CN107337442A - A kind of particle stabilized foam process prepares alumina ceramic supporting body and preparation method thereof - Google Patents
A kind of particle stabilized foam process prepares alumina ceramic supporting body and preparation method thereof Download PDFInfo
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- CN107337442A CN107337442A CN201710559212.7A CN201710559212A CN107337442A CN 107337442 A CN107337442 A CN 107337442A CN 201710559212 A CN201710559212 A CN 201710559212A CN 107337442 A CN107337442 A CN 107337442A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
A kind of particle stabilized foam process prepares alumina ceramic supporting body, it is characterised in that first by kaolin and zinc oxide combination drying, wet ball grinding, drying, obtains mixed-powder；Then after mixing alumina powder and mixed-powder, using titanium sulfate as presoma, Membranes On Alumina Particles Surface is modified；The finally gel injection-moulding system using acrylamide as high polymer monomer, mechanical agitation foaming, the solidification demoulding, dry and high temperature sintering, obtain particle stabilized foam process and prepare alumina ceramic supporting body.The alumina ceramic supporting body of the present invention, not only mechanical strength is good, permeation flux is high, and has good resistance to chemical corrosion.
Description
Technical field
The invention belongs to ceramic field, more particularly to a kind of particle stabilized foam process prepare alumina ceramic supporting body and
Its preparation method.
Background technology
Porous ceramic film is wide due to have the advantages that excellent heat endurance, chemical stability and being readily cleaned regeneration
Big scholar is of interest, is used widely at present in fields such as food, medicine, chemical industry, metallurgy, is particularly sent out in water treatment field
Wave important function.
Porous ceramic film is usually to be made up of supporter, transition zone and film layer three parts, and wherein supporter is porous ceramics
The basis of film application, it is desirable to which it has enough mechanical strengths and higher permeation flux, to ensure film layer process under arms
In stability.Ceramic supporting body at present on the market is the most frequently used for oxidation aluminium material, the particle diameter one of alumina raw material used
As at 20-40 μm.For 99 alumina ceramic supporting bodies, to ensure that it has sufficient mechanical strength, firing temperature is generally
1700 DEG C, even more high.Therefore the sintering temperature of alumina ceramic supporting body how is reduced, reduces and prepares cost as currently grinding
The emphasis studied carefully.
The content of the invention
It is an object of the invention to provide a kind of low particle stabilized foam process of cost to prepare alumina ceramic supporting body
And preparation method thereof.
In order to realize above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of particle stabilized foam process prepares alumina ceramic supporting body, it is characterised in that first by kaolin and zinc oxide
Combination drying, wet ball grinding, drying, obtain mixed-powder；Then after mixing alumina powder and mixed-powder, with titanium sulfate
For presoma, Membranes On Alumina Particles Surface is modified；The finally gel injection-moulding system using acrylamide as high polymer monomer, machine
Tool stirring foaming, the solidification demoulding, dry and high temperature sintering, obtains particle stabilized foam process and prepares alumina ceramic supporting body.
Described particle stabilized foam process prepares alumina ceramic supporting body, it is characterised in that it is by following steps system
It is standby to form：
（1）By kaolin, zinc oxide with 1：0.9-1.1 mass ratio mixing, is placed in 80-90 DEG C of vacuum drying chamber and dries 5-
6h, then through wet ball grinding, drying, pulverize and sieve to obtain the mixed-powder of 200-250 mesh, it is stand-by；
（2）By alumina powder and mixed-powder with 1：0.02-0.03 mass ratio is placed in reaction vessel, is added equivalent to oxygen
Change the deionized water of 15-20 times of aluminium micropowder weight part, ultrasonic vibration 50-60min, make its fully dispersed, sulphur is added dropwise while stirring
Sour titanium solution, magnetic agitation 30-40min, is then added dropwise ammoniacal liquor and adjusts the pH value of system to 9.5-10.5, continue magnetic at room temperature
Power stirs 2-3h, filtering, washing, dries, obtains surface modification alumina powder；
（3）By surface modification alumina powder, acrylic acid, acrylamide, N, N '-methylene-bisacrylamide, polyethylene glycol and
Deionized water is with 1：0.08-0.1：0.2-0.25：0.04-0.05：0.03-0.04：6-7 mass ratio mixing, is added to ball milling
In machine, drum's speed of rotation is ball milling mixing 4-5h under conditions of 600-800r/min；Add the fourth of 0.04-0.05 times of parts by weight
Acid, mix to uniformly, the pH value of regulation system under conditions of drum's speed of rotation is 300-400r/min, continues ball to 5-6
Mill mixing 2-3h, obtains ceramic slurry；
（4）Ceramic slurry is transferred in agitator, adds the ammonium persulfate and 0.004-0.005 of 0.008-0.01 times of parts by weight
The N, N, N of times parts by weight ', N '-tetramethylethylenediamine, starts to stir, and it is 250-300r/min to control agitator speed, stirring hair
5-8min is steeped, obtains ceramic foam slurry；
（5）Ceramic foam slurry is injected in mould rapidly, solidification 5-6min is stood, the demoulding, obtains foamed alumina ceramics embryo
Body；Ceramic wet blank is placed in 40-50 DEG C of baking oven and dries 20-24h, natural cooling, idiosome is put into Muffle furnace, with 2-3
DEG C/min heating rate temperature programming to 800-900 DEG C, be incubated 30-40min, continue with 2-3 DEG C/min heating rate point
Other temperature programming is to 1350 DEG C, 1400 DEG C, 1450 DEG C and 1500 DEG C, and each temperature section is incubated 20-30min, with 4-5 DEG C/min's
Rate of temperature fall is cooled to 500 DEG C, naturally cools to room temperature, obtains a kind of particle stabilized foam process and prepares aluminium oxide ceramics support
Body.
Described particle stabilized foam process prepares the preparation method of alumina ceramic supporting body, it is characterised in that step
（2）Titanium and the mass ratio of aluminum oxide are 1 in middle titanium sulfate solution：200-250.
Described particle stabilized foam process prepares the preparation method of alumina ceramic supporting body, it is characterised in that step
（4）The environment of Muffle furnace high-temperature calcination be atmospheric atmosphere.
By above-mentioned technical scheme, the beneficial effects of the invention are as follows：
The present invention obtains mixed-powder first by kaolin and zinc oxide combination drying, wet ball grinding, drying；Then will oxidation
After aluminium micro mist and mixed-powder mixing, using titanium sulfate as presoma, presoma is made with titanium sulfate, by cladding process to aluminum oxide
Powder surface is modified；On the one hand, the introducing of kaolin and titanium dioxide, kaolin can be used as fluxing agent, big of aluminum oxide
Realize that neck sinters by the reaction of the solid solution reaction and solid-phase sintering of titanium dioxide and aluminum oxide between grain, and then realize oxidation
The low temperature preparation of aluminium ceramic supporting body, reduce the sintering temperature for reducing alumina ceramic supporting body.The present invention is repaiied using butyric acid
Ceramic slurry is adornd, realizes that alumina particle is stable by mechanical agitation and foams, this is due to：On the one hand, have in butyric acid molecule
Hydrophobic group --- alkyl, after modifying powder granule, particle has more preferable hydrophobicity, so as to be easier to stable foam；It is another
Aspect, its acid degree of ionization of the carboxyl of butyric acid is big, and molecular weight is smaller, therefore is easy to absorption in alumina ceramic grain table
Face, realize the surface modification to alumina ceramic grain.Gel injection-moulding system of the present invention using acrylamide as high polymer monomer,
Aluminium oxide ceramics idiosome is prepared using gel injection molding process, its principle is that the monomers such as acrylamide come out in decomposition of initiator
Primary group of free radicals in the presence of form primary monomer free radical, by continuous chain addition reaction between macromolecule, formed and gathered
Acrylamide long-chain, network structure is formed in the presence of crosslinking agent, ceramic particle is fixed in network structure, ceramic particle with
Polymer gel forms the ceramic body with some strength by suction-operated.The present invention by by ceramic idiosome dry and
High temperature sintering, obtain particle stabilized foam process and prepare alumina ceramic supporting body, polymer gel produces in sintering process
Gas and burning are lost, and further increase the pore structure in alumina ceramic supporting body.The alumina ceramic supporting body of the present invention, no
Only mechanical strength is good, permeation flux is high, and has good resistance to chemical corrosion.
Embodiment
The particle stabilized foam process of the present embodiment prepares alumina ceramic supporting body, and it is prepared by following steps：
（1）By kaolin, zinc oxide with 1：0.9 mass ratio mixing, is placed in 90 DEG C of vacuum drying chamber and dries 6h, then through wet
Method ball milling, drying, pulverizes and sieves to obtain the mixed-powder of 250 mesh, stand-by；
（2）By alumina powder and mixed-powder with 1：0.03 mass ratio is placed in reaction vessel, is added equivalent to aluminum oxide
The deionized water that 20 times of micropowder weight part, ultrasonic vibration 60min, make its fully dispersed, titanium sulfate solution, room are added dropwise while stirring
The lower magnetic agitation 40min of temperature, ammoniacal liquor is then added dropwise and adjusts the pH value of system to 10, continue magnetic agitation 3h, filtering, washing,
Dry, obtain surface modification alumina powder；
（3）By surface modification alumina powder, acrylic acid, acrylamide, N, N '-methylene-bisacrylamide, polyethylene glycol and
Deionized water is with 1：0.1：0.25：0.05：0.04：7 mass ratio mixing, is added in ball mill, drum's speed of rotation 800r/
Ball milling mixing 5h under conditions of min；The butyric acid of 0.05 times of parts by weight is added, is mixed to uniformly, the pH value of regulation system is extremely
5, under conditions of drum's speed of rotation is 400r/min, continues ball milling mixing 3h, obtain ceramic slurry；
（4）Ceramic slurry is transferred in agitator, the ammonium persulfate of 0.01 times of parts by weight of addition and the N of 0.005 times of parts by weight,
N, N ', N '-tetramethylethylenediamine, start to stir, it is 300r/min to control agitator speed, stirring foaming 6min, obtains ceramics
Foamed slurry；
（5）Ceramic foam slurry is injected in mould rapidly, solidification 5min is stood, the demoulding, obtains foamed alumina ceramic idiosome；
Ceramic wet blank is placed in 50 DEG C of baking oven and dries 24h, natural cooling, idiosome is put into Muffle furnace, with 2 DEG C/min heating
Rate program is warming up to 900 DEG C, is incubated 40min, continue with 2 DEG C/min heating rate distinguish temperature programming to 1350 DEG C,
1400 DEG C, 1450 DEG C and 1500 DEG C, each temperature section is incubated 20-30min, and 500 DEG C are cooled to 5 DEG C/min rate of temperature fall,
Room temperature is naturally cooled to, a kind of particle stabilized foam process is obtained and prepares alumina ceramic supporting body.
The step of the present embodiment（2）Titanium and the mass ratio of aluminum oxide are 1 in middle titanium sulfate solution：250.
The step of the present embodiment（4）The environment of Muffle furnace high-temperature calcination be atmospheric atmosphere.
Claims (4)
1. a kind of particle stabilized foam process prepares alumina ceramic supporting body, it is characterised in that first by kaolin and oxidation
Zinc combination drying, wet ball grinding, drying, obtain mixed-powder；Then after mixing alumina powder and mixed-powder, with sulfuric acid
Titanium is presoma, and Membranes On Alumina Particles Surface is modified；The finally gel injection-moulding system using acrylamide as high polymer monomer,
Mechanical agitation foams, the solidification demoulding, dry and high temperature sintering, obtains particle stabilized foam process and prepares aluminium oxide ceramics support
Body.
2. the particle stabilized foam process according to claims 1 prepares alumina ceramic supporting body, it is characterised in that its
It is prepared by following steps：
（1）By kaolin, zinc oxide with 1：0.9-1.1 mass ratio mixing, is placed in 80-90 DEG C of vacuum drying chamber and dries 5-
6h, then through wet ball grinding, drying, pulverize and sieve to obtain the mixed-powder of 200-250 mesh, it is stand-by；
（2）By alumina powder and mixed-powder with 1：0.02-0.03 mass ratio is placed in reaction vessel, is added equivalent to oxygen
Change the deionized water of 15-20 times of aluminium micropowder weight part, ultrasonic vibration 50-60min, make its fully dispersed, sulphur is added dropwise while stirring
Sour titanium solution, magnetic agitation 30-40min, is then added dropwise ammoniacal liquor and adjusts the pH value of system to 9.5-10.5, continue magnetic at room temperature
Power stirs 2-3h, filtering, washing, dries, obtains surface modification alumina powder；
（3）By surface modification alumina powder, acrylic acid, acrylamide, N, N '-methylene-bisacrylamide, polyethylene glycol and
Deionized water is with 1：0.08-0.1：0.2-0.25：0.04-0.05：0.03-0.04：6-7 mass ratio mixing, is added to ball milling
In machine, drum's speed of rotation is ball milling mixing 4-5h under conditions of 600-800r/min；Add the fourth of 0.04-0.05 times of parts by weight
Acid, mix to uniformly, the pH value of regulation system under conditions of drum's speed of rotation is 300-400r/min, continues ball to 5-6
Mill mixing 2-3h, obtains ceramic slurry；
（4）Ceramic slurry is transferred in agitator, adds the ammonium persulfate and 0.004-0.005 of 0.008-0.01 times of parts by weight
The N, N, N of times parts by weight ', N '-tetramethylethylenediamine, starts to stir, and it is 250-300r/min to control agitator speed, stirring hair
5-8min is steeped, obtains ceramic foam slurry；
（5）Ceramic foam slurry is injected in mould rapidly, solidification 5-6min is stood, the demoulding, obtains foamed alumina ceramics embryo
Body；Ceramic wet blank is placed in 40-50 DEG C of baking oven and dries 20-24h, natural cooling, idiosome is put into Muffle furnace, with 2-3
DEG C/min heating rate temperature programming to 800-900 DEG C, be incubated 30-40min, continue with 2-3 DEG C/min heating rate point
Other temperature programming is to 1350 DEG C, 1400 DEG C, 1450 DEG C and 1500 DEG C, and each temperature section is incubated 20-30min, with 4-5 DEG C/min's
Rate of temperature fall is cooled to 500 DEG C, naturally cools to room temperature, obtains a kind of particle stabilized foam process and prepares aluminium oxide ceramics support
Body.
3. the particle stabilized foam process according to claims 2 prepares the preparation method of alumina ceramic supporting body, its
It is characterised by, step（2）Titanium and the mass ratio of aluminum oxide are 1 in middle titanium sulfate solution：200-250.
4. the particle stabilized foam process according to claims 2 prepares the preparation method of alumina ceramic supporting body, its
It is characterised by, step（4）The environment of Muffle furnace high-temperature calcination be atmospheric atmosphere.
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Cited By (5)
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| CN112661492A (en) * | 2019-10-16 | 2021-04-16 | 国家能源投资集团有限责任公司 | Composition for producing fly ash ceramic membrane, fly ash ceramic membrane and preparation method and application thereof |
| CN112661520A (en) * | 2019-10-16 | 2021-04-16 | 国家能源投资集团有限责任公司 | Fly ash-alumina composite ceramic membrane and preparation method and application 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 |
| WO2021073100A1 (en) * | 2019-10-18 | 2021-04-22 | 三达膜科技（厦门）有限公司 | Method for preparing high-strength ceramic filter membrane |
| CN113548871A (en) * | 2020-04-23 | 2021-10-26 | 国家能源投资集团有限责任公司 | Fly ash composition, raw material for producing fly ash ceramic membrane, preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661492A (en) * | 2019-10-16 | 2021-04-16 | 国家能源投资集团有限责任公司 | Composition for producing fly ash ceramic membrane, fly ash ceramic membrane and preparation method and application thereof |
| CN112661520A (en) * | 2019-10-16 | 2021-04-16 | 国家能源投资集团有限责任公司 | Fly ash-alumina composite ceramic membrane and preparation method and application 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 |
| WO2021073100A1 (en) * | 2019-10-18 | 2021-04-22 | 三达膜科技（厦门）有限公司 | Method for preparing high-strength ceramic filter membrane |
| CN113548871A (en) * | 2020-04-23 | 2021-10-26 | 国家能源投资集团有限责任公司 | Fly ash composition, raw material for producing fly ash ceramic membrane, preparation method and application thereof |
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Application publication date: 20171110 |
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