CN103381338B - Ceramic flat membrane supporting body and production method thereof - Google Patents
Ceramic flat membrane supporting body and production method thereof Download PDFInfo
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- CN103381338B CN103381338B CN201310325539.XA CN201310325539A CN103381338B CN 103381338 B CN103381338 B CN 103381338B CN 201310325539 A CN201310325539 A CN 201310325539A CN 103381338 B CN103381338 B CN 103381338B
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Abstract
The invention discloses a ceramic flat membrane supporting body and a production method thereof. The ceramic flat membrane supporting body is formed by two layers of flat membranes, the left lateral wall, the right lateral wall and at least a supporting column; the two layers of flat membranes, the left lateral wall and the right lateral wall form into a flat-pipe-shaped structure; the supporting column is arranged between the two layers of flat membranes; the flat membranes which are in asymmetric structures comprise surface layers of sponge hole structures and internal layers of finger-shaped hole structures; separation selectivity, permeation flux and mechanical strength of the flat membranes are high. The production method of the ceramic flat membrane supporting body comprises preparing slurry, producing dies through a phase inversion method, forming through a die pressing method and sintering. The production technology is easy and flexible, the costs are low, the dies are cheap, the replacing is convenient, a plurality of assemblies in different sizes can be formed at one time, and the production efficiency is high.
Description
Technical field
The present invention relates to a kind of ceramic film support and preparation method thereof, be specifically related to a kind of earthenware slab film support and preparation method thereof.
Background technology
UF membrane utilizes the Selective Separation of film to realize the separation of the different component of feed liquid, purifying, concentrated process, in this course, the change of phase do not occur, therefore has the features such as efficient, energy-conservation, apply increasingly extensive.The diffusion barrier that membrane separation technique adopts can be divided into organic film substantially according to material therefor and take ceramic membrane as the inoranic membrane of representative.Compared with organic film, ceramic membrane, owing to having high temperature resistant, the feature such as solvent resistant, acid-alkali-corrosive-resisting, has achieved large-scale application at many engineering fields, and has achieved good economic results in society.
From structure, mostly ceramic membrane common is at present tubular membrane, multi-channel membrane and hollow-fibre membrane, and Flat Membrane is compared less.But, Flat Membrane in specific occasion particularly the field such as membrane bioreactor there is very high application prospect, earthenware slab film is large due to its mechanical strength, can mechanical scrub, can greatly improve its service life.
Current domestic earthenware slab film manufacturing enterprise is few, the more common earthenware slab membrane module being the bright electricity house of Amada Co., Ltd. and producing on market, be applied in fields such as Industrial Wastewater Treatment, in addition, also there are Patents about earthenware slab film and product in SanDa film Science company, Henan Fang Zhouci industry Co., Ltd etc.
Chinese patent CN102596374A and CN102858440A discloses the employing earthenware slab film assembling film separator of Amada Co., Ltd.'s bright electricity house exploitation, by modularized design, reduces film blocking, reduces the load in filter operation, improve separative efficiency.
Chinese patent CN102688700A has prepared a kind of earthenware slab film support, is made up of two Flat Membrane, between leave certain space, be dispersed with at least one support column in space, preparation method adopt the technique of mixing for raw material rear extrusion molding is obtained.
Shaanxi Tech Univ with aluminium oxide, kaolin and talcum etc. for raw material, compression molding method is adopted to prepare plate type ceramic film and be applied to the field such as oily waste water, dyeing waste water, demonstrate good handling property, by preparing transition zone, separating layer controls ceramic membrane aperture, realizes the processing target of expection.
Comprehensive existing patent, literature research and market product, can find, plate type ceramic film main types has two kinds, individual Flat Membrane and two Flat Membrane combinations, the latter obviously applies convenient, product forming technique is mainly based on compression molding, extrusion molding and flow casting molding, and production cost is high, and the film in the supporter that these techniques obtain is symmetric membrane.In symmetric membrane, aperture is identical everywhere, pore size distribution even, and can meet the requirement of separation selectivity, but in symmetric membrane, resistance is identical, is unfavorable for Liquid Penetrant everywhere, filter efficiency is low.
Summary of the invention
In view of this, be necessary for the problems referred to above, a kind of earthenware slab film support and preparation method thereof is provided.
To achieve these goals, the present invention adopts following technical scheme:
A kind of earthenware slab film support, comprise 2 layers of Flat Membrane, left side wall, right side wall and at least one support column, described 2 layers of Flat Membrane, left side wall and right side wall form flat tubular structure, and described support column is between 2 layers of Flat Membrane; Described Flat Membrane is dissymmetrical structure, comprises the top layer of sponge pore structure and the internal layer of finger-like pore structure.
As a kind of preferred embodiment of earthenware slab film support of the present invention, the thickness of described Flat Membrane is 1.5-4.75mm, the thick 1-10 μm in described top layer.
As the one more preferably embodiment of earthenware slab film support of the present invention, the long 10-100cm of described earthenware slab film support, wide 2-40cm, thick 5-10mm.
As a kind of preferred embodiment of earthenware slab film support of the present invention, described support column is column or strip.
As a kind of preferred embodiment of earthenware slab film support of the present invention, described support column has multiple.
As a kind of preferred embodiment of earthenware slab film support of the present invention, there is multiple delivery port at described flat tubular structure two ends.
A preparation method for earthenware slab film support, comprises the following steps:
Prepared by A, slurry: binding agent and stirring solvent are dissolved, then add ceramic raw material, dispersant, obtain slurry after ball milling mixing 2-24h, deaeration 2-10h, slurry viscosity is between 10000 ~ 20000mPas;
B, phase inversion masking: with template flat board to above-mentioned slurry knifing, scraping film temperature is 10-50 DEG C, and scraping film thickness is 1-5mm, leaves standstill 0-3min in atmosphere, then solidify 0.5-2h after knifing in non-solvent, takes out and dries, obtain the half of film containing protuberance;
C, die pressing are shaping: on protuberance, apply one deck stickum, adopt die pressing that half of for two panels film is become green compact relative to adhesion;
D, sintering: under the condition of 1000-1800 DEG C, sinter above-mentioned green compact, insulation 2-20h, obtains earthenware slab film support;
Wherein, the mass ratio of each component of earthenware slab film support is as follows: binding agent 1, solvent 2-6, ceramic raw material 2-10; The quality of dispersant is the 0.2-5% of ceramic powder quality.
As a kind of preferred embodiment of the preparation method of earthenware slab film support of the present invention, the porosity of described earthenware slab film support is at 10-70%, and average pore size is 0.2-50 μm.
Described ceramic raw material is one or more in aluminium oxide, zirconia, titanium oxide, silica, diatomite, cocoon green stone, mullite; Described binding agent is the one in polysulfones or polyether sulfone; Solvent is 1-METHYLPYRROLIDONE or dimethylacetylamide; Dispersant is PVP, triethanolamine or polyvinyl alcohol.
As a kind of preferred embodiment of the preparation method of earthenware slab film support of the present invention, described template flat board is that rectangle or round rectangle are dull and stereotyped, template flat board there is the recess that some grades are dark, recess is cylindric, cube or strip, and the limit place that a group of template flat board is relative is strip recess.
As the one more preferably embodiment of the preparation method of earthenware slab film support of the present invention, described template flat board is made up of Kynoar, polytetrafluoroethylene (PTFE), silica gel, plastics, glass, timber or metal material.Template slab construction is simple, material is easy to get, it is easy to make, it is convenient to change, and by changing different templates, can prepare the earthenware slab film support that size, structure etc. are different.
Earthenware slab film support of the present invention, its Flat Membrane has the microscopic appearance of dissymmetrical structure, namely there is the relatively fine and close cortex in surface and inner fingers pore size distribution, the former can provide higher separation selectivity, the latter's short texture, porosity is high, and finger-like pore structure is beneficial to Liquid Penetrant, higher permeation flux can be provided, therefore higher than the ceramic membrane filter efficiency of homogeneous structural; The support column of inner distribution can the mechanical strength of effective guarantee earthenware slab film support; Be easy to further preparative separation layer in Flat Membrane; Earthenware slab film support is easy to cleaning, long service life.
The preparation method of earthenware slab film support of the present invention, phase inversion and die pressing are combined, obtain the earthenware slab film support of the Flat Membrane with dense skin and loose internal layer, simple process is flexible, cost is lower, mould is cheap, it is convenient to change, can the assembly of the multiple different size of one-shot forming, and production efficiency is high.
Accompanying drawing explanation
Fig. 1 is the side view of the embodiment 1 of earthenware slab film support of the present invention;
Fig. 2 is the structural representation of the half of film in embodiment 1;
Fig. 3 is the structural representation of template flat board in embodiment 1;
Fig. 4 is the micro-structure diagram of embodiment 1 flat sheet membranes;
Fig. 5 is the structural representation of the half of film in the embodiment 2 of earthenware slab film support of the present invention.
Detailed description of the invention
For a better understanding of the present invention, be described further below in conjunction with accompanying drawing.In order to simplified characterization, method well-known to those skilled in the art, condition, step, reagent etc. repeat no longer one by one.Only reason for convenience, in the following description, employ specific direction term, such as " on ", D score, "left", "right" etc., be reference with the accompanying drawing of correspondence, can not think limitation of the present invention, when the definition direction of drawing changes, the direction that these words represent should be interpreted as corresponding different directions.
Embodiment 1
By binding agent polyether sulfone (PES) and solvent N-methyl pyrilidone (NMP), at 70 DEG C, stirring and dissolving obtains vitreosol, adds polyethylene of dispersing agent pyrrolidones (PVP), ceramic powder Al
2o
3(particle diameter 0.5 μm), stirring ball-milling 24 hours, vacuum defoamation 2h obtains slurry, and slurry viscosity is between 10000 ~ 20000mPas; Material rate is m(PES): m(NMP): m (Al
2o
3)=1:4:6, m(PVP): m(Al
2o
3)=1:100;
Use the dull and stereotyped knifing of the glass template shown in Fig. 3, scraping film temperature is 30 DEG C, and scraping film thickness is 3mm, fast template flat board is immersed in the water solidification 0.5h, treats that the complete post-drying of inversion of phases obtains having the half of film of protuberance;
The aqueous solution of the polyvinyl alcohol (PVA) of preparation 8wt.%, get the half of film that two panels is identical, relative adhesion after the precoating one deck PVA solution of protuberance side also compresses, and then adopts die pressing to make the half of film of two panels closely bonding, obtains complete green compact;
Green compact are placed in Muffle furnace sinter, 1 DEG C/min is warming up to 450 DEG C, insulation 3h, and 2 DEG C/min is warming up to 1500 DEG C, and insulation 5h, slow cooling is to room temperature subsequently, obtains earthenware slab film support.
Template flat board 3 as shown in Figure 3, has the strip recess 31 that 5 grades are dark.Half of film 2 prepared therefrom as shown in Figure 2, there is the strip protuberance 21 that 5 contour, be coated with one deck PVA aqueous solution at the upper surface of protuberance, 2 half of films are bonded together, 3 middle protuberances form support column, and the protuberance of both sides forms left and right sidewall respectively.
As illustrated in fig. 1 and 2, described earthenware slab film support comprises upper panel film 11, lower floor's Flat Membrane 12, left side wall 13 and right side wall 14 and forms flat tubular structure, have 3 strip support columns 15 between 2 layers of Flat Membrane, respectively there are 4 delivery ports 16 at described flat tubular structure two ends.The long 80cm of described earthenware slab film support, wide 20cm, thick 7mm, porosity is 70%, and average pore size is about 0.5 μm.
As shown in Figure 4, described Flat Membrane is dissymmetrical structure, comprises the top layer of fine and close sponge pore structure and the internal layer of loose finger-like pore structure; Dull and stereotyped thickness 2mm, skin depth is about 2 μm, and aperture is little, and can provide higher permselective property, thickness is thin, little on permeation flux impact; Internal layer is loose porous, and finger-like pore structure is obvious, can reduce osmotic resistance, ceramic membrane permeance property is improved greatly; Compression strength is 20MPa, and under the pressure of 0.1MPa, pure water flux is 15m
3/ (m
2h).
Embodiment 2
By binding agent polysulfones (PSF), solvent dimethylacetylamide (DMAC), heating stirring and dissolving, add ceramic powder yttria-stabilized zirconia (YSZ again, particle diameter 0.2 μm), dispersant PVP, stirring ball-milling 24h, vacuum defoamation 6h obtains slurry, and slurry viscosity is between 10000 ~ 20000mPas; Material rate is m(PSF): m(DMAC): m (YSZ)=1:5:8, m(PVP): m(YSZ)=1:100.
Use with the dull and stereotyped knifing of silica gel pattern mould, scraping film temperature is 15 DEG C, and scraping film thickness is 5mm, leaves standstill 3min in atmosphere after knifing, fast template flat board is immersed in the water solidification 2h, treats that the complete post-drying of inversion of phases obtains having the half of film of protuberance;
The PVA aqueous solution of preparation 8wt.%, get the half of film that two panels is identical, relative adhesion after the precoating one deck PVA solution of protuberance side also compresses, and then adopts die pressing to make the half of film of two panels closely bonding, obtains complete green compact;
Green compact are placed in Muffle furnace, 1 DEG C/min is warming up to 450 DEG C, insulation 3h, and 2 DEG C/min is warming up to 1600 DEG C, insulation 5h, slow cooling is to room temperature subsequently, obtains earthenware slab film support, the long 20cm of described earthenware slab film support, wide 3cm, thick 5mm, supporter porosity is 55%, and average pore size is 400nm.Compression strength is 28MPa, and under the pressure of 0.1MPa, pure water flux is 10m
3/ (m
2h).
As shown in Figure 5, in the present embodiment, half of film 2 has the protuberance 21 of 2 strips, 4 cylindric and 4 squares, and described strip protruding parts is in two side edge of half of film; Be coated with one deck PVA aqueous solution at the upper surface of protuberance, be bonded together by 2 half of films, cylindric and square protuberance forms support column, and strip protuberance forms left and right sidewall respectively.
Embodiment 3
Selection polyether sulfone (PES) is binding agent, 1-METHYLPYRROLIDONE (NMP) is solvent, and polyvinylpyrrolidone (PVP) is dispersant, aluminium oxide (Al
2o
3, particle diameter 1 μm) and titanium oxide (TiO
2, particle diameter 50nm) in mass ratio 6:1 mix as ceramic powder.M(PES): m(NMP): m (ceramic powder)=1:5:6, m(PVP): m(ceramic powder)=1:120.
During green sintering, 1 DEG C/min is warming up to 450 DEG C, insulation 3h, and 2 DEG C/min is warming up to 1150 DEG C, and insulation 5h, other conditions are identical with embodiment 1.The earthenware slab film support that the present embodiment is obtained, supporter porosity is 60%, and average pore size is 100nm, and compression strength is 22MPa, and under the pressure of 0.1MPa, pure water flux is 12m
3/ (m
2h).
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for earthenware slab film support, comprises the following steps:
Prepared by A, slurry: binding agent and stirring solvent are dissolved, then add ceramic raw material, dispersant, obtain slurry after ball milling mixing 2-24h, deaeration, slurry viscosity is between 10000 ~ 20000mPas;
B, phase inversion masking: with template flat board to above-mentioned slurry knifing, scraping film temperature is 10-50 DEG C, and scraping film thickness is 1-5mm, leaves standstill 0-3min in atmosphere, then solidify 0.5-2h after knifing in non-solvent, takes out and dries, obtain the half of film containing protuberance;
C, die pressing are shaping: on protuberance, apply one deck stickum, adopt die pressing that half of for two panels film is become green compact relative to adhesion;
D, sintering: under the condition of 1000-1800 DEG C, sinter above-mentioned green compact, insulation 2-20h, obtains earthenware slab film support;
Wherein, the mass ratio of each component of earthenware slab film support is as follows: binding agent 1, solvent 2-6, ceramic raw material 2-10; The quality of dispersant is the 0.2-2% of ceramic raw material quality;
Described earthenware slab film support, comprises 2 layers of Flat Membrane, left side wall, right side wall and at least one support column, and described 2 layers of Flat Membrane, left side wall and right side wall form flat tubular structure, and described support column is between 2 layers of Flat Membrane; Described Flat Membrane is dissymmetrical structure, comprises the top layer of sponge pore structure and the internal layer of finger-like pore structure.
2. the preparation method of earthenware slab film support according to claim 1, is characterized in that: the porosity of described earthenware slab film support is at 10-70%, and average pore size is 0.2-50 μm.
3. the preparation method of earthenware slab film support according to claim 1, is characterized in that: described ceramic raw material is one or more in aluminium oxide, zirconia, titanium oxide, silica, diatomite, mullite; Described binding agent is the one in polysulfones or polyether sulfone; Solvent is 1-METHYLPYRROLIDONE or dimethylacetylamide; Dispersant is PVP, triethanolamine or polyvinyl alcohol.
4. the preparation method of earthenware slab film support according to claim 1, it is characterized in that: described template flat board is rectangle or round rectangle flat board, template flat board there is the recess that some grades are dark, recess is cylindric, cube or strip, and the limit place that a group of template flat board is relative is strip recess.
5. the preparation method of earthenware slab film support according to claim 4, is characterized in that: described template flat board is made up of Kynoar, polytetrafluoroethylene (PTFE), silica gel, plastics, glass, timber or metal material.
6. the preparation method of earthenware slab film support according to claim 1, is characterized in that: the thickness of described Flat Membrane is 1.5-4.75mm, the thick 1-10 μm in described top layer.
7. the preparation method of earthenware slab film support according to claim 1, is characterized in that: the long 10-100cm of described earthenware slab film support, wide 2-40cm, thick 5-10mm.
8. the preparation method of earthenware slab film support according to claim 1, is characterized in that: described support column is column or strip.
9. the preparation method of earthenware slab film support according to claim 1, is characterized in that: described support column has multiple; There is multiple delivery port at described flat tubular structure two ends.
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| CN103381338B true CN103381338B (en) | 2015-02-18 |
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| CN102389719A (en) * | 2011-07-27 | 2012-03-28 | 三达膜科技（厦门）有限公司 | Silicon carbide ceramic support body and preparation method thereof |
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| CN103086704A (en) * | 2013-02-22 | 2013-05-08 | 东台市节能耐火材料厂 | Preparation method of high-porosity mineral-based ceramic membrane support |
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| CN104801199A (en) * | 2015-04-02 | 2015-07-29 | 昆山艾可芬能源科技有限公司 | Phase-inversion casting film solidification and drying device and phase-inversion casting film solidification and drying technology |
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