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| CN111851651B (en) * | 2020-08-18 | 2021-12-21 | 哈尔滨工业大学（威海） | Catalytic membrane filtration secondary water supply equipment and method for using the same for catalytic membrane filtration secondary water supply |
| CN114105671A (en) * | 2021-12-28 | 2022-03-01 | 河南省高新技术实业有限公司 | A kind of gangue-quartz-based ceramic support and preparation method thereof |
| WO2023164923A1 (en) * | 2022-03-02 | 2023-09-07 | 哈尔滨工业大学（威海） | Method for low-temperature preparation of ceramic membrane |
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