CN110342938A - A kind of preparation method of high throughput porous silicon carbide seperation film - Google Patents
A kind of preparation method of high throughput porous silicon carbide seperation film Download PDFInfo
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- CN110342938A CN110342938A CN201910668952.3A CN201910668952A CN110342938A CN 110342938 A CN110342938 A CN 110342938A CN 201910668952 A CN201910668952 A CN 201910668952A CN 110342938 A CN110342938 A CN 110342938A
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- silicon carbide
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- porous silicon
- seperation film
- separating layer
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 55
- 239000000835 fiber Substances 0.000 claims abstract description 29
- 230000007704 transition Effects 0.000 claims abstract description 19
- 238000005507 spraying Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- -1 diethylenetriamine pentaacetic acid aluminum Chemical compound 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000007921 spray Substances 0.000 claims description 26
- 229920003091 Methocel™ Polymers 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 14
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 14
- 239000000292 calcium oxide Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 14
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 14
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052863 mullite Inorganic materials 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- 239000012300 argon atmosphere Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 5
- 230000001680 brushing effect Effects 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000000428 dust Substances 0.000 abstract description 8
- 230000035699 permeability Effects 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000003245 coal Substances 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 230000004907 flux Effects 0.000 description 11
- 239000007789 gas Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 239000012528 membrane Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 229920000609 methyl cellulose Polymers 0.000 description 5
- 239000001923 methylcellulose Substances 0.000 description 5
- 238000002459 porosimetry Methods 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000004575 stone Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 241000406668 Loxodonta cyclotis Species 0.000 description 1
- WTBIAPVQQBCLFP-UHFFFAOYSA-N N.N.N.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O Chemical compound N.N.N.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O WTBIAPVQQBCLFP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
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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
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- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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Abstract
The present invention relates to a kind of preparation methods of high-throughput porous silicon carbide seperation film.Using the silicon carbide supporter of macropore as substrate, preparation has the silicon carbide film of unsymmetric structure, transition zone can be sacrificed using the conduct of diethylenetriamine pentaacetic acid aluminum fiber, the separating layer particle of the supporter and small particle that make large aperture is mutually matched, and overcomes separating layer particle endosmosis；The separating layer that silicon carbide film is prepared by the method for spraying during high-temperature calcination separating layer, while removing median fiber transition zone, simplifies the structure of silicon carbide film, prepares high-throughput porous silicon carbide seperation film.The silicon carbide seperation film prepared by this method while having both the supporter of macropore and the separating layer of aperture; and without intermediate layer; gas permeability is preferable; filtering accuracy is higher; preparation process is easy to operate, is easy to large-scale production, can be used for industrial dust purifying device; in industries such as coal chemical industry, steam power plant and metallurgical works, it is with a wide range of applications.
Description
Technical field
The invention belongs to high-temperature dust removal Material Fields, and in particular to a kind of preparation of silicon carbide seperation film.
Background technique
In recent years, with the development of industrial technology, industrial activity is more and more frequently, and air pollution phenomenon is also more and more brighter
Aobvious, national multiple areas frequently occur large area haze phenomenon.Fine particulates discharge is exceeded, it is considered to be causes haze existing
The immediate cause of elephant, but in the exhaust gas of industry discharge, not only contain a large amount of dust, the temperature of gas is also higher, and companion
With there is a poisonous and harmful chemical component such as nitrogen oxides, oxysulfide, handle it is relatively difficult, requirement for equipment and materials compared with
It is high.Silicon carbide has high mechanical strength, good heat resistance and corrosion resistance.It is prepared using carbofrax material for gas-solid
Isolated silicon carbide film, gas permeability and filtering accuracy with higher, separation operation process is simple, operating cost compared with
It is low.
103721578 A of patent CN discloses a kind of pure matter silicon carbide separation membrane preparation method of multichannel unsymmetric structure.
The pure matter silicon carbide film of unsymmetric structure, is tubulose multi-channel structure, and channel number significantly increases elementary membrane between 7-3000
Area and membrane tube intensity.Aperture is successively reduced using multiple transition zones using the method sprayed layer by layer in technique, can be prepared
The silicon carbide seperation film of different pore size.But when preparing the filter membrane of small-bore, since transition layer number is more, not only work
Skill preparation process is complex, and the silicon carbide film permeability prepared is also smaller.The silicon carbide film aperture finally prepared is 1 μ
M, porosity 50%, filtration of demineralized water flux are 6500 L/m3·h·bar.106083060 A of patent CN discloses a kind of list
Channel unsymmetric structure silicon carbide separates membrane preparation method, and it is 10 μm that partial size is coated on the supporter that aperture is 15 μm
Silicon-carbide particle, in order to prepare the complete silicon carbide film in surface, separating layer thickness increases to 1 mm, the carbonization finally prepared
Silicon fiml pore-size distribution is 2.8 μm, and gas permeability is 120 m3/m2·h·kPa。
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of high-throughput porous silicon carbide seperation film.
In order to reach goal of the invention, the technical solution of the present invention is as follows:
A kind of preparation method of high throughput porous silicon carbide seperation film, specific preparation process is as follows:
(1) diethylenetriamine pentaacetic acid aluminum fiber is mixed with methocel solution, prepares fiber transition zone after mixing evenly
Solution；
(2) silicon-carbide particle and sintering aid are mixed with methocel solution, prepares coating liquid after mixing evenly；
(3) it by the fiber transition zone solution in step (1), brushes in porous silicon carbide supporting body surface；
(4) coating liquid in step (2) is formed with spray gun spraying porous silicon carbide supporting body surface obtained by step (3) again
Silicon carbide seperation film；
(5) it by silicon carbide supporter obtained by step (4), is placed in atmosphere furnace and carries out high-temperature calcination.
Wherein:
Methocel solution mass concentration described in step (1) is 0.5-3 wt%, and diethylenetriamine pentaacetic acid aluminum fiber is in methyl
Mass concentration in fiber solution is 0.5-4 wt%.
Methocel solution mass concentration described in step (2) is 0.5-3 wt%, and silicon-carbide particle partial size is 5-15 μ
M, sintering aid are calcium oxide, zirconium oxide and mullite, and sintering aid partial size is 0.5-3 μm；Each object in methocel solution
The mass fraction of matter are as follows: silicon-carbide particle is 10-30 wt%, and calcium oxide is 0.1-0.5 wt%, and zirconium oxide is 0.1-0.5 wt%,
Mullite is 0.1-0.5 wt%.
Step (3) the silicon carbide support body aperture is 20-35 μm, and it is 1-5 times that step (3), which brushes number, is brushed every time
30 min are dried afterwards.
The distance between gun slot and silicon carbide supporter are 10-30 cm in step (4) spraying process, and spray pressure is
0.1-0.3 MPa, spray time are 4-8 s, are sprayed 1-4 times, every time dry 10-30 min after spraying.
Step (5) described calcination procedure are as follows: at 0-1200 DEG C, calcined in air atmosphere, heating rate 1-10
DEG C/min, 2-4 h is kept the temperature at 1200-1500 °C；Argon atmosphere is then turned to, continues to keep the temperature 2-6 h, last Temperature fall.
Beneficial effects of the present invention:
(1) the invention operating procedure is simple, and porous silicon carbide separates film properties and stablizes, and repeatability is high, and parameter is easily controllable, can be with
Amplify experiment, large-scale production.
(2) using diethylenetriamine pentaacetic acid aluminum fiber as transition zone, during the preparation process, can make macropore supporter and
Small particle separating layer particle is mutually matched, and effectively prevent being seeped into supporter in separating layer particle；During calcining separating layer,
Fiber transition zone can be efficiently removed, and only retained supporter and separating layer, simplified the structure of silicon carbide film, and having can sacrifice
The feature of transition zone.
(3) present invention, which uses macropore supporter and can sacrifice transition zone, prepares silicon carbide film, greatly improves carbonization
The gas permeability of silicon fiml, and the separating layer of small-bore ensure that and guarantee silicon carbide membrane separation efficiency.
Detailed description of the invention
Fig. 1 is the microcosmic scanning electron microscope (SEM) photograph of silicon carbide film in embodiment 1, transition zone section before a is calcined；Silicon carbide before b is calcined
Film section；Silicon carbide film surface after c calcining；Silicon carbide film section after d calcining.
Fig. 2 is silicon carbide film graph of pore diameter distribution in embodiment 2.
Fig. 3 is silicon carbide film profile scanning electron microscope in embodiment 2.
Fig. 4 is silicon carbide film profile scanning electron microscope in embodiment 3.
Fig. 5 is silicon carbide film surface scan electron microscope in embodiment 4.
Fig. 6 is silicon carbide film surface scan electron microscope in embodiment 5.
Specific embodiment
The present invention is done below with reference to embodiment and is further explained, the following example is merely to illustrate the present invention, but
It is not used to limit practical range of the invention.
Embodiment 1
(1) diethylenetriamine pentaacetic acid aluminum fiber is mixed with the methylcellulose of 0.5 wt%, after mixing evenly, obtains transition zone
Fiber solution mass concentration is 4 wt%.
It (2) is 10 wt% silicon carbide, 0.1 wt% calcium oxide, 0.1 wt% zirconium oxide and 0.1 wt% mullite point by content
Be dispersed in the methocel solution of 0.5 wt%, wherein the average grain diameter of silicon carbide powder be 5 μm, calcium oxide, zirconium oxide and
The average grain diameter of mullite is 0.5 μm, obtains coating liquid after mixing evenly.
(3) the fiber transition zone solution in step (1) is brushed to the silicon carbide supporting body surface for being 20 μm to aperture, brush
It applies 5 times, 30 min is then dried.
(4) coating liquid obtained in step (1) is sprayed into the supporting body surface in step (3), spray gun in spraying process
It mouthful is 10 cm at a distance from silicon supporter between carbonization, spray pressure is 0.1 MPa, and spray time is 8 s, sprays 4 times, often
Dry 30 min after secondary spraying.
(5) porous silicon carbide obtained in step (5) is separated and carries out high-temperature calcination, at 0-1200 DEG C, in air
It is calcined in atmosphere, heating rate is 1 DEG C/min, keeps the temperature 2 h at 1200 DEG C；Argon atmosphere is then turned to, continues to keep the temperature 4 h,
Last Temperature fall.
Experimental result: using Porosimetry PSDA-20 type, carries out aperture and flux point to porous silicon carbide seperation film
Analysis, air flux are 135 m3/m2HkPa, average pore size be 2.43 μm, Fig. 1 scanning electron microscope (SEM) photograph show separating layer with a thickness of
100 μm, be 0.3 μm of aluminum oxide dust rejection 99.9% to partial size, but connect between separating layer and supporter poor.
Embodiment 2
(1) diethylenetriamine pentaacetic acid aluminum fiber is mixed with the methylcellulose of 0.5 wt%, after mixing evenly, obtains diethyl three
Triamine pentaacetic acid aluminum fiber concentration of polymer solution is 0.5 wt%.
It (2) is 25 wt% silicon carbide, 0.2 wt% calcium oxide, 0.2 wt% zirconium oxide and 0.2 wt% mullite point by content
It is dispersed in the methocel solution of 2 wt%, wherein the average grain diameter of silicon carbide powder is 10 μm, calcium oxide, zirconium oxide and not
The average grain diameter for carrying out stone is 1 μm, obtains coating liquid after mixing evenly.
(3) the fiber transition zone solution in step (1) is brushed to the silicon carbide supporting body surface for being 30 μm to aperture, brush
It applies 1 time, 30 min is then dried.
(4) coating liquid obtained in step (1) is sprayed into the supporting body surface in step (3), spray gun in spraying process
It mouthful is 10 cm with the distance between silicon carbide supporter, spray pressure is 0.3 MPa, and spray time is 8 s, it sprays 4 times, often
Dry 30 min after secondary spraying.
(5) porous silicon carbide seperation film obtained in step (5) is subjected to high-temperature calcination, at 0-1200 DEG C, in air
It is calcined in atmosphere, heating rate is 1 DEG C/min, keeps the temperature 2 h at 1300 DEG C；Argon atmosphere is then turned to, heat preservation 2 is continued
H, last Temperature fall.
Experimental result: Fig. 2 uses Porosimetry PSDA-20 type, carries out aperture and flux to porous silicon carbide seperation film
Analysis, air flux are 236 m3/m2HkPa, average pore size are 3.48 μm, and Fig. 3 scanning electron microscopic picture shows separating layer thickness
120 μm, be 0.3 μm of aluminum oxide dust rejection 99.9% to partial size, forms good neck between separating layer and supporter and connects
It connects.
Embodiment 3
(1) diethylenetriamine pentaacetic acid aluminum fiber is mixed with the methylcellulose of 2 wt%, after mixing evenly, obtains Diethylenetriamine
Pentaacetic acid aluminum fiber concentration of polymer solution is 2 wt%.
It (2) is 25 wt% silicon carbide, 0.3 wt% calcium oxide, 0.3 wt% zirconium oxide and 0.3 wt% mullite point by content
It is dispersed in the methocel solution of 2 wt%, wherein the average grain diameter of silicon carbide powder is 10 μm, calcium oxide, zirconium oxide and not
The average grain diameter for carrying out stone is 0.5 μm, obtains coating liquid after mixing evenly.
(3) the fiber transition zone solution in step (1) is brushed to the silicon carbide supporting body surface for being 30 μm to aperture, brush
It applies 3 times, dry 30 min after brushing every time.
(4) coating liquid obtained in step (1) is sprayed into the supporting body surface in step (3), spray gun in spraying process
It mouthful is 20 cm with the distance between silicon carbide supporter, spray pressure is 0.3 MPa, and spray time is 8 s, sprays 3 times, often
Dry 30 min after secondary spraying.
(5) porous silicon carbide obtained in step (5) is separated and carries out high-temperature calcination, at 0-1200 DEG C, in air gas
It is calcined in atmosphere, heating rate is 5 DEG C/min, keeps the temperature 4 h at 1300 DEG C；Argon atmosphere is then turned to, continues to keep the temperature 6 h,
Last Temperature fall.
Experimental result: using Porosimetry PSDA-20 type, carries out aperture and flux point to porous silicon carbide seperation film
Analysis, air flux are 245 m3/m2HkPa, average pore size be 3.65 μm, 120 μm of thickness of Fig. 4 scanning electron microscope (SEM) photograph separating layer,
It is 0.3 μm of aluminum oxide dust rejection 99.9% to partial size, forms good neck connection between separating layer and supporter.
Embodiment 4
(1) diethylenetriamine pentaacetic acid aluminum fiber is mixed with the methylcellulose of 2 wt%, after mixing evenly, obtains Diethylenetriamine
Pentaacetic acid aluminum fiber concentration of polymer solution is 2 wt%.
It (2) is 30 wt% silicon carbide, 0.3 wt% calcium oxide, 0.3 wt% zirconium oxide and 0.3 wt% mullite point by content
It is dispersed in the methocel solution of 2 wt%, wherein the average grain diameter of silicon carbide powder is 10 μm, calcium oxide, zirconium oxide and not
The average grain diameter for carrying out stone is 1 μm, obtains coating liquid after mixing evenly.
(3) the fiber transition zone solution in step (1) is brushed to the silicon carbide supporting body surface for being 30 μm to aperture, brush
It applies 5 times, dry 30 min after brushing every time.
(4) coating liquid obtained in step (1) is sprayed into the supporting body surface in step (3), spray gun in spraying process
It mouthful is 20 cm with the distance between silicon carbide supporter, spray pressure is 0.3 MPa, and spray time is 8 s, sprays 3 times, often
Dry 30 min after secondary spraying.
(5) porous silicon carbide obtained in step (5) is separated and carries out high-temperature calcination, at 0-1200 DEG C, in air gas
It is calcined in atmosphere, heating rate is 1 DEG C/min, keeps the temperature 2 h at 1400 DEG C；Argon atmosphere is then turned to, continues to keep the temperature 4 h,
Last Temperature fall.
Experimental result: using Porosimetry PSDA-20 type, carries out aperture and flux point to porous silicon carbide seperation film
Analysis, air flux are 571 m3/m2HkPa, average pore size are 6.58 μm, and it is a small amount of that Fig. 5 scanning electron microscope (SEM) photograph shows that separating layer occurs
Excess agglomeration phenomenon, 120 μm of separating layer thickness, be 0.3 μm of aluminum oxide dust rejection 73.6%, separating layer and branch to partial size
Good neck connection is formed between support body.
Embodiment 5
(1) diethylenetriamine pentaacetic acid aluminum fiber is mixed with the methylcellulose of 3 wt%, after mixing evenly, obtains Diethylenetriamine
Pentaacetic acid aluminum fiber concentration of polymer solution is 1 wt%.
It (2) is 30 wt% silicon carbide, 0.5 wt% calcium oxide, 0.5 wt% zirconium oxide and 0.5 wt% mullite point by content
It is dispersed in the methocel solution of 3 wt%, wherein the average grain diameter of silicon carbide powder is 15 μm, calcium oxide, zirconium oxide and not
The average grain diameter for carrying out stone is 3 μm, obtains coating liquid after mixing evenly.
(3) the fiber transition zone solution in step (1) is brushed to the silicon carbide supporting body surface for being 35 μm to aperture, brush
It applies 3 times, dry 30 min after brushing every time.
(4) coating liquid obtained in step (1) is sprayed into the supporting body surface in step (3), spray gun in spraying process
It mouthful is 30 cm with the distance between silicon carbide supporter, spray pressure is 0.3 MPa, and spray time is 4 s, sprays 1 time, so
After 30 min are dried.
(5) porous silicon carbide obtained in step (5) is separated and carries out high-temperature calcination, at 0-1200 DEG C, in air
It is calcined in atmosphere, heating rate is 10 DEG C/min, keeps the temperature 2 h at 1500 DEG C；Argon atmosphere is then turned to, heat preservation 4 is continued
H, last Temperature fall.
Experimental result: using Porosimetry PSDA-20 type, carries out aperture and flux point to porous silicon carbide seperation film
Analysis, air flux are 1167 m3/m2HkPa, average pore size are 32.4 μm；Fig. 6 scanning electron microscope (SEM) photograph shows that separating layer occurred
Degree sintering, it is 34.2% that 120 μm of separating layer thickness, which are 0.3 μm of dust rejection to partial size, shape between separating layer and supporter
It is connected at good neck.
Claims (7)
1. a kind of preparation method of high throughput porous silicon carbide seperation film, which is characterized in that specific preparation process is as follows:
(1) diethylenetriamine pentaacetic acid aluminum fiber is mixed with methocel solution, diethylenetriamine pentaacetic acid aluminum fiber is in methyl
Mass concentration in fiber solution is 0.5-4 wt%, prepares fiber transition zone solution after mixing evenly；
(2) silicon-carbide particle and sintering aid are mixed with methocel solution, prepares coating liquid after mixing evenly；
(3) it by the fiber transition zone solution in step (1), brushes in porous silicon carbide supporting body surface；
(4) again by the coating liquid in step (2), with spray gun spraying porous silicon carbide supporting body surface obtained by step (3)；
(5) it by silicon carbide supporter obtained by step (4), is placed in atmosphere furnace and carries out high-temperature calcination.
2. a kind of preparation method of high-throughput porous silicon carbide seperation film according to claim 1, which is characterized in that step
(1) the methocel solution mass concentration described in is 0.5-3 wt%.
3. a kind of preparation method of high-throughput porous silicon carbide seperation film according to claim 1, which is characterized in that step
(2) the methocel solution mass concentration in coating liquid is 0.5-3 wt%, and silicon-carbide particle partial size is 5-15 μm, and sintering helps
Agent is calcium oxide, zirconium oxide and mullite, and sintering aid partial size is 0.5-3 μm.
4. a kind of preparation method of high-throughput porous silicon carbide seperation film according to claim 3, which is characterized in that step
(2) mass fraction of each substance in methocel solution are as follows: silicon-carbide particle is 10-30 wt%, and calcium oxide is
0.1-0.5 wt%, zirconium oxide are 0.1-0.5 wt%, and mullite is 0.1-0.5 wt%.
5. a kind of preparation method of high-throughput porous silicon carbide seperation film according to claim 1, which is characterized in that step
(3) the silicon carbide support body aperture is 20-35 μm, and it is 1-5 times that step (3), which brushes number, dry 30 after brushing every time
min。
6. a kind of preparation method of high-throughput porous silicon carbide seperation film according to claim 1, which is characterized in that step
(4) the distance between gun slot and silicon carbide supporter are 10-30 cm in spraying process, and spray pressure is 0.1-0.3 MPa,
Spray time is 4-8 s, is sprayed 1-4 times, every time dry 10-30 min after spraying.
7. a kind of preparation method of high-throughput porous silicon carbide seperation film according to claim 1, which is characterized in that step
(5) calcination procedure are as follows: at 0-1200 DEG C, to be calcined in air atmosphere, heating rate is 1-10 DEG C/min,
2-4 h is kept the temperature at 1200-1500 DEG C；Argon atmosphere is then turned to, continues to keep the temperature 2-6 h, last Temperature fall.
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