CN106631044A - Method for shaping gradient-straight-hole double-layer asymmetric ceramic oxygen separation membrane - Google Patents
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Abstract
The invention provides a method for shaping a gradient-straight-hole double-layer asymmetric ceramic oxygen separation membrane by a freeze drying and tape casting method. According to the method, a tape casting process and a gradient straight hole forming process by freeze drying are combined, a raw membrane band body in a specific thickness is prepared by the tape casting process and is then transferred onto a low-temperature freezing bed; a water-base slurry is quickly frozen and cured on the freezing bed, and in the cuing process, gradient straight ice crystals are formed inside the raw membrane band body; the raw membrane band body is finally transferred into a vacuum kettle, the ice crystals in the raw membrane band body is directly evaporated into vapor in the low-temperature and vacuum condition, and the gradient straight holes are reserved at the positions of the ice crystals. The method has the advantages that the asymmetric membrane with the gradient straight hole structures is low in tortuosity, high in porosity and the like, remarkable reduction of concentration polarization in the ceramic oxygen separation membrane is hopeful, and oxygen penetrating quality and energy utilization rate of the ceramic oxygen separation membrane are increased.
Description
Technical field
The present invention relates to gas separation membrane field, more particularly to a kind of shaping of the asymmetric ceramic oxygen separation membrane of gradient straight hole
Method.
Background technology
Oxygen is important industrial chemicals, is needed during fossil energy processing and conversion, metallic article machine-shaping etc.
Consume a large amount of oxygen.Traditional cryogenic fractionation technology and pressure swing adsorption are due to initial outlay is huge, equipment is complicated
And energy consumption it is higher the shortcomings of, constrain the extensive popularization of above-mentioned oxygenerating technology.Ceramic oxygen separation membrane oxygenerating technology is relative to biography
The oxygen technique processed of system is expected to reduce by more than 30% system energy consumption, of increased attention, and achieves major progress.
Ceramic oxygen separation membrane Oxygen permeation process is mainly subject to Surface Oxygen exchange process, body diffusion process and gas diffusion process
Impact.The structure and configuration only rationally studied, design and prepare ceramic oxygen separation membrane can just significantly improve ceramic oxygen separating
The oxygen permeability of film and the comprehensive benefit of system.
When Oxygen permeation process is subject to body diffusion process to control, reducing thickness can significantly improve its Oxygen permeation speed, when
When film is relatively thin, introduce homogeneity supporter to improve the mechanical strength and impact resistance of film；But when thickness is reduced to critical thickness,
Further reduce thickness affects less to its oxygen permeability, now can enter one by surface modification oxygen exchange process catalyst
Step improves its oxygen permeability.Meanwhile, the asymmetric ceramic oxygen separation membrane prepared using methods such as traditional dry pressing, the tape castings
There is tortuosity height, the low shortcoming of porosity in support body, reduce gas and supporting internal transmission speed, under running conditions
Serious concentration polarization problem is easily faced, its oxygen permeability is restricted.Therefore, optimize ceramic oxygen separation membrane structure and then improve
Ceramic oxygen separation membrane performance is a problem for being worth exploring.
The content of the invention
The technical problem to be solved proposes a kind of double-deck asymmetric ceramic oxygen separation membrane of gradient straight hole
Forming method.The present invention increased on the basis of traditional casting molding processes and be frozen into ice crystal, vacuum sublimation except ice crystal pore-forming
Technique, obtains the ceramic film support with gradient straight hole structure, and with reference to dense film thin layer forming technique gradient straight hole is prepared
The asymmetric ceramic oxygen separation membrane of double-decker.
The present invention proposes a kind of forming method of the asymmetric ceramic oxygen separation membrane of gradient straight hole double-decker, concrete steps
It is as follows：
（1）With ammonium polyacrylate as dispersant, polypropylene is as binding agent and polysaccharide is slurry thickener, be dissolved in from
Group water solution is formed in sub- water；Group water solution, ball milling mixing is added uniformly to obtain stable aqueous-based ceramic slurry ceramic powder；
In the aqueous-based ceramic slurry, by mass, the ceramic powder accounts for 30 ~ 85%, and the deionized water accounts for 10 ~ 65%, described poly-
Ammonium acrylate accounts for 0.2 ~ 5%, and the polypropylene accounts for 1 ~ 5%, and the polysaccharide accounts for 0.1 ~ 2%；
（2）The bubble that vacuum outgas removes introducing during ball milling mixing is carried out to aqueous-based ceramic slurry using vavuum pump；In stream
Prolong and spread on coating machine polymeric membrane band, pull polymeric membrane band to drive slurry to advance and realize casting processes, adjust doctor knife coater and scrape
Knife up degree controls film forming thickness；
（3）The idiosome of flow casting molding is transferred in freezing bed and realizes slurry curing film forming；
（4）Ceramic membrane band idiosome after solidification is transferred in vacuum kettle, it is straight by solid-state ice crystal under low temperature and vacuum condition
Jie Sheng Huawei vapor realizes dry, pore-forming；
（5）After ceramic membrane band idiosome is fully dried, it is taken out from vacuum kettle, ceramic membrane idiosome is cut into into specific dimensions,
It is then transferred into pre-sintering in high temperature furnace and makes gradient straight hole supporter；
（6）Functional layer is coated on gradient straight hole supporter using dense film thin layer forming technique, high temperature co-firing knot prepares ladder
The asymmetric ceramic oxygen separation membrane of degree straight hole double-decker.
Preferably, described ceramic powder（Active material）Can be all ceramic oxygen separation membranes not reacted with water
Material, such as monophase materialses Ln1-xAxM1-yByO3-δ(LAMBO, wherein Ln are lanthanide series La, Pr, Sm, Ce etc., and A is alkaline-earth metal
Elements Sr, Ba, Ca, Mg etc., M and B are transition metal Co, Fe, Mn, Ni, Cu etc.), double-phase composite（Led by oxonium ion
Body and electronic conductor or mixed conductor LAMBO compositions）.
Preferably, the average grain diameter of the ceramic powder is 0.05 ~ 10 micron.
Preferably, described dispersant can be all ammonium salt dispersants.
Preferably, described binding agent can be all water-soluble binders, such as polypropylene, polyvinyl alcohol, polyvinyl alcohol
Butyral, polyvinylpyrrolidone etc..
Preferably, described thickener（Slurry stabilizer）Can be all water-soluble polysaccharide type organics.
Preferably, described freezing bed tempertaure is subzero 70 ~ zero degree.
Preferably, the temperature of described vacuum kettle is subzero 70 ~ zero degree, and the pressure of the vacuum kettle is 50 ~ 1000 Pa.
Preferably, described dense film thin layer forming technique include but is not limited to dip coating techniques, screen printing technique,
Chemical vapour deposition technique, physical gas phase deposition technology, technique for atomic layer deposition, electrochemical deposition technique etc..
Preferably, step（5）Described in pre-sintering temperature be 700 ~ 1200 DEG C, the time be 0.5 ~ 10h.
Preferably, step（6）Described in high temperature co-firing junction temperature be 1200 ~ 1700 DEG C, the time be 2 ~ 20h.
Compared with prior art, the present invention is more with ceramic powder, water, ammonium salt dispersant, water-soluble binder and water solubility
Carbohydrate thickener is raw material, after mixing, grinding, freeze-drying curtain coating, vacuum sublimation pore-forming, obtains being tied with gradient straight hole
The ceramic supporting body of structure.In the present invention, dense film thin layer forming technique ceramic membrane of gradient straight hole structure with made by is adopted to be
Prepared by supporter has the asymmetric ceramic oxygen separation membrane of gradient straight hole structure.
Because the asymmetric ceramic oxygen separation membrane of gradient straight hole structure has high porosity, low tortuosity obtained in the present invention
The advantages of, therefore with larger Oxygen permeation flux.In addition, the present invention Surface Oxygen exchange catalysts are coated in dense film can
To significantly improve Surface Oxygen exchange rate, and then improve the Oxygen permeation flux of oxygen separation membrane.Experiment shows that the present invention is obtained terraced
When degree straight hole structure anisotropic membrane is used for oxygen separating, when supporter exposes in atmosphere, when compacted zone is helium, 950oDuring C,
The Oxygen permeation speed of film is 0.105 cm3 cm-2 min-1, compared with symmetrical dense film, Oxygen permeation speed improves 81%；Causing
After close layer coating oxygen exchange catalysts, the Oxygen permeation speed of film is significantly increased to 0.780 cm3 cm-2 min-1, with symmetrical densification
Film is compared, and Oxygen permeation speed improves 1100%.
Description of the drawings
Fig. 1 is the process flow diagram that the present invention prepares double-deck asymmetric ceramic oxygen separation membrane.
Fig. 2 is cross-sectional scanning electron microscope (SEM) photo of double-deck asymmetric ceramic oxygen separation membrane
Fig. 3 is dense functional layer surface Scanning Electron microscope（SEM）Photo.
Fig. 4 is the ceramic oxygen separation membrane performance comparison that traditional dry pressing is prepared with freeze-drying the tape casting.
Specific embodiment
（1）Ammonium polyacrylate, polypropylene and polysaccharide are dissolved in deionized water and form the aqueous solution；Gd2 O3 will be aoxidized
Cerium oxide（Ce0.9Gd0.1O1.95, GDC）The lanthanum manganate of powder and oxidation strontium doping（(La0.8Sr0.2)0.95MnO3-δ, LSM）Powder
In mass ratio 62.2:37.8 ball milling mixings uniformly make GDC-LSM composite ceramic materials；GDC-LSM composite ceramic materials are added
Enter it is above-mentioned made by the aqueous solution, ball milling mixing uniformly obtains stable aqueous-based ceramic slurry, deionized water in aqueous-based ceramic slurry,
The mass content of ceramic powder and organic matter is respectively 32.2%, 57.8% and 10.0%, organic matter be 4.5% ammonium polyacrylate, 4%
Polypropylene and 1.5% polysaccharide；
（2）Aqueous-based ceramic slurry is placed in vavuum pump, vacuum outgas removes the gas introduced during ball milling mixing in 10 minutes
Bubble；
（3）Polymeric membrane band is spread on curtain coating coating machine, with 0.1 m min-1It is real that speed pulls film strips to drive slurry to advance
Existing casting processes, adjust doctor knife coater scraper and highly control the mm of film forming idiosome thickness 1.5；
（4）The film strips idiosome of flow casting molding is transferred in subzero 60 DEG C of freezing bed and realizes that aqueous-based ceramic slurry freezes admittedly
Change；
（5）Ceramic membrane band idiosome after solidification is transferred in vacuum kettle, solid-state is passed through under the conditions of 70 Pa, subzero 35 DEG C
Ice directly rises Huawei's vapor and realizes drying of the ceramic membrane with idiosome, pore-forming；
（6）Holding makes ceramic membrane band idiosome fully be dried for 10 hours, then takes out it from vacuum kettle；
（7）Ceramic membrane is cut into into the disk of a diameter of 20 mm, then disk pre-sintering in 5 hours is incubated at 1100 DEG C and is made
Gradient straight hole supporter；
（8）GDC-LSM ultrathin functional layers are coated on gradient straight hole supporter using screen printing technique, in 1500 DEG C of guarantors
Warm 5 hours co-sinterings make supporter（0.9 mm）/ functional layer（0.02 mm）Double-decker ceramics oxygen separation membrane.
（9）Using be cleaned by ultrasonic instrument in absolute ethyl alcohol ultrasound 30 minutes cleaning made by disc-shaped ceramics oxygen separation membrane,
Then by the dense functional layer of disc-shaped sample down, porous supporting body layer upward, with high temp glass ring at 1020 DEG C by this piece
Shape membrane sealing is in the centre of two alundum tubes.Then it is reduced to test temperature（875-950℃）, in the dense functional layer side of film and
Porous supporting body layer side each leads into purge gass（Helium）And air, the ceramic oxygen separation membrane of test is under air/helium gradient
Oxygen permeation speed.The oxygen partial pressure difference of film both sides causes oxygen from high keto sectional pressure side（Air side）Densified functional layer penetrates into hypoxemia
Partial pressure end is come, the purge gass of the oxygen utilization dense functional layer side being permeated（Helium）Gas-chromatography is brought into, using gas phase color
The composition and concentration of spectrometry gas, then by the Oxygen permeation speed of the composition of tail gas, concentration and flow relocity calculation membrane.
In order to further improve the performance of ceramic oxygen separation membrane, using screen printing technique by the SDC-LSCF of 20 microns of thickness
Surface Oxygen exchange catalysts are coated on gradient straight hole supporter, are then allowed to and dense functional layer within 2 hours in 1100 DEG C of insulations
Combine closely.Then using be cleaned by ultrasonic instrument in absolute ethyl alcohol ultrasound 30 minutes clean, then by porous catalyst layer down,
Porous supporting body layer upward, with high temp glass ring 1020 DEG C by this sheet membrane sealing in the centre of two alundum tubes.Finally adopt
Use step（9）In apparatus and method obtain film Oxygen permeation speed.
Claims (8)
1. a kind of forming method of the asymmetric ceramic oxygen separation membrane of gradient straight hole double-decker, comprises the following steps that：
(1) with ammonium polyacrylate as dispersant, polypropylene is as binding agent and polysaccharide is slurry thickener, is dissolved in deionization
Group water solution is formed in water；Group water solution, ball milling mixing is added uniformly to obtain stable aqueous-based ceramic slurry ceramic powder；Institute
In stating aqueous-based ceramic slurry, by mass, the ceramic powder accounts for 30 ~ 85%, and the deionized water accounts for 10 ~ 65%, described poly- third
Olefin(e) acid ammonium accounts for 0.2 ~ 5%, and the polypropylene accounts for 1 ~ 5%, and the polysaccharide accounts for 0.1 ~ 2%；
(2) bubble that vacuum outgas removes introducing during ball milling mixing is carried out to aqueous-based ceramic slurry using vavuum pump；In stream
Prolong and spread on coating machine polymeric membrane band, pull polymeric membrane band to drive slurry to advance and realize casting processes, adjust doctor knife coater and scrape
Knife up degree controls film forming thickness；
(3) idiosome of flow casting molding is transferred in freezing bed and realizes slurry curing film forming；
(4) the ceramic membrane band idiosome after solidification is transferred in vacuum kettle, it is straight by solid-state ice crystal under low temperature and vacuum condition
Jie Sheng Huawei vapor realizes dry, pore-forming；
(5) after ceramic membrane band idiosome is fully dried, it is taken out from vacuum kettle, ceramic membrane idiosome is cut into into specific dimensions,
It is then transferred into pre-sintering in high temperature furnace and makes gradient straight hole supporter；
(6) functional layer is coated on gradient straight hole supporter using dense film thin layer forming technique, high temperature co-firing knot prepares ladder
The asymmetric ceramic oxygen separation membrane of degree straight hole double-decker.
2. forming method according to claim 1, it is characterised in that described ceramic powder is that monophase materialses or two-phase are multiple
Condensation material.
3. forming method according to claim 1, it is characterised in that the average grain diameter of the ceramic powder is 0.05 ~ 10
Micron.
4. forming method according to claim 1, it is characterised in that described freezing bed tempertaure is subzero 70 ~ zero degree.
5. forming method according to claim 1, it is characterised in that the temperature of described vacuum kettle is subzero 70 ~ zero degree,
The pressure of the vacuum kettle is 50 ~ 1000 Pa.
6. forming method according to claim 1, it is characterised in that described dense film thin layer forming technique includes dipping
Paint-on technique, screen printing technique, chemical vapour deposition technique, physical gas phase deposition technology, technique for atomic layer deposition, electrochemistry
Deposition technique.
7. forming method according to claim 1, it is characterised in that step（5）Described in pre-sintering temperature be 700 ~
1200 DEG C, the time is 0.5 ~ 10h.
8. forming method according to claim 1, it is characterised in that step（6）Described in high temperature co-firing junction temperature be
1200 ~ 1700 DEG C, the time is 2 ~ 20h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108751950A (en) * | 2018-06-14 | 2018-11-06 | 哈尔滨工业大学 | A method of it is cast based on freezing and prepares Functional Graded Ceramics/metallic composite |
| CN109912314A (en) * | 2019-04-18 | 2019-06-21 | 武汉大学 | The hydrophobic membrane preparation method of energy-saving, environment-friendly and high-efficiency |
| CN109939256A (en) * | 2019-04-01 | 2019-06-28 | 南京华开生物科技有限公司 | A kind of asymmetric dressing for skin and preparation method thereof |
| CN114751725A (en) * | 2022-04-26 | 2022-07-15 | 景德镇陶瓷大学 | Preparation and application method of embedded flat ceramic membrane layer slurry |
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| CN1872794A (en) * | 2006-06-27 | 2006-12-06 | 哈尔滨工业大学 | Improved coating method for preparing membrane of oxide ceramics |
| CN101182233A (en) * | 2007-11-12 | 2008-05-21 | 中国科学院上海硅酸盐研究所 | Gradient porous ceramics film and method for preparing the same |
| CN103253982A (en) * | 2013-05-23 | 2013-08-21 | 上海大学 | Preparation method of tubular asymmetric oxygen-permeable membrane |
| CN103319182A (en) * | 2013-07-04 | 2013-09-25 | 清华大学 | High-performance solid oxide electrolytic tank support |
| CN104529448A (en) * | 2015-01-23 | 2015-04-22 | 景德镇陶瓷学院 | High-porosity high-permeability Nb2O5 ceramic membrane and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872794A (en) * | 2006-06-27 | 2006-12-06 | 哈尔滨工业大学 | Improved coating method for preparing membrane of oxide ceramics |
| CN101182233A (en) * | 2007-11-12 | 2008-05-21 | 中国科学院上海硅酸盐研究所 | Gradient porous ceramics film and method for preparing the same |
| CN103253982A (en) * | 2013-05-23 | 2013-08-21 | 上海大学 | Preparation method of tubular asymmetric oxygen-permeable membrane |
| CN103319182A (en) * | 2013-07-04 | 2013-09-25 | 清华大学 | High-performance solid oxide electrolytic tank support |
| CN104529448A (en) * | 2015-01-23 | 2015-04-22 | 景德镇陶瓷学院 | High-porosity high-permeability Nb2O5 ceramic membrane and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108751950A (en) * | 2018-06-14 | 2018-11-06 | 哈尔滨工业大学 | A method of it is cast based on freezing and prepares Functional Graded Ceramics/metallic composite |
| CN109939256A (en) * | 2019-04-01 | 2019-06-28 | 南京华开生物科技有限公司 | A kind of asymmetric dressing for skin and preparation method thereof |
| CN109939256B (en) * | 2019-04-01 | 2021-09-17 | 南京华开生物科技有限公司 | Asymmetric skin dressing and manufacturing method thereof |
| CN109912314A (en) * | 2019-04-18 | 2019-06-21 | 武汉大学 | The hydrophobic membrane preparation method of energy-saving, environment-friendly and high-efficiency |
| CN114751725A (en) * | 2022-04-26 | 2022-07-15 | 景德镇陶瓷大学 | Preparation and application method of embedded flat ceramic membrane layer slurry |
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Application publication date: 20170510 |