CN106215704A - A kind of combined flat plate ceramic honey comb film and preparation method thereof - Google Patents
A kind of combined flat plate ceramic honey comb film and preparation method thereof Download PDFInfo
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- CN106215704A CN106215704A CN201610800019.3A CN201610800019A CN106215704A CN 106215704 A CN106215704 A CN 106215704A CN 201610800019 A CN201610800019 A CN 201610800019A CN 106215704 A CN106215704 A CN 106215704A
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- honey comb
- ceramic honey
- comb film
- tabular
- film unit
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/08—Flat membrane modules
- B01D63/081—Manufacturing thereof
-
- 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
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
Abstract
The invention discloses a kind of combined flat plate ceramic honey comb film, be made up of tabular ceramic honey comb film unit split;Described tabular ceramic honey comb film unit is narrow boards shape, and the edge shape of its two avris is that central rotation is symmetrical;It is connected with avris in the width direction between described tabular ceramic honey comb film unit and splices.Additionally, also disclose the preparation method of combinations thereof formula flat board ceramic honey comb film.The present invention, with tabular ceramic honey comb lamina membranacea as unit, can obtain the combined flat plate ceramic honey comb film of large scale, difformity structure by the way of split, and flexibly, it is convenient to change in combination.In preparation technology, only need to prepare tabular ceramic honey comb film unit, greatly reduce molding difficulty and the probability of supporter defect occurs;And can extrude continuously, efficiency high, decrease simultaneously flat board ceramic honey comb film the later stage be dried, the probability of deformation in calcination process.
Description
Technical field
The present invention relates to technical field of membrane separation, particularly relate to a kind of flat board ceramic honey comb film and preparation method thereof.
Background technology
Membrane separation technique is by one of new and high technology being referred to as 21st century most application prospect in the world.Ceramic membrane is
A new generation's membrane separation technique, is with Al2O3、ZrO2、TiO2、SiO2, the tool that is made through a series of special process of the raw material such as SiC
There is the separation material of loose structure.Ceramic membrane is divided into tubulose, multichannel and tabular according to shape.With traditional tubulose and manifold
Road ceramic membrane is different, and ceramic membrane uses external-compression type to filter, and the outer surface of ceramic membrane is stratum disjunctum, and fenestra road is that penetrating fluid leads to
Road.Owing to having eggshell effect, using this structure, for ultra-thin ceramic membrane, the wall thickness of its supporter can be as small as
1mm, the thickness of whole Flat Membrane is 3~5mm, thus significantly reduces the osmotic resistance of ceramic membrane.But, this structure also must
So bring problems with:
(1) requirement to forming technique is added.In particular by extrusion moulding, need to control pug character to avoid
Ceramic film support deforms.
(2) bulk strength of ceramic membrane is inadequate.Although the buckling strength of membrane material is not changed in, but, due to supporter
Thickness is less, and the pressure that ceramic membrane can bear is less, easily snaps off.
(3) membrane area of unit volume is less.Owing to using slab construction, the external surface area of ceramic membrane is film surface
Long-pending, for assembly, the membrane area of the ceramic membrane can installed in unit volume is less than Multichannel ceramic membrane.
(4) the preparation difficulty of ceramic membrane separation layer increases.Owing to the thickness of supporter reduces, tradition cement-dipping method is used to be difficult to
Obtain enough thicknesses of layers (general < 10 μm), be easily generated film defect.
At present, prior art, for the preparation of tabular ceramic film support, also has employing injection moulding, gel injection-moulding to become
The methods such as type, but consider from performance and the preparation efficiency of ceramic film support, extrusion moulding still has obvious advantage.So
And, the method for prior art extrusion molding not technology of preparing for ultra-thin ceramic membrane proposes to be effectively improved and arrange
Execute.Additionally, be to improve unit volume membrane area further, currently also research and develop large-sized thin wall hollow flat ceramic
Film.But size is the biggest, either still it is dried in the later stage in molding and is all easily caused deformation in calcination process, particularly can increase
Add ceramic membrane and the probability of film defect occurs.And, along with the change of size is big, thin plate easily occurs in membrane filtration processes that vibration is existing
As, easily rupture because of resonance.
In terms of preparative separation film layer, prior art generally uses cement-dipping method, is coated with in addition with using vacuum impregnation
The method of film, but not special adaptations.To this end, also researched and developed plasma spraying preparative separation film layer, but substantially increase
Ceramic membrane cost;And using compressed air is source of the gas, preparing film layer by spraying, under compressed-air actuated brushing, film layer holds
Easily ftracture because of rapid draing.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of combined flat plate ceramic honey comb film, with flat
Tabular ceramic honey comb lamina membranacea is unit, obtains the combined flat plate honeycomb of large scale, difformity structure by the way of split
Ceramic membrane.Another object of the present invention is to provide the preparation method of combinations thereof formula flat board ceramic honey comb film.
The purpose of the present invention is achieved by the following technical programs:
A kind of combined flat plate ceramic honey comb film that the present invention provides, is made up of tabular ceramic honey comb film unit split;
Described tabular ceramic honey comb film unit is narrow boards shape, and the edge shape of its two avris is that central rotation is symmetrical;Described tabular
It is connected with avris in the width direction between ceramic honey comb film unit and splices.
The edge of tabular two avris of ceramic honey comb film unit of the present invention is that central rotation is symmetrical, therefore at width
Can be fitting to connection well between ceramic membrane unit.Further, the width of tabular ceramic honey comb film unit of the present invention
Degree≤15cm.
In such scheme, its edge cross-section of avris of tabular ceramic honey comb film unit of the present invention be shaped as straight line,
One in camber line, curve, broken line or a combination thereof.Between described tabular ceramic honey comb film unit in plane, beveled structure or
W type corrugated split connects, it is hereby achieved that plane or the large scale flat board ceramic honey comb film of bending structure combination, and
Bending structure is conducive to improving flat board ceramic honey comb film structural stability in running.
In such scheme, tabular ceramic honey comb film unit of the present invention on it outer lower face surface be separation membrane layer, in it
There is single or double penetrating fluid duct.
Another object of the present invention is achieved by the following technical programs:
The preparation method of the combinations thereof formula flat board ceramic honey comb film that the present invention provides, wherein said tabular ceramic honey comb
The preparation of film unit, comprises the following steps:
(1) extrusion moulding prepares the supporter of tabular ceramic honey comb film unit
After aluminium oxide, pore creating material, binding agent mix homogeneously, add lubricant, plasticizer, water in clay kneading machine, mediate shape
Become pug;Described pore creating material, binding agent, lubricant, plasticizer, the consumption of water be respectively the 1~8wt% of aluminium oxide, 2~
6wt%, 3~6wt%, 0.5~1.5wt%, 10~18wt%;Described pug is by after horizontal extruder extrusion molding, through dry
Dry, calcining, obtains the supporter that two ends are the symmetrical tabular ceramic honey comb film unit of central rotation;
(2) ink-jet printing process prepares the separation membrane layer of tabular ceramic honey comb film unit
Aluminium oxide, dispersant, stabilizer, water mixing are obtained stable suspension, described dispersant, stabilizer, water
Consumption be respectively 0.5~1.2wt%, 1~4wt%, 700~the 920wt% of aluminium oxide;Described suspension is placed in ink-jet beat
In print machine, it is sprayed at the surface of described tabular ceramic honey comb film unit supporter and obtains separation membrane layer;By controlling ink-jet
Amount controls the thickness of separation membrane layer, obtains tabular ceramic honey comb film unit after drying, calcining.
Further, particle mean size≤40 μm of aluminium oxide in step (1) described in preparation method of the present invention;Described calcining temperature
Degree is 1500~1650 DEG C, and calcination time is 2~4h;The average pore size of the supporter of described tabular ceramic honey comb film unit is
1~4.5 μm.
Further, in step (2) described in preparation method of the present invention, the particle mean size of aluminium oxide is 0.5~1 μm;Described point
Thickness from film layer is 15~25 μm;Described calcining heat is 1300~1450 DEG C, and calcination time is 2~4h;Described tabular
The average pore size of the separation membrane layer of ceramic honey comb film unit is 0.1~0.5 μm.
In such scheme, in step (1) described in preparation method of the present invention, pore creating material is starch;Binding agent is carboxymethyl cellulose
One in element, methylcellulose, polyvinyl alcohol, hydroxypropyl methyl cellulose or a combination thereof;Lubricant is glycerol and/or oil
Acid;Plasticizer is polyvinyl alcohol.
In such scheme, in step (2) described in preparation method of the present invention, dispersant is that polyacrylic acid, Dolapix series are divided
One in powder, polyvinylpyrrolidone or a combination thereof, or, for polymine and/or polyvinylpyrrolidone, the most poly-
Aziridine can not use with polyacrylic acid, Dolapix Series Dispersant interworking;Stabilizer be poly propenoic acid aziridine,
One in polyvinyl pyrilodone, polyvinyl alcohol or a combination thereof, i.e. polymine can not use with polyacrylic acid interworking.
The method have the advantages that
(1) present invention only prepares tabular ceramic honey comb film unit, can be by the split of multiple unit, it is thus achieved that big chi
Combined flat plate ceramic honey comb film very little, difformity structure.Splice in the way of by 180 °, in planar structure, can obtain big
The unit volume membrane area of size flat-panel ceramic honey comb film;Split is formed at other angles bending structure, W type corrugated,
There is gusseted effect, be conducive to improving structural stability when running, for the flat board ceramic honey comb film (example of long length
Such as larger than 1m), can effectively reduce feed liquid in membrane filtration processes and supporter be washed away and the ceramic membrane resonance that causes, thus effectively
Reduce the probability of ceramic membrane fracture;And, the structure such as this bending, W type corrugated, it helps improve the turbulent flow of feed liquid
Degree, reduces fouling membrane, improves permeability of the membrane energy.
(2) present invention uses the mode of splicing, and flexibly, it is convenient to change in combination.Separation film due to flat board ceramic honey comb film
Layer is at the upper outer lower face surface of ceramic membrane, and the split of the most each ceramic membrane unit connects and membrane separating property will not be produced impact, can
With independent assortment.And, the separating property such as single ceramic film unit declines, only by changing defective ceramic membrane unit,
The performance of large scale flat board ceramic honey comb film can be kept.
(3) present invention only need to prepare tabular ceramic honey comb film unit, owing to width is less, uses the horizontal of routine to squeeze
Go out forming machine to extrude.Need to use specific vertical honeycomb ceramics extrusion machine relative to large scale flat board ceramic honey comb film and
Speech, greatly reduces molding difficulty, there is not the situation of wet base bending, occur that the probability of supporter defect is big in extrusion
Width reduces;And can extrude continuously, efficiency high, and flat board ceramic honey comb film can be reduced be dried in the later stage, calcination process become
The probability of shape.
(4) preparation method of the present invention uses ink-jet printing process to prepare the separation membrane layer of ceramic membrane.By controlling ink-jet
Amount, can control the thickness of separation membrane layer.In spraying process, shower nozzle is not directly contacted with flat ceramic film support, flat board
The shape of ceramic film support and defect do not interfere with the character of separation membrane layer, thus largely avoid separation membrane layer defect and deposit
Possibility.
Accompanying drawing explanation
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail:
Fig. 1 is the schematic cross-section of the embodiment of the present invention one tabular ceramic honey comb film unit;
Fig. 2 is the connected mode schematic diagram of embodiment illustrated in fig. 1 tabular ceramic honey comb film unit;
Fig. 3 is that the scanning of the embodiment of the present invention two preparation method gained tabular ceramic honey comb its separation membrane layer of film unit is shone
Sheet;
Fig. 4 is that the scanning of the embodiment of the present invention three preparation method gained tabular ceramic honey comb its separation membrane layer of film unit is shone
Sheet.
In figure: the width W of tabular ceramic honey comb film unit, supporter 1, penetrating fluid duct 2, tabular ceramic honey comb film
Splicing angle [alpha] in the width direction, β between unit
Detailed description of the invention
Embodiment one:
Fig. 1 and Fig. 2 show the embodiment of the present invention a kind of combined flat plate ceramic honey comb film, by tabular ceramic honey comb
Film unit split is constituted.As it is shown in figure 1, tabular ceramic honey comb film unit is narrow boards shape, its width W is 7~15cm, a length of
1~1.2m, the edge shape of its two avris is that central rotation is symmetrical.Its cross sectional shape of the edge of avris is straight line, camber line, song
One in line, broken line or a combination thereof.
Tabular ceramic honey comb film unit is by supporter 1 and is positioned at the separation membrane layer of outer lower face surface on supporter and forms.
As it is shown in figure 1, have the single or double penetrating fluid duct 2 being positioned at middle part, the width in single penetrating fluid duct 2 in supporter 1
It is 1mm for 3mm, height.For the tabular ceramic honey comb film unit in single penetrating fluid duct, its thickness is 3mm, wall thickness is
1mm;For the tabular ceramic honey comb film unit in double penetrating fluid duct, its thickness is 5mm, wall thickness is 1mm, upper and lower penetrating fluid
Duct spacing is 1mm.
The edge cross-section shape of tabular ceramic honey comb its avris of film unit, can be radius be that the camber line of 1.5mm is (see figure
1a) or the curve (see Fig. 1 b) that is combined into of camber line that radius is 1.5mm or straight line (see Fig. 1 c) that angle is 60 ° or radius
The curve (see Fig. 1 d) being combined into for the camber line of 2.5mm.
The present embodiment combined flat plate ceramic honey comb film, by the split structure of above-mentioned multiple tabular ceramic honey comb film units
Become, owing to the edge shape of its two avris of ceramic membrane unit is that central rotation is symmetrical, therefore, along width between each ceramic membrane unit
Direction is connected can be fitting to connection well with avris.Can to use 180 °, in planar structure in the way of splice and obtain big chi
The unit volume membrane area of very little flat board ceramic honey comb film;Can also use other angles is bending structure or the side of W type corrugated
Formula is spliced, and is to connect with arbitrarily angled (such as α, β) as shown in Figure 2 a, is to connect with fixed angle as shown in Figure 2 b.
Embodiment two:
The preparation method of the present embodiment a kind of combined flat plate ceramic honey comb film, is made pottery by the tabular honeycomb of embodiment one
Porcelain film unit split is constituted, the wherein preparation of tabular ceramic honey comb film unit, and its step is as follows:
(1) extrusion moulding prepares the supporter of tabular ceramic honey comb film unit
By 50kg alumina powder (mean diameter is 40 μm), 4kg starch, 2.5kg hydroxypropyl methyl cellulose at batch mixer
After middle mix homogeneously, addition 2kg glycerol, 0.5kg polyvinyl alcohol, 9kg water are kneaded into mud in clay kneading machine, after old 1 week, pass through
Horizontal extruder extrusion molding, then in constant temperature and humidity drying case, (temperature is 80 DEG C, and humidity is 90%) is dried 24h, warp
1650 DEG C of calcining 4h, obtain average pore size be 4.2 μm, two ends be the symmetrical tabular ceramic honey comb film unit of central rotation
Support body;
(2) ink-jet printing process prepares the separation membrane layer of tabular ceramic honey comb film unit
0.05g Dolapix CE-64 is dissolved in 90g water, adds 10g alumina powder (mean diameter is 1 μm), then
Add 0.35g polyvinyl alcohol 1750 (it is 12wt% solution that polyvinyl alcohol need to be configured to concentration in advance), under intense agitation
Carry out mixing and obtaining stable suspension;Suspension is placed in ink-jet printer, is sprayed at above-mentioned tabular ceramic honey comb
The surface of film unit supporter and obtain separation membrane layer, thicknesses of layers is 25 μm;After drying at room temperature, calcine 3h through 1450 DEG C,
To the tabular ceramic honey comb film unit that separation membrane layer average pore size is 0.5 μm.
As it is shown on figure 3, uniform by spraying the particle packing formed, it is possible to form uniform separation membrane layer, its surface
Without big hole defect.
Embodiment three:
The preparation method of the present embodiment a kind of combined flat plate ceramic honey comb film, is with embodiment one difference, flat
The preparation of tabular ceramic honey comb film unit, its step is as follows:
(1) extrusion moulding prepares the supporter of tabular ceramic honey comb film unit
By 50kg alumina powder (mean diameter is 10 μm), 4kg starch, 3.0kg hydroxypropyl methyl cellulose at batch mixer
After middle mix homogeneously, addition 2kg glycerol, 0.75kg polyvinyl alcohol, 9kg water are kneaded into mud in clay kneading machine, after old 2 weeks, logical
Crossing horizontal extruder extrusion molding, then in constant temperature and humidity drying case, (temperature is 80 DEG C, and humidity is 90%) is dried 24h, warp
1550 DEG C of calcining 4h, obtain average pore size be 1.2 μm, two ends be the symmetrical tabular ceramic honey comb film unit of central rotation
Support body;
(2) ink-jet printing process prepares the separation membrane layer of tabular ceramic honey comb film unit
0.10g Dolapix CE-64 is dissolved in 90g water, adds 10g alumina powder (mean diameter is 0.1 μm),
Add 0.35g polyvinyl alcohol 1799 (it is 12wt% solution that polyvinyl alcohol need to be configured to concentration in advance), in intense agitation
Under carry out mixing and obtaining stable suspension;Suspension is placed in ink-jet printer, is sprayed at above-mentioned tabular honeycomb pottery
The surface of porcelain film unit supporter and obtain separation membrane layer, thicknesses of layers is 20 μm;After drying at room temperature, calcine 2h through 1350 DEG C,
Obtain the tabular ceramic honey comb film unit that separation membrane layer average pore size is 0.1 μm.
As shown in Figure 4, the particle packing that spraying is formed is uniform, and after 1350 DEG C are calcined, nano aluminium oxide presents good
Good sintering, is well combined between granule.Separation membrane layer surface does not has big hole defect, even aperture distribution.
Claims (10)
1. a combined flat plate ceramic honey comb film, it is characterised in that: it is made up of tabular ceramic honey comb film unit split;Described
Tabular ceramic honey comb film unit is narrow boards shape, and the edge shape of its two avris is that central rotation is symmetrical;Described tabular honeycomb
It is connected with avris in the width direction between ceramic membrane unit and splices.
Combined flat plate ceramic honey comb film the most according to claim 1, it is characterised in that: described tabular ceramic honey comb film
Width≤the 15cm of unit.
Combined flat plate ceramic honey comb film the most according to claim 1 and 2, it is characterised in that: described tabular honeycomb is made pottery
Its edge cross-section of the avris of porcelain film unit is shaped as the one in straight line, camber line, curve, broken line or a combination thereof.
Combined flat plate ceramic honey comb film the most according to claim 1, it is characterised in that: described tabular ceramic honey comb film
In plane between unit, beveled structure or W type corrugated split connect.
Combined flat plate ceramic honey comb film the most according to claim 1, it is characterised in that: described tabular ceramic honey comb film
Unit on it outer lower face surface be separation membrane layer, there is in it single or double penetrating fluid duct.
6. the preparation method of one of claim 1-5 described combined flat plate ceramic honey comb film, it is characterised in that: wherein said flat
The preparation of tabular ceramic honey comb film unit, comprises the following steps:
(1) extrusion moulding prepares the supporter of tabular ceramic honey comb film unit
After aluminium oxide, pore creating material, binding agent mix homogeneously, add lubricant, plasticizer, water in clay kneading machine, mediate formation mud
Material;Described pore creating material, binding agent, lubricant, plasticizer, the consumption of water be respectively 1~8wt%, 2~6wt% of aluminium oxide, 3
~6wt%, 0.5~1.5wt%, 10~18wt%;After described pug passes through horizontal extruder extrusion molding, drying, calcining,
Obtain the supporter that two ends are the symmetrical tabular ceramic honey comb film unit of central rotation;
(2) ink-jet printing process prepares the separation membrane layer of tabular ceramic honey comb film unit
Aluminium oxide, dispersant, stabilizer, water mixing are obtained stable suspension, described dispersant, stabilizer, the use of water
Amount is respectively 0.5~1.2wt%, 1~4wt%, 700~the 920wt% of aluminium oxide;Described suspension is placed in ink-jet printer
In, it is sprayed at the surface of described tabular ceramic honey comb film unit supporter and obtains separation membrane layer;By controlling ink ejection amount
Control the thickness of separation membrane layer, after drying, calcining, obtain tabular ceramic honey comb film unit.
The preparation method of combined flat plate ceramic honey comb film the most according to claim 6, it is characterised in that: described step
(1) particle mean size≤40 μm of aluminium oxide in;Described calcining heat is 1500~1650 DEG C, and calcination time is 2~4h;Described flat
The average pore size of the supporter of tabular ceramic honey comb film unit is 1~4.5 μm.
The preparation method of combined flat plate ceramic honey comb film the most according to claim 6, it is characterised in that: described step
(2) in, the particle mean size of aluminium oxide is 0.5~1 μm;The thickness of described separation membrane layer is 15~25 μm;Described calcining heat is
1300~1450 DEG C, calcination time is 2~4h;The average pore size of the separation membrane layer of described tabular ceramic honey comb film unit is
0.1~0.5 μm.
The preparation method of combined flat plate ceramic honey comb film the most according to claim 6, it is characterised in that: described step
(1) in, pore creating material is starch;Binding agent is in carboxymethyl cellulose, methylcellulose, polyvinyl alcohol, hydroxypropyl methyl cellulose
One or a combination thereof;Lubricant is glycerol and/or oleic acid;Plasticizer is polyvinyl alcohol.
The preparation method of combined flat plate ceramic honey comb film the most according to claim 6, it is characterised in that: described step
(2) one during dispersant is polyacrylic acid, Dolapix Series Dispersant, polyvinylpyrrolidone in or a combination thereof, or,
For polymine and/or polyvinylpyrrolidone;Stabilizer is poly propenoic acid aziridine, polyvinyl pyrilodone, gathers
One in vinyl alcohol or a combination thereof.
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CN114307665A (en) * | 2020-09-29 | 2022-04-12 | 三达膜科技(厦门)有限公司 | Preparation method of large-diameter side ponding flow channel honeycomb ceramic filter membrane |
CN115231902A (en) * | 2022-07-10 | 2022-10-25 | 上海熊猫机械(集团)有限公司 | W-type alumina-supported silicon carbide ceramic membrane and preparation method thereof |
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CN108426455B (en) * | 2018-03-28 | 2023-11-24 | 景德镇陶瓷大学 | Pad foot for ceramic membrane support calcination and method for controlling deformation of ceramic membrane support |
CN114307665A (en) * | 2020-09-29 | 2022-04-12 | 三达膜科技(厦门)有限公司 | Preparation method of large-diameter side ponding flow channel honeycomb ceramic filter membrane |
CN114307665B (en) * | 2020-09-29 | 2023-02-14 | 三达膜科技(厦门)有限公司 | Preparation method of large-diameter side ponding flow channel honeycomb ceramic filter membrane |
CN115231902A (en) * | 2022-07-10 | 2022-10-25 | 上海熊猫机械(集团)有限公司 | W-type alumina-supported silicon carbide ceramic membrane and preparation method thereof |
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