CN108911706A - A kind of co-sintering preparation method of fly ash base ceramic micro filter film - Google Patents
A kind of co-sintering preparation method of fly ash base ceramic micro filter film Download PDFInfo
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Abstract
The present invention relates to a kind of co-sintering preparation methods of inexpensive fly ash base ceramic membrane.By adulterating rigid oxide whisker in flyash whisker, the then coating alumina ceramic micro filter film on green compact fly ash base carrier, using co-sintering technology, step sintering is prepared for fly ash base ceramic micro filter film.The doping of rigid whisker alleviates flyash carrier excess shrinkage, has matched the macroscopic property of top layer pellumina, and perfect sunken fly ash base ceramic membrane can be prepared by one step of co-sintering technology.Cost of material and sintering energy consumption that fly ash base ceramic micro filter film considerably reduces ceramic membrane are prepared, the performance of ceramic micro filter film more reported in the literature is higher.
Description
Technical field
The present invention relates to a kind of co-sintering preparation methods of inexpensive fly ash base ceramic micro filter film, belong to membrane material preparation
Field.
Background technique
It is unrivaled that ceramic membrane with its excellent material property shows organic film in many harsh application systems
Advantage, but the higher preparation cost of ceramic membrane is a very important problem, it has also become limitation ceramic membrane is applied main
Factor, the preparation cost for how reducing ceramic membrane become one of the key problem of current ceramic field concern.
Co-sintering technology is simultaneously from shortening technique and reducing the angle of energy consumption, by original multiple sintering process letter
It is melted into once sintered process, the sintering energy consumption and preparation cost of material can be greatly lowered, shorten the manufacturing cycle of material,
It is widely used in function ceramics element, oxide fuel cell and the preparation process of ceramic membrane, and is made pottery in multichannel
Also good application has been obtained in the preparation process of porcelain microfiltration membranes.When different material layer etc. carries out co-sintering, need to control difference
Reaction and interface diffusion between interface, need to match the cofiring performance of each dielectric layer, make densification rate, sintering shrinkage and heat
The parameters such as expansion rate reach unanimously as far as possible, be otherwise easy to produce layer split, warpage and the defects of crackle.
Dong etc. (J Membr Sci, 2006,281:592-599) with two kinds of low costs and the similar violet of macroscopic property
Green stone powder is raw material, is prepared for high-performance ceramic microfiltration membranes by co-sintering technology, average pore size be respectively 1.55 μm and
2.17μm.Feng etc. (J Membr Sci, 2007,305:20-26) propose co-sintering process in addition to needing to investigate two layers of membrane material
Outside matching and film layer defects controlling in sintering character, it is also necessary to pay attention to co-sintering process in conjunction with the section between carrier
Intensity.Qiu etc. (J Mater Sci, 2009,44:Depth analysis 689-699) is carried out to co-sintering theory on this basis, it is right
The limited sintering micro pore structure of supported film has carried out improvement and pervasive Journal of Sex Research, to accumulation mode, soaking time in sintering process
And the direction film layer z caused by carrier restriction effect accelerates the factors such as contraction to be investigated, and uses improved model pair
Zirconium oxide supported film predicts the parameters such as pore-size distribution, porosity, thicknesses of layers after 1000 DEG C or so sintering.In addition,
(J the Membr Sci, 2010,348 (1-2) such as Qiu:252-259) in this theoretical basis, using titanium oxide sol and titanium oxide
Whisker is configured to preparation liquid as transition zone, and pure zirconia titanium colloidal sol is as top layer separating layer, on the carrier that average pore size is 3 μm
The double-deck titanium oxide ultrafiltration membrane is prepared for using the sintering of one step of co-sintering technique.
Summary of the invention
A kind of being total to for fly ash base ceramic micro filter film is proposed the purpose of the invention is to improve the deficiencies in the prior art
Sintering preparation method alleviates the contraction rate of carrier and the contraction rate one of separating layer membrane by the doping of rigid whisker
It causes, high-performance fly ash base ceramic micro filter film is prepared for using one step of co-sintering technology, considerably reduces the sintering of ceramic membrane
Energy consumption and cost of material.
The technical scheme is that：A kind of co-sintering preparation method of fly ash base ceramic micro filter film, specific steps
It is as follows：Flyash after classification is pressed with rigid oxide whisker and is mixed than column by A, and binder is then added, and by mixing, is refined
After mud, granulation, by dry-pressing formed, extrusion green compact chip flyash-whisker carrier；B by the alumina powder of certain partial size, point
Powder and thickener prepare stable microfiltration membranes preparation liquid under ultrasonication, by preparation liquid using spray gun spraying in green sheet
On formula flyash-whisker carrier, by drying, co-sintering process, fly ash base ceramic micro filter film is obtained.
It is preferred that the flyash after the classification is to carry out separation raw material flyash using the sieve of 100-1000 mesh.
It is preferred that the rigid oxide whisker is from one of mullite, aluminium oxide, silicon carbide or silica whisker
Or it is a variety of；Rigid whisker and flyash use mechanical stirring 1-60min；The mass ratio of rigid oxide whisker and flyash is
1:(6-10)。
It is preferred that the binder is one or more of glycerol, polyvinyl alcohol or methylcellulose；Wherein bond
The additive amount of agent is the 2%-10% for accounting for flyash and whisker gross mass.
It is preferred that molded pressure is 5MPa-30MPa, pressing time 5-60s.
It is preferred that the partial size of the alumina powder is between 300-1000nm；The thickener be methylcellulose,
One or more of polyvinyl alcohol or polyethylene glycol；Dispersing agent is one of nitric acid, sulfuric acid or hydrochloric acid；The film of preparation
The mass fraction of aluminium oxide is 5%-35% in liquid, and the mass fraction of thickener is controlled in 5%-20%, the additional amount of dispersing agent
It is 2-4 to control the pH value of preparation liquid.
It is preferred that spray gun is used to spray the spraying number of preparation liquid on green compact chip flyash-whisker carrier as 2-16 times,
Each spray time is 5-10 seconds.
It is preferred that the drying, co-sintering process are：Dry 12-24h at room temperature, then 70-120 DEG C at a temperature of
12-24h is dried, cofiring junction temperature controls between 900 DEG C -1100 DEG C, soaking time 1-5h, heating and rate of temperature fall control
In 0.5-3 DEG C/min.
The thicknesses of layers of fly ash base ceramic micro filter film produced by the present invention is 10-100 μm, average pore size 100-
300nm, permeability 400-2500Lm-2h-1bar-1。
Beneficial effect：
The present invention alleviates inexpensive carrier and small-bore ceramics is micro- by adulterating rigid fiber into fly ash base carrier
The matching problem of filter membrane during the sintering process, co-sintering are prepared for inexpensive fly ash base ceramic micro filter film, considerably reduce
The cost of material and sintering energy consumption of ceramic membrane.
Detailed description of the invention
Fig. 1 is the regulation figure of the fly ash base carrier shrinks rate in embodiment 3；
The SEM photograph of the fly ash base carrier of whisker is adulterated in the position Fig. 2 embodiment 3；
Fig. 3 is the fault structure figure of double-deck flyash-Alumina Membrane for Microfiltration in embodiment 3；
Fig. 4 is the exterior view of fly ash base ceramic micro filter film in embodiment 3；
Fig. 5 is fly ash base ceramic micro filter film graph of pore diameter distribution in embodiment 3.
Specific embodiment
Embodiment 1
Classification processing is carried out to flyash using the sieve of 100 mesh first, by the flyash and alumina whisker after classification
(mass ratio of rigid oxide whisker and flyash is 1:6) it using 1min is stirred, is added and accounts in powder upon mixing
The glycerol that flyash and alumina whisker gross mass are 2% carries out mixing, and mud refining prepares green compact by dry-pressing formed process
Chip flyash/whisker carrier controls pressure in 5Mpa, residence time 60s.Secondly the oxidation for being 300nm by average grain diameter
Aluminium powder body, a certain amount of sulfuric acid, a certain amount of polyvinyl alcohol are configured to stable preparation liquid under the action of Ultrasound Instrument, preparation
Preparation liquid in the mass fraction of aluminium oxide be 5wt.%, the mass fraction of thickener controls the system finally prepared in 20wt.%
The pH value of film liquid is 2.By spray gun spraying method, preparation liquid is sprayed on green compact chip flyash/whisker carrier, coating times are
2 times, each spray time is 5s.Dry 12h at room temperature, then 70 DEG C at a temperature of dry 12h, the control of cofiring junction temperature
At 900 DEG C, soaking time 5h, heating and rate of temperature fall control are in 0.5 DEG C/min.The film for the fly ash base microfiltration membranes prepared
Layer average pore size is 100nm, and thicknesses of layers is 10 μm, permeance property 950Lm-2h-1bar-1。
Embodiment 2
Classification processing is carried out to flyash using the sieve of 1000 mesh first, by the flyash and silicon carbide whisker after classification
(mass ratio of rigid oxide whisker and flyash is 1:10) mixing 60min, powder upon mixing are carried out using tradition stirring
It is added in body and accounts for flyash and alumina whisker gross mass as 10% polyvinyl alcohol progress mixing, mud refining, by dry-pressing formed
Process prepares green compact chip flyash/whisker carrier, controls pressure in 30Mpa, residence time 5s.It secondly will average grain
Diameter is alumina powder, a certain amount of hydrochloric acid of 1000nm, and a certain amount of polyethylene glycol is configured to steady under the action of Ultrasound Instrument
Fixed preparation liquid, the mass fraction of aluminium oxide is 35wt.% in the preparation liquid of preparation, and the mass fraction control of thickener exists
5wt.%, the pH value of the preparation liquid finally prepared are 4.By spray gun spraying method, by preparation liquid be sprayed on green compact chip flyash/
Whisker carrier, coating times are 16 times, and each spray time is 10s.Dry at room temperature for 24 hours, then 120 DEG C at a temperature of
For 24 hours, cofiring junction temperature is controlled at 1100 DEG C, soaking time 1h for drying, and heating and rate of temperature fall control are in 3 DEG C/min.Preparation
Film layer average pore size out is 300nm, and thicknesses of layers is 100 μm, permeance property 2500Lm-2h-1bar-1。
Embodiment 3
Classification processing is carried out to flyash using the sieve of 300 mesh first, by the flyash and mullite crystal whisker after classification
(mass ratio of rigid oxide whisker and flyash is 1:8) mixing 5min, powder upon mixing are carried out using tradition stirring
The polyvinyl alcohol that middle addition accounts for flyash and alumina whisker gross mass is 4% carries out mixing, and mud refining passes through dry-pressing formed mistake
Journey prepares green compact chip flyash/whisker carrier, controls pressure in 20Mpa, residence time 20s.Secondly by average grain diameter
Alumina powder, a certain amount of nitric acid for 300nm, a certain amount of methylcellulose are configured to steady under the action of Ultrasound Instrument
Fixed preparation liquid, the mass fraction of aluminium oxide is 20wt.% in the preparation liquid of preparation, and the mass fraction control of thickener exists
14wt.%, the pH value of the preparation liquid finally prepared are 2.By spray gun spraying method, preparation liquid is sprayed on green compact chip fine coal
Ash/whisker carrier, coating times are 8 times, and each spray time is 6s.Dry 18h at room temperature, then 70 DEG C at a temperature of
18h is dried, cofiring junction temperature is controlled at 1050 DEG C, soaking time 2h, and heating and rate of temperature fall control are in 2 DEG C/min.Preparation
Film layer average pore size out is 100nm, and thicknesses of layers is 40 μm, permeance property 450Lm-2h-1bar-1.Fig. 1 is the present embodiment
Middle ceramic monolith and microfiltration membranes contraction rate, the doping of mullite crystal whisker can slow down the contraction rate of fly ash base carrier.Fig. 2
It is the SEM photograph of the flyash carrier in the present embodiment, to characterize the microscopic appearance for preparing carrier.As can be seen from the figure fine coal
Apparent rigid whisker is mixed in grey carrier, and there is no impact the integrality of carrier surface for the addition of whisker.Fig. 3
It is the film layer structure for the fly ash base ceramic micro filter film that in the present embodiment prepared by co-sintering, wherein thicknesses of layers is about 40-50 μ
M or so.The SEM electromicroscopic photograph of the microfiltration membranes prepared in Fig. 4 the present embodiment, surface is completely without defect.It is made in Fig. 5 the present embodiment
The pore-size distribution of standby fly ash base ceramic micro filter film, aperture are about 100nm or so.The micro-filtration prepared in 1 the present embodiment of table
The comparison of performance in film and document, as seen from the figure, the pico- filter (average pore size is 100nm or so) of this method preparation is compared with document ratio
More preferable compared with permeability, cost is lower.
Embodiment 4
Classification processing is carried out to flyash using the sieve of 300 mesh first, by the flyash and silica whisker after classification
(mass ratio of rigid oxide whisker and flyash is 1:8) mixing 5min, powder upon mixing are carried out using tradition stirring
The glycerol that middle addition accounts for flyash and alumina whisker gross mass is 4% carries out mixing, and mud refining passes through dry pressing, preparation
Green sheet formula flyash/whisker carrier out controls pressure in 20Mpa, residence time 20s.It secondly is 300nm by average grain diameter
Alumina powder, a certain amount of nitric acid, a certain amount of methylcellulose is configured to stable film under the action of Ultrasound Instrument
Liquid, the mass fraction of aluminium oxide is 20wt.% in the preparation liquid of preparation, and the mass fraction of thickener is controlled in 14wt.%, finally
The pH value of the preparation liquid of preparation is 2.By spray gun spraying method, preparation liquid is sprayed on green compact chip flyash/whisker carrier, is applied
Film number is 8 times, and each spray time is 6s.Dry 18h at room temperature, then 70 DEG C at a temperature of dry 18h, co-sintering
Temperature is controlled at 1050 DEG C, soaking time 2h, and heating and rate of temperature fall control are in 2 DEG C/min.The film layer prepared is averaged hole
Diameter is 100nm, and thicknesses of layers is 40 μm, permeance property 400Lm-2h-1bar-1。
Table 1 is that the microfiltration membranes of preparation in embodiment 3 and document compare, as seen from table, the microfiltration membranes of this method preparation
(average pore size be 100nm or so) compares that permeability is more preferable, and cost is lower compared with document
The micro-filtration film properties and document of 1 embodiment 3 of table preparation compare the (unit in aperture：Nm, permeance property unit:Lm-2h-1bar-1)
Claims (9)
1. a kind of co-sintering preparation method of fly ash base ceramic micro filter film, specific step is as follows：A is by the flyash after classification
It presses with rigid oxide whisker and is mixed than column, binder is then added, after mixing, mud refining, granulation, by dry-pressing formed
Method extrudes green compact chip flyash-whisker carrier；B makees the alumina powder, dispersing agent and thickener of certain partial size in ultrasound
With lower obtained microfiltration membranes preparation liquid, by microfiltration membranes preparation liquid using spray gun spraying on green compact chip flyash-whisker carrier, warp
Dry, co-sintering process is crossed, fly ash base ceramic micro filter film is obtained.
2. co-sintering preparation method according to claim 1, it is characterised in that：Flyash after the classification is to use
The sieve of 100-1000 mesh carries out separation raw material flyash.
3. co-sintering preparation method according to claim 1, it is characterised in that：The rigid oxide whisker is from not
Come one or more of stone, aluminium oxide, silicon carbide or silica whisker；Rigid whisker and flyash use mechanical stirring 1-
60min；The mass ratio of rigid oxide whisker and flyash is 1:(6-10).
4. co-sintering preparation method according to claim 1, it is characterised in that：The binder is glycerol, polyethylene
One or more of alcohol or methylcellulose；Wherein the addition quality of binder is to account for flyash and whisker gross mass
2%-10%.
5. co-sintering preparation method according to claim 1, it is characterised in that：Pressure during dry-pressing formed is
5MPa-30MPa, pressing time 5-60s.
6. co-sintering preparation method according to claim 1, it is characterised in that：The partial size of the alumina powder exists
Between 300-1000nm；The thickener is one or more of methylcellulose, polyvinyl alcohol or polyethylene glycol；Point
Powder is one of nitric acid, sulfuric acid or hydrochloric acid；The mass fraction of aluminium oxide is 5%-35% in the microfiltration membranes preparation liquid of preparation,
The mass fraction of thickener is controlled in 5%-20%, and the additional amount of dispersing agent is that the pH value of control film liquid is 2-4.
7. co-sintering preparation method according to claim 1, it is characterised in that：Using spray gun in green compact chip flyash-
The spraying number that preparation liquid is sprayed on whisker carrier is 2-16 times, and each spray time is 5-10 seconds.
8. co-sintering preparation method according to claim 1, it is characterised in that：The drying, co-sintering process are：?
Dry 12-24h at room temperature, then 70-120 DEG C at a temperature of dry 12-24h, cofiring junction temperature is controlled at 900 DEG C -1100
Between DEG C, soaking time 1-5h, heating and rate of temperature fall control are in 0.5-3 DEG C/min.
9. co-sintering preparation method according to claim 1, it is characterised in that：Fly ash base ceramic micro filter film obtained
Thicknesses of layers is 10-100 μm, average pore size 100-300nm, permeability 400-2500Lm-2h-1bar-1。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110357655A (en) * | 2019-07-23 | 2019-10-22 | 武汉理工大学 | A kind of biomimetic features silicon carbide-based porous ceramics and preparation method thereof |
| CN111763069A (en) * | 2020-07-10 | 2020-10-13 | 武汉理工大学 | Waste FCC catalyst ceramic membrane support and preparation method and application thereof |
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| CN110357655A (en) * | 2019-07-23 | 2019-10-22 | 武汉理工大学 | A kind of biomimetic features silicon carbide-based porous ceramics and preparation method thereof |
| CN110357655B (en) * | 2019-07-23 | 2021-09-14 | 武汉理工大学 | Silicon carbide-based porous ceramic with bionic structure and preparation method thereof |
| CN112661493A (en) * | 2019-10-16 | 2021-04-16 | 国家能源投资集团有限责任公司 | Modified fly ash support body, modification method of fly ash support body, fly ash ceramic membrane, preparation method and application of fly ash ceramic membrane |
| CN111763069A (en) * | 2020-07-10 | 2020-10-13 | 武汉理工大学 | Waste FCC catalyst ceramic membrane support and preparation method and application thereof |
| CN115155334A (en) * | 2021-04-01 | 2022-10-11 | 国家能源投资集团有限责任公司 | Coal-based solid waste coating liquid and application thereof, coal-based solid waste ceramic membrane and preparation method and application thereof |
| CN115180926A (en) * | 2021-04-01 | 2022-10-14 | 国家能源投资集团有限责任公司 | Coal-based solid waste-alumina composite ceramic membrane and preparation method and application thereof |
| CN115180926B (en) * | 2021-04-01 | 2023-09-12 | 国家能源投资集团有限责任公司 | Coal-based solid waste-alumina composite ceramic membrane and preparation method and application thereof |
| CN115155334B (en) * | 2021-04-01 | 2023-12-22 | 国家能源投资集团有限责任公司 | Coal-based solid waste coating liquid and application thereof, coal-based solid waste ceramic membrane and preparation method and application thereof |
| CN113336529A (en) * | 2021-07-12 | 2021-09-03 | 南京九思高科技有限公司 | Multi-channel water-in-oil type emulsion membrane and preparation method thereof |
| CN113336529B (en) * | 2021-07-12 | 2023-01-31 | 南京九思高科技有限公司 | Multi-channel water-in-oil type emulsion membrane and preparation method thereof |
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