CN105000871B - A kind of multifunctional flat ceramic membrane and its preparation technology - Google Patents
A kind of multifunctional flat ceramic membrane and its preparation technology Download PDFInfo
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- CN105000871B CN105000871B CN201510396590.9A CN201510396590A CN105000871B CN 105000871 B CN105000871 B CN 105000871B CN 201510396590 A CN201510396590 A CN 201510396590A CN 105000871 B CN105000871 B CN 105000871B
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Abstract
The invention provides a kind of preparation technology of multifunctional flat ceramic membrane, comprise the following steps:S1, using extrusion moulding produce flat ceramic film support;S2, multifunctional flat ceramic membrane is prepared using vacuum impregnation technology.Present invention also offers a kind of multifunctional flat ceramic membrane.The beneficial effects of the invention are as follows:The multifunctional flat ceramic membrane for preparing not only has filtering function, the other functions such as is also equipped with being catalyzed, aoxidizes;Production cost is greatly reduced, and flux can be set in higher level;Fouling membrane performance and restorability are significantly improved;Fenestra size is easily controlled.
Description
Technical field
The present invention relates to the preparation technology of ceramic membrane, more particularly to a kind of multifunctional flat ceramic membrane and its preparation technology.
Background technology
The film overwhelming majority that water process is used is macromolecule organic film (based on PVDF, PVC, PES etc.), but organic film is anti-
Oxidability and contamination resistance are generally poor, limit its range of application, such as in drinking water treatment be difficult with ozone combination,
Sewage disposal flux it is relatively low and decline quickly, be difficult to apply to the complicated special industry water treatment field of water quality.With organic film phase
Possess advantage at many aspects than, ceramic membrane, be such as made of the aluminum oxide of good hydrophilic property, transmembrane pressure is low, be difficult by organic
Thing pollutes;Acid-resistant and anti-high-temperature, is not likely to produce fouling membrane, considerably increases service life.
The ceramic membrane of current production both at home and abroad is generally tubular filter film, and aperture is generally micron order or so, the life of these products
High cost is produced, is usually used in chemical industry or field of food, in order to reduce investment, flux design is higher, and energy consumption is big, fouling membrane is big;Fenestra
Size is difficult direct visual test, is not suitable for field of Environment Protection;Ceramic membrane only possesses filtering function, it is difficult to ozonisation, catalysis,
The high-level oxidation technologies such as antipollution are combined, it is impossible to play more multi-functional, therefore have to dissolubility or micro-content organism removal ability
Limit.
The content of the invention
In order to solve the problems of the prior art, the invention provides a kind of multifunctional flat ceramic membrane and its preparation work
Skill, the multifunctional flat ceramic membrane of preparation not only has filtering function, the other functions such as is also equipped with being catalyzed, aoxidizes;Production cost
It is greatly reduced, flux can be set in higher level;Fouling membrane performance and restorability are significantly improved;Fenestra size is easily controlled.
The invention provides a kind of preparation technology of multifunctional flat ceramic membrane, comprise the following steps:
S1, using extrusion moulding produce flat ceramic film support;
S2, multifunctional flat ceramic membrane is prepared using vacuum impregnation technology.
As a further improvement on the present invention, step S1 includes following sub-step:
It is prepared by S101, pug;80~90wt% of high purity aluminium hydroxide, 5~12wt% of pore creating material, base substrate are bonded in proportion
3~8wt% of agent, 2~5wt% of plasticizer, 5~25wt% of water are well mixed, and pouring into carries out mud refining in vacuum pugmill, finally put
Enter 20h~30h in vapor tight tank;
S102, body preparation;
S103, body drying;
S104, blank sintering, are obtained flat ceramic film support.
As a further improvement on the present invention, in step S102, the pug that will be prepared uses extrusion molding, extrusion pressure
It is 5~15MPa.
As a further improvement on the present invention, in step S103, base substrate is put into 40~50 DEG C of drying box and dries 2~
10h。
As a further improvement on the present invention, in step S104, dried base substrate is burnt in 1200~1400 DEG C
Knot.
As a further improvement on the present invention, the raw material of the flat ceramic film support use high-purity hydroxide
Aluminium, between 2~5 μm, the pore creating material is polyvinyl alcohol or starch to its average grain diameter, and average grain diameter is 0.5~1 μm;Bond
Agent uses carboxymethylcellulose calcium;Plasticizer uses polyacrylamide, and molecular weight is 1000~15,000,000.
As a further improvement on the present invention, step S2 includes following sub-step:
S201, maceration extract are prepared;Aluminum oxide, zirconium oxide, titanium oxide, binding agent, active component are made into by a certain percentage
Maceration extract;
S202, vacuum impregnation film;
S203, film are dried;
S204, film sintering, are obtained multifunctional flat ceramic membrane.
As a further improvement on the present invention, in step S202, first in 90~110 DEG C of 1~3h of drying of drying box before film,
Removal supporting body surface and the moisture of inside;In step S203, the film that will be hung up properly is in 40~60 DEG C of 2~12h of drying.
As a further improvement on the present invention, in step S204, dried ceramic membrane is burnt in 800~1500 DEG C
Knot.
As a further improvement on the present invention, impregnated raw material is:In aluminum oxide, zirconium oxide or titanium oxide any one or
Several, the particle diameter of every kind of impregnated raw material is each about 10~200 nm;Binding agent is activated silicic acid;Active component be palladium, platinum, nickel,
Any one or a few in cobalt, manganese.
Present invention also offers a kind of multifunctional flat ceramic membrane, the multifunctional flat ceramic membrane is by any as described above
The preparation technology of the function ceramic membrane described in is prepared from.
The beneficial effects of the invention are as follows:By such scheme, the multifunctional flat ceramic membrane for preparing not only had
Filter function, the other functions such as is also equipped with being catalyzed, aoxidizes;Production cost is greatly reduced, and flux can be set in higher level;Fouling membrane
Performance and restorability are significantly improved;Fenestra size is easily controlled.
Specific embodiment
With reference to specific embodiment, the present invention is further described.
A kind of preparation technology of multifunctional flat ceramic membrane is comprised the following steps:
It is prepared by flat ceramic film support:(1)Raw material:It is high-purity that the raw material of the flat ceramic film support are used
Aluminium hydroxide, its average grain diameter between 2~5 μm, preferably 2 μm, 3 μm, 4 μm, 5 μm;Pore creating material is selected from polyvinyl alcohol or shallow lake
Powder etc., about 0.5~1 μm or so, preferably 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm, 1 μm of average grain diameter;Binding agent is adopted
With carboxymethylcellulose calcium etc.;Plasticizer uses polyacrylamide, and molecular weight is 1000~15,000,000, preferably 10,000,000,1100
Ten thousandth, 12,000,000,13,000,000,14,000,000,15,000,000;(2)Production technology:1. prepared by pug:In proportion by high purity aluminium hydroxide 80
~90wt%, 5~12wt% of pore creating material, 3~8wt% of base substrate binding agent, 2~5wt% of plasticizer, 5~25wt% of water, by raw material
Well mixed, pouring into carries out pugging in vacuum deairing machine, be finally putting into 20h~30h in vapor tight tank;2. body preparation:To prepare
Good pug uses extrusion molding, 5~15MPa of extrusion pressure;3. body drying:Base substrate is put into 40~50 DEG C of drying box
Dry 2~10h;4. blank sintering:Dried base substrate is sintered in 1200~1400 DEG C, ceramic membrane support is obtained
Body.
Flat ceramic film support prepare preferred embodiment 1 be:1. prepared by pug:In proportion by high purity aluminium hydroxide
80wt%, pore creating material 5wt%, base substrate binding agent 3wt%, plasticizer 2wt%, water 5wt%, raw material is well mixed, and is poured into true
Pugging is carried out in empty pug mill, 20h in vapor tight tank is finally putting into;2. body preparation:The pug that will be prepared uses extrusion molding,
Extrusion pressure 5MPa;3. body drying:Base substrate is put into 40 DEG C of drying box and dries 2h;4. blank sintering:Will be dried
Base substrate is sintered in 1200 DEG C, and flat ceramic film support is obtained.
Flat ceramic film support prepare preferred embodiment 2 be:1. prepared by pug:In proportion by high purity aluminium hydroxide
90wt%, pore creating material 12wt%, base substrate binding agent 8wt%, plasticizer 5wt%, water 25wt%, raw material is well mixed, and is poured into
Pugging is carried out in vacuum deairing machine, 30h in vapor tight tank is finally putting into;2. body preparation:The pug that will be prepared is used and is extruded into
Type, extrusion pressure 15MPa;3. body drying:Base substrate is put into 50 DEG C of drying box and dries 10h;4. blank sintering:By drying
Good base substrate is sintered in 1400 DEG C, and flat ceramic film support is obtained.
Multifunctional flat ceramics film preparation:(1)Impregnated raw material:Aluminum oxide, zirconium oxide or titanium oxide etc. one or more, often
Plant raw material particle size and be each about 10~200 nm, preferably 10 nm, 100 nm, 200 nm;Binding agent is activated silicic acid etc.;(2)Instead
Active component is answered, is needed that the compositions such as palladium, platinum, nickel, cobalt, manganese can be added according to applied environment;(3)Preparation technology:1. maceration extract is matched somebody with somebody
System.Aluminum oxide, zirconium oxide, titanium oxide, binding agent, active component are made into maceration extract by a certain percentage;2. vacuum impregnation film.
First the moisture of supporting body surface and inside is removed before film in 90~110 DEG C of 1~3h of drying of drying box;3. film is dried.To hang up properly
Film in 40~60 DEG C of 2~12h of drying.4. film is sintered:Dried ceramic membrane is sintered in 800~1500 DEG C, is obtained
Multifunctional flat ceramic membrane.
Multifunctional flat ceramics film preparation embodiment 1 be:1. maceration extract is prepared.By aluminum oxide, zirconium oxide, titanium oxide,
Binding agent, active component are made into maceration extract by a certain percentage;2. vacuum impregnation film.First in 90 DEG C of dryings of drying box before film
The moisture of 1h, removal supporting body surface and inside;3. film is dried.The film that will be hung up properly dries 2h at 40 DEG C.4. film is sintered:By drying
Good ceramic membrane is sintered in 800 DEG C, and multifunctional flat ceramic membrane is obtained.
Multifunctional flat ceramics film preparation embodiment 2 be:1. maceration extract is prepared.By aluminum oxide, zirconium oxide, titanium oxide,
Binding agent, active component are made into maceration extract by a certain percentage;2. vacuum impregnation film.First in 110 DEG C of dryings of drying box before film
The moisture of 3h, removal supporting body surface and inside;3. film is dried.The film that will be hung up properly dries 12h at 60 DEG C.4. film is sintered:Will be dry
Dry good ceramic membrane is sintered in 1500 DEG C, and multifunctional flat ceramic membrane is obtained.
A kind of preparation technology of multifunctional flat ceramic membrane that the present invention is provided,(1)Extrusion moulding produces flat ceramic
Film support:Ceramic film support is prepared by primary raw material sintering of high purity aluminium hydroxide, ceramic film support can be greatly increased
Stability, and ensure that the enough intensity of supporter;(2)Vacuum impregnation technology prepares ceramic membrane.The present invention is preparing pottery
During porcelain film support, selected primary raw material is aluminum oxide, zirconium oxide or titanium oxide etc., while adding palladium, platinum, nickel, cobalt, manganese
Isoreactivity composition.Can be very good to control ceramic film quality, control thicknesses of layers, and film layer even aperture distribution;Film layer and branch
Inorganic bond is used between support body, film layer is tightly combined, and sintering temperature is low;Not only there is filtering function, catalysis, oxygen is also equipped with
The other functions such as change, antipollution;Ceramic membrane production cost, improve production efficiency can be effectively reduced, water process is can be widely used for, is given up
The field such as gas disposal and separation of solid and liquid.
Present invention also offers a kind of multifunctional flat ceramic membrane, the multifunctional flat ceramic membrane is by any as described above
The preparation technology of the function ceramic membrane described in is prepared from.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
Specific implementation of the invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should be all considered as belonging to of the invention
Protection domain.
Claims (9)
1. a kind of preparation technology of multifunctional flat ceramic membrane, it is characterised in that comprise the following steps:
S1, using extrusion moulding produce flat ceramic film support;
S2, multifunctional flat ceramic membrane is prepared using vacuum impregnation technology;
Wherein,
Step S2 includes following sub-step:
S201, maceration extract are prepared;Aluminum oxide, zirconium oxide, titanium oxide, binding agent, active component are made into maceration extract in proportion;
S202, vacuum impregnation film;
S203, film are dried;
S204, film sintering, are obtained multifunctional flat ceramic membrane.
2. the preparation technology of multifunctional flat ceramic membrane according to claim 1, it is characterised in that step S1 includes following
Sub-step:
It is prepared by S101, pug;In proportion by 80~90wt% of high purity aluminium hydroxide, pore creating material 5wt%, base substrate binding agent 3~
8wt%, 2~5wt% of plasticizer, water 5wt% are well mixed, and pouring into carries out mud refining in vacuum pugmill, be finally putting into vapor tight tank
Interior 20h~30h;
S102, body preparation;
S103, body drying;
S104, blank sintering, are obtained flat ceramic film support.
3. the preparation technology of multifunctional flat ceramic membrane according to claim 2, it is characterised in that:In step S102, will
The pug for preparing uses extrusion molding, and extrusion pressure is 5~15MPa.
4. the preparation technology of multifunctional flat ceramic membrane according to claim 2, it is characterised in that:In step S103, will
Base substrate dries 2~10h in being put into 40~50 DEG C of drying box.
5. the preparation technology of multifunctional flat ceramic membrane according to claim 2, it is characterised in that:In step S104, will
Dried base substrate is sintered in 1200~1400 DEG C.
6. the preparation technology of multifunctional flat ceramic membrane according to claim 2, it is characterised in that:The ceramic membrane
The raw material of supporter use high purity aluminium hydroxide, and between 2~5 μm, the pore creating material is polyethylene to its average grain diameter
Alcohol or starch, average grain diameter are 0.5~1 μm;Binding agent uses carboxymethylcellulose calcium;Plasticizer uses polyacrylamide, molecule
Measure is 1000~15,000,000.
7. the preparation technology of multifunctional flat ceramic membrane according to claim 1, it is characterised in that:In step S202, apply
First flat ceramic 1~3h of film support is dried before film in 90~110 DEG C of drying box, removal ceramic membrane supporting body surface and interior
The moisture in portion;In step S203, the film that will be hung up properly in 40~60 DEG C of 2~12h of drying, in step S204, by dried ceramics
Film is sintered in 800~1500 DEG C.
8. the preparation technology of multifunctional flat ceramic membrane according to claim 1, it is characterised in that:Impregnated raw material is:Oxygen
Change aluminium, zirconium oxide and titanium oxide, the particle diameter of every kind of impregnated raw material is 10~200 nm;Binding agent is activated silicic acid;Activity into
It is divided into any one or a few in palladium, platinum, nickel, cobalt, manganese.
9. a kind of multifunctional flat ceramic membrane, it is characterised in that:The multifunctional flat ceramic membrane is by such as claim 1 to 8
Any one of the preparation technology of multifunctional flat ceramic membrane be prepared from.
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CN106238102A (en) * | 2016-08-26 | 2016-12-21 | 北京理工大学 | There are the preparation method and applications of chirality Salen catalysis ceramic membrane |
CN106390767A (en) * | 2016-11-08 | 2017-02-15 | 华南理工大学 | Honeycomb ceramic composite membrane and method for preparing same |
CN106810212B (en) * | 2016-12-30 | 2020-10-23 | 海天水务集团股份公司 | Manufacturing process of efficient flat ceramic membrane |
CN109516822B (en) * | 2017-09-19 | 2022-02-18 | 萍乡市普天高科实业有限公司 | High-strength filtering ceramic material and preparation method thereof |
CN111056858A (en) * | 2019-12-20 | 2020-04-24 | 上海巴安水务股份有限公司 | Preparation method of flat ceramic membrane support and ceramic pug thereof |
CN111704439A (en) * | 2020-06-05 | 2020-09-25 | 江苏埃梯恩膜过滤技术有限公司 | Ceramic pug of flat ceramic membrane for tap water treatment and preparation method |
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