CN106215704B - 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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- CN106215704B CN106215704B CN201610800019.3A CN201610800019A CN106215704B CN 106215704 B CN106215704 B CN 106215704B CN 201610800019 A CN201610800019 A CN 201610800019A CN 106215704 B CN106215704 B CN 106215704B
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- honey comb
- ceramic honey
- comb film
- film unit
- tabular
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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 films, are made of tabular ceramic honey comb film unit split；The tabular ceramic honey comb film unit is narrow boards shape, and the edge shape of two avris is in center rotational symmetry；It is connected in the width direction with avris between the tabular ceramic honey comb film unit and is spliced.In addition, also disclosing the preparation method of said combination formula plate ceramic honey comb film.The present invention can get the combined flat plate ceramic honey comb film of large scale, different shape structure, flexibly, replacement is convenient for combination using tabular ceramic honey comb diaphragm plate as unit by way of split.In preparation process, tabular ceramic honey comb film unit only need to be prepared, greatly reduce molding difficulty and the probability of support volume defect occurs；And it can continuously squeeze out, is high-efficient, while decreasing a possibility that plate ceramic honey comb film deforms in later period drying, calcination process.
Description
Technical field
The present invention relates to technical field of membrane separation more particularly to a kind of plate ceramic honey comb film and preparation method thereof.
Background technique
Membrane separation technique has been known as one of the new and high technology of 21st century most application prospect in the world.Ceramic membrane is
Membrane separation technique of new generation is with Al2O3、ZrO2、TiO2、SiO2, a series of tool that is made through special process of the raw materials such as SiC
There is the separation material of porous structure.Ceramic membrane is divided into tubulose, multichannel and tabular according to shape.With traditional tubulose and multi-pass
Road ceramic membrane is different, and ceramic membrane is filtered using external-compression type, and the outer surface of ceramic membrane is separating layer, and fenestra road is logical for penetrating fluid
Road.Since with eggshell effect, using this structure, for ultra-thin ceramic membrane, the wall thickness of supporter be can be as small as
1mm, the thickness of entire plate membrane is in 3~5mm, to significantly reduce the osmotic resistance of ceramic membrane.But this structure also must
So bring following problems:
(1) requirement to forming technique is increased.In particular by extrusion moulding, need to control pug property to avoid
Ceramic film support deformation.
(2) integral strength of ceramic membrane is inadequate.Although the buckling strength of membrane material does not change, due to supporter
Thickness is smaller, and the pressure that ceramic membrane can bear is smaller, easily snaps off.
(3) membrane area of unit volume is smaller.Due to being film surface using the external surface area of slab construction, ceramic membrane
Product, for component, the membrane area for the ceramic membrane that can be installed in unit volume is less than Multichannel ceramic membrane.
(4) the preparation difficulty of ceramic membrane separation layer increases.Since the thickness of supporter reduces, it is difficult to using traditional cement-dipping method
Enough thicknesses of layers (10 μm of general <) is obtained, film defect is also easy to produce.
Currently, preparation of the prior art for tabular ceramic film support, also have using injection moulding, gel injection-moulding at
The methods of type, but consider from the performance of ceramic film support and preparation efficiency, extrusion moulding still has apparent advantage.So
And the technology of preparing that the method for prior art extrusion molding is not directed to ultra-thin ceramic membrane proposes that effective improve is arranged
It applies.In addition, also having researched and developed large-sized thin wall hollow flat ceramic at present to further increase unit volume membrane area
Film.But size is bigger, is either easy to cause deformation during forming or in later period drying and calcination, can especially increase
Ceramic membrane is added the probability of film defect occur.Moreover, becoming larger with size, thin plate is easy to occur in membrane filtration processes trembling now
As being easily broken because of resonance.
In terms of preparative separation film layer, what the prior art generallyd use is cement-dipping method, and in addition there are applied using vacuum impregnation
The method of film, but there is no special adaptations.For this purpose, also having researched and developed plasma spraying preparative separation film layer, but obviously increase
Ceramic membrane cost；And use compressed air for gas source, film layer is prepared by spraying, under the brushing of compressed air, film layer is held
Easily crack because of rapid draing.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of combined flat plate ceramic honey comb films, with flat
Plate ceramic honey comb diaphragm plate is unit, and the combined flat plate honeycomb of large scale, different shape structure is obtained by way of split
Ceramic membrane.Another object of the present invention is to provide the preparation methods of said combination formula plate 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 provided by the invention is made of tabular ceramic honey comb film unit split；
The tabular ceramic honey comb film unit is narrow boards shape, and the edge shape of two avris is in center rotational symmetry；The tabular
It is connected in the width direction with avris between ceramic honey comb film unit and is spliced.
The edge of two avris of tabular ceramic honey comb film unit of the present invention is in center rotational symmetry, therefore in width direction
It 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 above scheme, its edge cross-section shape of the avris of tabular ceramic honey comb film unit of the present invention be straight line,
One of camber line, curve, broken line or combinations thereof.Between the tabular ceramic honey comb film unit in plane, beveled structure or
W type corrugated split connection, it is hereby achieved that plane or the large scale plate ceramic honey comb film of bending structure combination, and
Bending structure is conducive to improve the structural stability of plate ceramic honey comb film in the process of running.
In above scheme, outer lower face surface is separation membrane layer to tabular ceramic honey comb film unit of the present invention thereon, in
With single or double penetrating fluid duct.
Another object of the present invention is achieved by the following technical programs:
The preparation method of said combination formula plate ceramic honey comb film provided by the invention, wherein the tabular ceramic honey comb
The preparation of film unit, comprising the following steps:
(1) supporter of extrusion moulding preparation tabular ceramic honey comb film unit
After mixing by aluminium oxide, pore creating material, binder, lubricant, plasticizer, water is added and mediates shape in clay kneading machine
At pug；The pore creating material, binder, lubricant, plasticizer, water dosage be respectively 1~8wt% of aluminium oxide, 2~
6wt%, 3~6wt%, 0.5~1.5wt%, 10~18wt%；After the pug passes through horizontal extruder extrusion molding, through dry
Dry, calcining obtains both ends in the supporter of the tabular ceramic honey comb film unit of center rotational symmetry；
(2) separation membrane layer of ink-jet printing preparation tabular ceramic honey comb film unit
Aluminium oxide, dispersing agent, stabilizer, water are mixed and obtain stable suspension, the dispersing agent, stabilizer, water
Dosage be respectively aluminium oxide 0.5~1.2wt%, 1~4wt%, 700~920wt%；The suspension is placed in ink-jet to beat
In print machine, it is sprayed at the surface of the tabular ceramic honey comb film unit supporter and obtains separation membrane layer；By controlling ink-jet
It measures to control the thickness of separation membrane layer, tabular ceramic honey comb film unit is obtained after drying, calcining.
Further, in step (1) described in preparation method of the present invention aluminium oxide average particle size≤40 μm；The calcining temperature
Degree is 1500~1650 DEG C, and calcination time is 2~4h；The average pore size of the supporter of the tabular ceramic honey comb film unit is
1~4.5 μm.
Further, the average particle size of aluminium oxide is 0.5~1 μm in step (2) described in preparation method of the present invention；Described point
From film layer with a thickness of 15~25 μm；The calcination temperature is 1300~1450 DEG C, and calcination time is 2~4h；The tabular
The average pore size of the separation membrane layer of ceramic honey comb film unit is 0.1~0.5 μm.
In above scheme, pore creating material is starch in step described in preparation method of the present invention (1)；Binder is carboxymethyl cellulose
One of element, methylcellulose, polyvinyl alcohol, hydroxypropyl methyl cellulose or combinations thereof；Lubricant is glycerol and/or oil
Acid；Plasticizer is polyvinyl alcohol.
In above scheme, dispersing agent is polyacrylic acid, Dolapix series point in step described in preparation method of the present invention (2)
One of powder, polyvinylpyrrolidone or combinations thereof gather alternatively, being polyethyleneimine and/or polyvinylpyrrolidone
Aziridine cannot be used with polyacrylic acid, Dolapix Series Dispersant interworking；Stabilizer be poly propenoic acid aziridine,
One of polyvinyl pyrilodone, polyvinyl alcohol or combinations thereof, i.e. polyethyleneimine cannot be used with polyacrylic acid interworking.
The invention has the following advantages:
(1) present invention only prepares tabular ceramic honey comb film unit, can obtain big ruler by the split of multiple units
Very little, different shape structure combined flat plate ceramic honey comb film.By 180 °, in planar structure in a manner of splice, can get big
The unit volume membrane area of size flat-panel ceramic honey comb film；Split is formed by bending structure, W type corrugated at other angles,
With gusseted effect, be conducive to improve structural stability when operation, for the plate ceramic honey comb film (example of long length
Such as larger than 1m), it can effectively reduce feed liquid in membrane filtration processes to ceramic membrane resonance caused by the washing away of supporter, thus effectively
A possibility that reducing ceramic membrane fracture；Moreover, the structures 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 is by the way of splicing, and flexibly, replacement is convenient for combination.Due to the seperation film of plate ceramic honey comb film
Layer ceramic membrane upper outer lower face surface, therefore each ceramic membrane unit split connection membrane separating property will not be had an impact, can
With independent assortment.Moreover, the separating property such as single ceramic film unit declines, only by replacing defective ceramic membrane unit,
It can keep the performance of large scale plate ceramic honey comb film.
(3) present invention only need to prepare tabular ceramic honey comb film unit, and since width is smaller, horizontal using routine is squeezed
Molding machine squeezes out out.Need relative to large scale plate ceramic honey comb film using specific vertical honeycomb ceramics extrusion machine and
The case where speech, greatly reduces molding difficulty, and there is no the bendings of wet base in extrusion process, the probability for support volume defect occur is big
Width reduces；And it can continuously squeeze out, is high-efficient, and can be reduced plate ceramic honey comb film and become in later period drying, calcination process
A possibility that shape.
(4) preparation method of the present invention prepares the separation membrane layer of ceramic membrane using ink-jet printing.By controlling ink-jet
Amount, can control the thickness of separation membrane layer.In spraying process, spray head is not directly contacted with flat ceramic film support, plate
The shape and defect of ceramic film support will not influence the property of separation membrane layer, deposit to largely avoid separation membrane layer defect
Possibility.
Detailed description of the invention
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail:
Fig. 1 is the schematic cross-section of one tabular ceramic honey comb film unit of the embodiment of the present invention；
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 its separation membrane layer of tabular ceramic honey comb film unit obtained by two preparation method of the embodiment of the present invention is shone
Piece；
Fig. 4 is that the scanning of its separation membrane layer of tabular ceramic honey comb film unit obtained by three preparation method of the embodiment of the present invention is shone
Piece.
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], β between unit in the width direction
Specific embodiment
Embodiment one:
Fig. 1 and Fig. 2 show a kind of embodiment of combined flat plate ceramic honey comb film of the present invention, by tabular ceramic honey comb
Film unit split is constituted.As shown in Figure 1, tabular ceramic honey comb film unit is narrow boards shape, width W is 7~15cm, length is
1~1.2m, the edge shape of two avris is in center rotational symmetry.Its cross sectional shape of the edge of avris is straight line, camber line, song
One of line, broken line or combinations thereof.
By supporter 1 and on supporter, the separation membrane layer of outer lower face surface forms tabular ceramic honey comb film unit.
As shown in Figure 1, having in supporter 1 positioned at the single or double penetrating fluid duct 2 at middle part, the width in single penetrating fluid duct 2
For 3mm, be highly 1mm.For the tabular ceramic honey comb film unit in single penetrating fluid duct, it is with a thickness of 3mm, wall thickness
1mm；For the tabular ceramic honey comb film unit in double penetrating fluid duct, with a thickness of 5mm, wall thickness 1mm, upper and lower penetrating fluid
Duct spacing is 1mm.
The edge cross-section shape of its avris of tabular ceramic honey comb film unit, can be radius is the camber line of 1.5mm (see figure
1a) or radius be 1.5mm the curve (see Fig. 1 b) that is combined into of camber line or angle be 60 ° straight line (see Fig. 1 c) or radius
The curve being combined into for the camber line of 2.5mm (see Fig. 1 d).
The present embodiment combined flat plate ceramic honey comb film passes through the split structure of above-mentioned multiple tabular ceramic honey comb film units
At, since the edge shape of ceramic membrane unit its two avris is in center rotational symmetry, along width between each ceramic membrane unit
Direction is connected with avris to be fitting to connection well.Can using 180 °, in planar structure by the way of splice and obtain big ruler
The unit volume membrane area of very little plate ceramic honey comb film；It can also be using other angles in bending structure or the side of W type corrugated
Formula splicing is with any angle (such as α, β) connection as shown in Figure 2 a, is connected with fixed angle as shown in Figure 2 b.
Embodiment two:
A kind of preparation method of combined flat plate ceramic honey comb film of the present embodiment is made pottery by the tabular honeycomb of embodiment one
Porcelain film unit split is constituted, and the wherein preparation of tabular ceramic honey comb film unit, its step are as follows:
(1) supporter of extrusion moulding preparation tabular ceramic honey comb film unit
By 50kg alumina powder (average grain diameter is 40 μm), 4kg starch, 2.5kg hydroxypropyl methyl cellulose in batch mixer
In after mixing, 2kg glycerol is added, 0.5kg polyvinyl alcohol, 9kg water are kneaded into mud in clay kneading machine and pass through after aging 1 week
Horizontal extruder extrusion molding, then (temperature is 80 DEG C, humidity 90%) is dry for 24 hours in constant temperature and humidity drying case, warp
1650 DEG C of calcining 4h, obtain average pore size be 4.2 μm, both ends in center rotational symmetry tabular ceramic honey comb film unit branch
Support body；
(2) separation membrane layer of ink-jet printing preparation tabular ceramic honey comb film unit
0.05g Dolapix CE-64 is dissolved in 90g water, is added 10g alumina powder (average grain diameter is 1 μm), then
0.35g polyvinyl alcohol 1750 (it is 12wt% solution that polyvinyl alcohol need to be configured to concentration in advance) is added, under intense agitation
It is mixed and obtains stable suspension；Suspension is placed in ink-jet printer, above-mentioned tabular ceramic honey comb is sprayed at
The surface of film unit supporter and obtain separation membrane layer, thicknesses of layers be 25 μm；After drying at room temperature, through 1450 DEG C of calcining 3h, obtain
The tabular ceramic honey comb film unit for being 0.5 μm to separation membrane layer average pore size.
As shown in figure 3, it is uniform to be formed by particle packing by spraying, it is capable of forming uniform separation membrane layer, surface
Without big hole defect.
Embodiment three:
A kind of preparation method of combined flat plate ceramic honey comb film of the present embodiment the difference is that, is put down with embodiment one
The preparation of plate ceramic honey comb film unit, its step are as follows:
(1) supporter of extrusion moulding preparation tabular ceramic honey comb film unit
By 50kg alumina powder (average grain diameter is 10 μm), 4kg starch, 3.0kg hydroxypropyl methyl cellulose in batch mixer
In after mixing, 2kg glycerol is added, 0.75kg polyvinyl alcohol, 9kg water are kneaded into mud in clay kneading machine, after aging 2 weeks, leads to
Horizontal extruder extrusion molding is crossed, then (temperature is 80 DEG C, humidity 90%) is dry for 24 hours in constant temperature and humidity drying case, warp
1550 DEG C of calcining 4h, obtain average pore size be 1.2 μm, both ends in center rotational symmetry tabular ceramic honey comb film unit branch
Support body；
(2) separation membrane layer of ink-jet printing preparation tabular ceramic honey comb film unit
0.10g Dolapix CE-64 is dissolved in 90g water, 10g alumina powder (average grain diameter is 0.1 μm) is added,
0.35g polyvinyl alcohol 1799 (it is 12wt% solution that polyvinyl alcohol need to be configured to concentration in advance) is added, in intense agitation
Lower mixed and obtain stable suspension；Suspension is placed in ink-jet printer, above-mentioned tabular honeycomb pottery is sprayed at
The surface of porcelain film unit supporter and obtain separation membrane layer, thicknesses of layers be 20 μm；After drying at room temperature, through 1350 DEG C of calcining 2h,
Obtain the tabular ceramic honey comb film unit that separation membrane layer average pore size is 0.1 μm.
As shown in figure 4, spraying is formed by, particle packing is uniform, and after 1350 DEG C of calcinings, nano aluminium oxide presents good
Good sintering is well combined between particle.Separation membrane layer surface does not have big hole defect, even aperture distribution.
Claims (7)
1. a kind of combined flat plate ceramic honey comb film, it is characterised in that: be made of tabular ceramic honey comb film unit split；It is described
Outer lower face surface is separation membrane layer to tabular ceramic honey comb film unit thereon, interior to have single or double penetrating fluid duct；It is described
Tabular ceramic honey comb film unit is narrow boards shape, and width≤15cm, the edge shape of two avris is in center rotational symmetry；Institute
It states and is connected in the width direction with avris between tabular ceramic honey comb film unit, is connected in beveled structure or W type corrugated split.
2. combined flat plate ceramic honey comb film according to claim 1, it is characterised in that: the tabular ceramic honey comb film
Its edge cross-section shape of the avris of unit is one of straight line, camber line, curve, broken line or combinations thereof.
3. the preparation method of combined flat plate ceramic honey comb film as claimed in claim 1 or 2, it is characterised in that: the wherein plate
The preparation of shape ceramic honey comb film unit, comprising the following steps:
(1) supporter of extrusion moulding preparation tabular ceramic honey comb film unit
After mixing by aluminium oxide, pore creating material, binder, lubricant, plasticizer, water is added to mediate in clay kneading machine and form mud
Material；The pore creating material, binder, lubricant, plasticizer, water dosage be respectively 1~8wt% of aluminium oxide, 2~6wt%, 3~
6wt%, 0.5~1.5wt%, 10~18wt%；After the pug passes through horizontal extruder extrusion molding, through drying, calcining, obtain
Both ends are in the supporter of the tabular ceramic honey comb film unit of center rotational symmetry；
(2) separation membrane layer of ink-jet printing preparation tabular ceramic honey comb film unit
Aluminium oxide, dispersing agent, stabilizer, water are mixed and obtain stable suspension, the use of the dispersing agent, stabilizer, water
Amount is respectively 0.5~1.2wt%, 1~4wt%, the 700~920wt% of aluminium oxide；The suspension is placed in ink-jet printer,
It is sprayed at the surface of the tabular ceramic honey comb film unit supporter and obtains separation membrane layer；It is controlled by control ink ejection amount
The thickness of separation membrane layer obtains tabular ceramic honey comb film unit after drying, calcining.
4. the preparation method of combined flat plate ceramic honey comb film according to claim 3, it is characterised in that: the step
(1) average particle size≤40 μm of aluminium oxide in；The calcination temperature is 1500~1650 DEG C, and calcination time is 2~4h；It is described flat
The average pore size of the supporter of plate ceramic honey comb film unit is 1~4.5 μm.
5. the preparation method of combined flat plate ceramic honey comb film according to claim 3, it is characterised in that: the step
(2) average particle size of aluminium oxide is 0.5~1 μm in；The separation membrane layer with a thickness of 15~25 μm；The calcination temperature is
1300~1450 DEG C, calcination time is 2~4h；The average pore size of the separation membrane layer of the tabular ceramic honey comb film unit is
0.1~0.5 μm.
6. the preparation method of combined flat plate ceramic honey comb film according to claim 3, it is characterised in that: the step
(1) pore creating material is starch in；Binder is carboxymethyl cellulose, in methylcellulose, polyvinyl alcohol, hydroxypropyl methyl cellulose
One kind or combinations thereof；Lubricant is glycerol and/or oleic acid；Plasticizer is polyvinyl alcohol.
7. the preparation method of combined flat plate ceramic honey comb film according to claim 3, it is characterised in that: the step
(2) dispersing agent is one of polyacrylic acid, Dolapix Series Dispersant, polyvinylpyrrolidone or combinations thereof in, alternatively,
For polyethyleneimine and/or polyvinylpyrrolidone；Stabilizer is poly propenoic acid aziridine, polyvinyl pyrilodone, gathers
One of vinyl alcohol or combinations thereof.
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Families Citing this family (3)
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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 |
| 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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| CN106215704A (en) | 2016-12-14 |
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