CN109248566A - A kind of hollow plate type ceramic film of helical duct and preparation method thereof - Google Patents
A kind of hollow plate type ceramic film of helical duct and preparation method thereof Download PDFInfo
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- CN109248566A CN109248566A CN201811438253.1A CN201811438253A CN109248566A CN 109248566 A CN109248566 A CN 109248566A CN 201811438253 A CN201811438253 A CN 201811438253A CN 109248566 A CN109248566 A CN 109248566A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/06—Flat membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/025—Aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2315/00—Details relating to the membrane module operation
- B01D2315/10—Cross-flow filtration
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention discloses a kind of hollow plate type ceramic film of helical duct and preparation method thereof, the hollow plate type ceramic film shape is in disk shape, center has a circumferential notch to collect the substance for penetrating UF membrane, there is a helical channel in inside, make the substance through UF membrane under the action of draft, is pooled to the collection of central circular indentation, there;The hollow circular plate type ceramic membrane outer closures, inner hollow only communicate with the outside world at circumferential notch;This structure can form cross-flow filtration as long as rotating ceramic membrane, achieve the effect that self-cleaning film surface, and filtration path is short, filter efficiency is high, does not need to encapsulate.
Description
Technical field
The present invention relates to ceramic separation film technical field more particularly to a kind of hollow plate type ceramic films of helical duct and its system
Preparation Method, this structure achieve the effect that self-cleaning film surface convenient for forming cross-flow filtration.
Background technique
Ceramic separation film is due to excellent high separating efficiency, high temperature resistant, corrosion-resistant, solvent resistant, long service life, height
The advantages that mechanical strength and renewable easy cleaning, application have penetrated into environmental protection, water process, food, beverage, biological medicine, hair
The various fields such as ferment, petrochemical industry, separation, clarification, purifying, concentration, degerming, the desalination etc. that can be used in technical process.At present
The ceramic membrane used in the market is broadly divided into two major classes, and one kind is tubular ceramic membrane, and another kind of is hollow planar ceramic membrane.Pipe
Although formula ceramic membrane is cross-flow filtration, but filtration path is long, and filter efficiency is low;Although hollow planar ceramic membrane filtration path
It is short, but encapsulation is not easy, and loading density is smaller, and due to its plate structure, is not easy to implement cross-flow filtration.In view of tubular ceramic membrane
With the deficiency of hollow plate type ceramic film, therefore making for tubular ceramic membrane and hollow planar ceramic membrane is limited to a certain extent
With range and field.
During the filtration process, with the increase of filtration time, trapped substance is gradually rich long-pending on the surface of the film for ceramic membrane, forms one
Layer trapped substance separation layer, and then increase filtration resistance, filtering rate is reduced, concentration polarization is formed.Concentration polarization will increase film table
Face is trapped the concentration of substance, accelerates the generation of fouling membrane, leads to flux depression, and transmembrane pressure rises, and influences UF membrane effect
The service life of rate and film.Hollow circular plate type ceramic membrane can form one with filtered fluid in itself rotation on film surface and be parallel to
The shear stress of film surface, suitable scraping brushing device wiper on film surface, plays the role of self-cleaning, film surface is made to be not easy to form retention
Object separation layer reduces filtration resistance and fouling membrane, and then improves the service life of UF membrane efficiency and film.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of hollow plate type ceramic film of helical duct and its preparation side
Method.
To achieve the above object, the specific technical solution of the present invention is as follows:
A kind of hollow plate type ceramic film of helical duct a comprising inner supporting body and two hollow laminar film supporting surfaces, two film branch
Support face is encapsulated in inner supporting body upper and lower surface;The inner supporting body is the helical structure of integral type, and the axial bore that end coils are formed is not small
In the hollow dimension of film supporting surface, and the gutter channel that end coils are formed is connected to two film supporting surface hollow parts.
Above-mentioned axial bore is greater than or equal to the hollow dimension of film supporting surface, is to guarantee that end coils are encapsulated in film branch
Non- hollow part between support face, in addition, the end coils gutter channel of film supporting surface formation is clipped in, with two film supporting surfaces
Hollow passageway connection.
As an of the invention preferred embodiment, the spiral thickness h of the everywhere of the helical structure of the inner supporting body and
The size range of channel span b is 0.1-10000mm.
As a preferred embodiment of the invention, the inner supporting body cross sectional shape is rectangle, polygon or ellipse.
As a preferred embodiment of the invention, the inner supporting body and two film supporting surfaces are in disc-shaped.
In the present invention, this hollow circular plate type ceramic film support is supported by an inner supporting body and two panels open circles laminar film
Face is constituted, and inner supporting body is the spiral ring structure for forming one, and the hollow circular plate type ceramic membrane of domestic and international multichannel is logical
Road be it is trapezoidal, the supporting point span from the farther away position film supporting surface in the center of circle is big, with the increase of film outer diameter, supporting point across
Degree also increases, when by filtered fluid to the impact force action of film surface, easily damage film surface, film surface jackknifing, this pole even occurs
The outer dimension of film is limited greatly, reduces effective filtration area;Compared to the hollow circular plate type ceramic membrane of domestic and international multichannel, this hair
The supporting point span variation of bright film supporting surface is controllable, even up to equal to every place's span, and can adjust span, film according to demand
The pressure that face can be born is bigger, can bear when high speed itself rotation filtered fluid to the impact force of film surface, and inner supporting body has a style of one's own,
It can individually process, convenient for the production of hollow circular plate type ceramic membrane, processing and the integral strength for improving film;Filtration path is short, mistake
Filter it is high-efficient, do not need to encapsulate, cross-flow filtration easy to implement, widened use scope and the field of ceramic separation film.
The present invention also provides the preparation methods of the hollow plate type ceramic film of above-mentioned helical duct, and wherein supporter green compact are using note
Molding technique, manufacturing method step is:
(1) by organic monomer acrylamide (AM), crosslinking agent methylene-bisacrylamide (MBAM), dispersing agent lemon acid amide
(AC) and water is mixed to get premixed liquid according to a certain percentage;Ball mill is added in ceramic powder and premixed liquid by a certain percentage again
In, it is spare to obtain high solid phase, the slurry of low viscosity by ball milling 1-4h;
(2) catalyst tetramethylethylenediamine (TEMED), initiator over cure is added in the good slurry of ball milling according to a certain percentage
Acid amide (APS) injects the metal die of hollow laminar film supporting surface and helical form inner supporting body after mixing evenly or other is non-porous
In the mold of material;The organic monomer polymerization crosslinking in suspended substance is set to form three-dimensional net structure, so that liquid slurry be made to change
At solid-state green body, slurry is formed by curing gel by certain time at 40-80 DEG C;Then demoulding obtains hollow laminar film support
Face and helical form inner supporting body green compact;
(3) it is carried out with the inner supporting body green body that two panels one upper and lower surface of hollow laminar film supporting surface green body folder all applies clay
Combination, the green body that will be combined are sintered in 400-1800 DEG C of temperature tripping in kiln, and soaking time 1-5h obtains hollow platy branch
Support body h;
(4) preparative separation film layer, the material of separation membrane layer include aluminum oxide, carbon on hollow platy support external surface
SiClx matter, cordierite, zirconium oxide, siliceous and titanium dioxide matter;The method of preparative separation film includes infusion process, spray
Coating and spin-coating method enter kiln sintering, finally obtain the helical duct hollow plate after being covered with the supporter drying of separation membrane layer
Formula ceramic membrane.
As a preferred embodiment of the invention, the ceramic powder in step (a) includes alumina powder, carbonization
Si powder, cordierite powder, Zirconium oxide powder, titania powder, SiO 2 powder.
As a preferred embodiment of the invention, the ceramic powder in step (a) further includes pore creating material, the pore-creating
Any one of agent in silicon carbide, graphite, starch.
As an of the invention preferred embodiment, inner supporting body in hollow platy supporter after the sintering in step (c)
The spiral thickness h of the everywhere of helical structure and the size range of channel span b are 0.1-10000mm.
As an of the invention preferred embodiment, inner supporting body in hollow platy supporter after the sintering in step (c)
Cross sectional shape is rectangle, polygon or ellipse.
As a preferred embodiment of the invention, the inner supporting body and two film supporting surfaces are in disc-shaped.
Using technical solution of the present invention, have the advantages that
The hollow circular plate type ceramic membrane structure of the present invention can form cross-flow filtration as long as rotating ceramic membrane, reach self-cleaning film
The effect in face, filtration path is short, filter efficiency is high, does not need to encapsulate.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the hollow plate type ceramic film of the present invention;
Fig. 2 is the structural schematic diagram that the hollow plate type ceramic film of the present invention omits upper film supporting surface.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further described.
Embodiment 1
(1) to weigh each substance by following weight percent spare: alumina powder (5 μm, 95.3wt%), carbonic acid magnesium powder (5 μ
M, 1wt%), titanium oxide powder (5 μm, 1wt%), organic monomer acrylamide AM (2wt%), crosslinking agent methylene-bisacrylamide
MBAM (0.2wt%), dispersing agent lemon acid amide AC (0.3wt%), tetramethylethylenediamine TEMED (0.1wt%), concentration 5%
The initiator Ammonium Persulfate 98.5 APS (0.1wt%) of aqueous solution.
(2) the organic monomer acrylamide (AM) that will have been weighed, crosslinking agent methylene-bisacrylamide (MBAM), dispersing agent
Lemon acid amide (AC) and the 45wt% water of the above spare substance total weight is mixed to get premixed liquid, then by premixed liquid with weighed
Alumina powder (5 μm, 95.3wt%), carbonic acid magnesium powder (5 μm, 1wt%), ball in (5 μm, 1wt%) addition ball mills of titanium oxide powder
2h is ground, it is spare to obtain high solid phase, the slurry of low viscosity.
(3) catalyst tetramethylethylenediamine (TEMED), the initiator Ammonium Persulfate 98.5 weighed is added in the good slurry of ball milling
(APS), the metal die for injecting supporting surface and inner supporting body after mixing evenly, forms the organic monomer polymerization crosslinking in suspended substance
Three-dimensional net structure, so that liquid slurry be made to be transformed into solid-state green body, slurry is formed by curing solidifying by certain time at 70 DEG C
Glue.Then demoulding can be obtained shown in Fig. 1 and Fig. 2 and have compared in the open circles laminar film supporting surface and helical form of high green
Support body green body.
(4) upper and lower surface is pressed from both sides with two panels open circles laminar film supporting surface green body all apply the inner supporting body green body of clay such as
Fig. 1 is combined, the green body that will be combined, and is sintered in 1350 DEG C of temperature tripping in kilns, soaking time 1.5h, so that it may be obtained such as figure
Hollow disk-shaped supporter shown in 1.
(5) aluminum oxide film layer is prepared by spin-coating method on support external surface, 3-25 μm of thicknesses of layers, modifies film thickness
Between 3-30nm, membrane aperture 1.5-2000nm, 4h is dried after the completion of film forming at a temperature of 80 DEG C, then enters kiln in 1000 DEG C of temperature
Lower sintering, soaking time 2h obtain the hollow plate type ceramic film of the helical duct.
Embodiment 2
(1) to weigh each substance by following weight percent spare: cordierite powder (5 μm, 97.55wt%), organic monomer
Acrylamide AM (1.8wt%), crosslinking agent methylene-bisacrylamide MBAM (0.2wt%), dispersing agent lemon acid amide AC
(0.25wt%), tetramethylethylenediamine TEMED (0.1wt%), concentration are the initiator Ammonium Persulfate 98.5 APS of 5% aqueous solution
(0.1wt%).
(2) the organic monomer acrylamide (AM) that will have been weighed, crosslinking agent methylene-bisacrylamide (MBAM), dispersing agent
Lemon acid amide (AC) and the 45wt% water of the above spare substance total weight is mixed to get premixed liquid, then by premixed liquid with weighed
Cordierite powder (5 μm, 97.55wt%), while (3 μm, 0.5wt%) of additional silicon carbide powder are added ball as pore creating material together
It is spare to obtain high solid phase, the slurry of low viscosity by ball milling 2.5h in grinding machine.
(3) catalyst tetramethylethylenediamine (TEMED), the initiator Ammonium Persulfate 98.5 weighed is added in the good slurry of ball milling
(APS), the metal die for injecting supporting surface and inner supporting body after mixing evenly, forms the organic monomer polymerization crosslinking in suspended substance
Three-dimensional net structure, so that liquid slurry be made to be transformed into solid-state green body, slurry is formed by curing solidifying by certain time at 65 DEG C
Glue.Then demoulding can be obtained shown in Fig. 1 and Fig. 2 and have compared in the open circles laminar film supporting surface and helical form of high green
Support body green body.
(4) upper and lower surface is pressed from both sides with two panels open circles laminar film supporting surface green body all apply the inner supporting body green body of clay such as
Fig. 1 is combined, the green body that will be combined, and is sintered in 1200 DEG C of temperature tripping in kilns, soaking time 1h, so that it may obtain such as Fig. 1
Shown in hollow disk-shaped Porous supporter.
(5) titanium oxide layer is prepared by infusion process on support external surface, 3-25 μm of thicknesses of layers, modifies film thickness
Between 3-30nm, membrane aperture 1.5-2000nm, 4h is dried after the completion of film forming at a temperature of 70 DEG C, then enters kiln in 450 DEG C of temperature
Lower sintering, soaking time 2h obtain the hollow plate type ceramic film of the helical duct.
Embodiment 3
(1) to weigh each substance by following weight percent spare: carborundum powder (5 μm, 97.3wt%), organic monomer propylene
Amide AM (1.9wt%), crosslinking agent methylene-bisacrylamide MBAM (0.25wt%), dispersing agent lemon acid amide AC
(0.3wt%), tetramethylethylenediamine TEMED (0.15wt%), concentration are the initiator Ammonium Persulfate 98.5 APS of 5% aqueous solution
(0.1wt%).
(2) the organic monomer acrylamide (AM) that will have been weighed, crosslinking agent methylene-bisacrylamide (MBAM), dispersing agent
Lemon acid amide (AC) and the 47wt% water of the above spare substance total weight is mixed to get premixed liquid, then by premixed liquid with weighed
Ball milling 2.5h in (5 μm, 97.3wt%) addition ball mills of carborundum powder, it is spare to obtain high solid phase, the slurry of low viscosity.
(3) catalyst tetramethylethylenediamine (TEMED), the initiator Ammonium Persulfate 98.5 weighed is added in the good slurry of ball milling
(APS), the metal die for injecting supporting surface and inner supporting body after mixing evenly, forms the organic monomer polymerization crosslinking in suspended substance
Three-dimensional net structure, so that liquid slurry be made to be transformed into solid-state green body, slurry is formed by curing solidifying by certain time at 45 DEG C
Glue.Then demoulding can be obtained shown in Fig. 1 and Fig. 2 and have compared in the open circles laminar film supporting surface and helical form of high green
Support body green body.
(4) upper and lower surface is pressed from both sides with two panels open circles laminar film supporting surface green body all apply the inner supporting body green body of clay such as
Fig. 1 is combined, the green body that will be combined, and is sintered in 1450 DEG C of temperature tripping in kilns, soaking time 2h, so that it may obtain such as Fig. 1
Shown in hollow disk-shaped film support.
(5) silica coating is prepared by spray coating method on support external surface, 3-25 μm of thicknesses of layers, modifies film thickness
Between degree 3-30nm, membrane aperture 1.5-2000nm, 4h is dried after the completion of film forming at a temperature of 80 DEG C, then enters kiln in 1200 DEG C of temperature
The lower sintering of degree, soaking time 2h obtain the hollow plate type ceramic film of the helical duct.
Referring to Fig. 1 and Fig. 2, in the present invention, inner supporting body 1 is encapsulated in therebetween by two film supporting surfaces 2,1 cross sectional shape of inner supporting body
It can be rectangle, polygon and ellipse, the spiral thickness h of everywhere and the size of channel span b can be according to traffic requirement and intensity
It is required that adjusting, the thickness h and channel span b at every place can be identical, can not also be identical, size range 0.1-10000mm.
As a preferred embodiment of the invention, the inner supporting body 1 and two film supporting surfaces 2 are in disc-shaped.
Work principle of filter of the invention:
With reference to Fig. 1, first the centre bore of two film supporting surfaces 2 (can be circle, square hole etc., preferably circular hole) upper and lower surface
Then sealing applies a draft, so that the helical duct in the inner supporting body inside film is formed negative pressure, in the work of film internal and external pressure difference
Under, phase (liquid or gas) need to be filtered and separated by film surface, the separation of transmission is mutually gathered in helical duct, in the work of draft
Under, the separate substance in helical duct flows to end coils, and by the opening of centre bore, (i.e. gutter channel is end coils in
The opening that heart hole is formed about, the opening are connected to centre bore) at collect.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all at this
Under the inventive concept of invention, using equivalent structure transformation made by description of the invention and accompanying drawing content, or directly/use indirectly
It is included in other related technical areas in scope of patent protection of the invention.
Claims (10)
1. a kind of hollow plate type ceramic film of helical duct, which is characterized in that it includes an inner supporting body and two hollow laminar film supports
Face, two film supporting surfaces are encapsulated in inner supporting body upper and lower surface;The inner supporting body is the helical structure of integral type, the axial direction that end coils are formed
Hole is not less than the hollow dimension of film supporting surface, and the gutter channel that end coils are formed is connected to two film supporting surface hollow parts.
2. the hollow plate type ceramic film of helical duct according to claim 1, which is characterized in that the spiral knot of the inner supporting body
The spiral thickness h of the everywhere of structure and the size range of channel span b are 0.1-10000mm.
3. the hollow plate type ceramic film of helical duct according to claim 1, which is characterized in that the inner supporting body cross sectional shape
For rectangle, polygon or ellipse.
4. the hollow plate type ceramic film of helical duct according to claim 1, which is characterized in that the inner supporting body and two film branch
Support face is in disc-shaped.
5. a kind of preparation method of the hollow plate type ceramic film of helical duct, which comprises the following steps:
(a), by organic monomer acrylamide (AM), crosslinking agent methylene-bisacrylamide (MBAM), dispersing agent lemon acid amide
(AC) and water is mixed to get premixed liquid according to a certain percentage;Ball mill is added in ceramic powder and premixed liquid by a certain percentage again
In, it is spare to obtain high solid phase, the slurry of low viscosity by ball milling 1-4h;
(b), catalyst tetramethylethylenediamine, initiator Ammonium Persulfate 98.5 is added in the good slurry of ball milling according to a certain percentage, is stirred
After uniformly in the mold of the metal die or other non-porous materials of the hollow laminar film supporting surface of injection and helical form inner supporting body;Make
Organic monomer polymerization crosslinking in suspended substance forms three-dimensional net structure, to make liquid slurry be transformed into solid-state green body, in 40-
Slurry is formed by curing gel by certain time at 80 DEG C;Then demoulding obtains hollow laminar film supporting surface and helical form inner supporting body
Green compact;
(c), group is carried out with the inner supporting body green body that two panels one upper and lower surface of hollow laminar film supporting surface green body folder all applies clay
It closes, the green body that will be combined, is sintered in 400-1800 DEG C of temperature tripping in kiln, soaking time 1-5h, obtain hollow platy support
Body;
(d) preparative separation film layer, the material of separation membrane layer include aluminum oxide, silicon carbide on hollow platy support external surface
Matter, cordierite, zirconium oxide, siliceous and titanium dioxide matter;The method of preparative separation film includes infusion process, spray coating method
And spin-coating method enters kiln sintering, finally obtains the hollow circular plate type of the helical duct after being covered with the supporter drying of separation membrane layer
Ceramic membrane.
6. the preparation method of the hollow plate type ceramic film of helical duct according to claim 5, which is characterized in that step (a)
In the ceramic powder include alumina powder, silicon carbide powder, cordierite powder, Zirconium oxide powder, titania powder,
SiO 2 powder.
7. the preparation method of the hollow plate type ceramic film of helical duct according to claim 6, which is characterized in that step (a)
In the ceramic powder pore creating material, any one of the pore creating material in silicon carbide, graphite, starch.
8. the preparation method of the hollow plate type ceramic film of helical duct according to claim 5, which is characterized in that step (c)
In sintering after the ruler of the spiral thickness h of the everywhere of the helical structure of inner supporting body and channel span b in hollow platy supporter
Very little range is 0.1-10000mm.
9. the preparation method of the hollow plate type ceramic film of helical duct according to claim 5, which is characterized in that step (c)
In sintering after in hollow platy supporter the cross sectional shape of inner supporting body be rectangle, polygon or ellipse.
10. the preparation method of the hollow plate type ceramic film of helical duct according to claim 5, which is characterized in that in described
Support body and two film supporting surfaces are in disc-shaped.
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CN112159239A (en) * | 2020-09-28 | 2021-01-01 | 景德镇陶瓷大学 | Preparation method of roll type ceramic membrane support and ceramic membrane product thereof |
CN112675712A (en) * | 2020-12-10 | 2021-04-20 | 景德镇陶瓷大学 | Preparation method of roll-type ceramic membrane, prepared product and filtration water purifier |
CN114053877A (en) * | 2020-08-01 | 2022-02-18 | 常启兵 | Preparation method of disc-type ceramic membrane support and ceramic membrane product thereof |
CN114311225A (en) * | 2022-01-18 | 2022-04-12 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and high-pressure slip casting method thereof |
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