CN106747557A - The preparation method of plate diamond spar ceramic film support - Google Patents
The preparation method of plate diamond spar ceramic film support Download PDFInfo
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- CN106747557A CN106747557A CN201611055785.8A CN201611055785A CN106747557A CN 106747557 A CN106747557 A CN 106747557A CN 201611055785 A CN201611055785 A CN 201611055785A CN 106747557 A CN106747557 A CN 106747557A
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- diamond spar
- plate diamond
- ceramic film
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0038—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by superficial sintering or bonding of particulate matter
- C04B38/0041—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by superficial sintering or bonding of particulate matter the particulate matter having preselected particle sizes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The present invention relates to a kind of preparation method of plate diamond spar ceramic film support, belong to ceramic membrane technology field.The preparation method of plate diamond spar ceramic film support of the present invention, it is with alumina powder, promotees the plate diamond spar of agglutinant and pretreatment as raw material, pug is made after stirring, then by pug extrusion molding and sintering, described plate diamond spar ceramic film support is obtained；The pretreatment is that the particle surface of plate diamond spar is modified using surface modifier.The present invention is simple and easy to apply, and low cost, sintering temperature is low, energy-saving and emission-reduction.
Description
Technical field
The present invention relates to a kind of preparation method of plate diamond spar ceramic film support, belong to ceramic membrane technology field.
Background technology
Since the eighties in 20th century porous ceramic film first since French industrial application, its high score is from effect
Rate, high temperature resistant, solvent resistant, antimicrobial, resistance to acids and bases, high mechanical properties and the excellent properties such as easy cleaning is renewable are gradually by work
Industry receives and has been widely applied.Inorganic ceramic membrane can be used for gas separation, liquid isolation of purified and membrane reactor,
Food industry, pharmacy and bioengineering, chemistry and the field such as petrochemical industry and environmental protection are widely used.When
Before, the increasingly raising with world wide to process industrial energy-conserving and emission-cutting technology demand, the nanofiltration membrane with nanostructured,
Pervaporation membrane and gas separation membrane have turned into one of the study hotspot and following important developing direction in ceramic membrane field.
Porous ceramic film typically has three layers of unsymmetric structure, i.e., the top layer of centrifugation, transition zone and supporting layer by.
Must have enough mechanical strengths, permeance property higher, the smooth and preferable acid-proof alkaline in surface as supporting layer.Support
The quality of body performance directly affects the preparation of follow-up porous ceramic film.
The electro-corundum (10~80 μm of particle diameter) that current supporter is mainly by being surface-treated by shaping (is carried as aggregate
For permeance property) prepare, on the one hand, the electro-corundum bulky grain sintering activity being surface-treated by shaping is relatively low, and this just leads
Cause inorganic ceramic film support sintering temperature is higher, and for example its firing temperature of Japanese NGK company is 1700 DEG C, and U.S. Pall
Its firing temperature of company reaches 1800 DEG C；On the other hand, it is this by shaping be surface-treated electro-corundum price it is higher (>=
20000 yuan/ton), its accounting in inorganic ceramic film support formula is (mass percent reaches 70-85%) high.Therefore, make
It is high into inorganic ceramic membrane product price, have impact on the large scale application of the product.
Because plate diamond spar calcining heat is more lower slightly than electro-corundum temperature, with the presence of Minute pores rate, its particle is to water
Suction-operated makes the extremely difficult extrusion pug for being made function admirable of the material, and pug easily produces cracking etc. to lack in drying process
Fall into, although this allow for plate diamond spar price than current supporter commonly use by shaping be surface-treated electro-corundum valency
The low 60-70% of lattice, but the technology application of the material is there is no in the industry.
The content of the invention
It is an object of the invention to provide a kind of preparation method of plate diamond spar ceramic film support, its is simple and easy to apply, cost
Low, sintering temperature is low, energy-saving and emission-reduction.
The preparation method of plate diamond spar ceramic film support of the present invention, be with alumina powder, promote agglutinant and
The plate diamond spar of pretreatment is raw material, and pug is made after stirring, then by pug extrusion molding and sintering, obtains described tabular
Corundum ceramic film support；The pretreatment is that the particle surface of plate diamond spar is modified using surface modifier.
The surface modifier is hydraulic oil, machine oil or tung oil, and addition is the 2-7% of plate diamond spar powder quality.
The detailed process of the pretreatment is as follows：To surface modifier is persistently slowly added in plate diamond spar powder, fully
Stirring mixing, infiltration package status are in surface modifier by the particle surface of plate diamond spar.
The particle diameter of the plate diamond spar is 30-50 μm；The particle diameter of alumina powder is 0.5-1 μm.
In the raw material, the mass percent of the plate diamond spar of pretreatment is 70-85%, the quality percentage of alumina powder
Than being 13-25%, the mass percent for promoting agglutinant is 0.5-5%.
The rush agglutinant is magnesia, titanium oxide or lanthana.
After the stirring 1h, deionized water, organic bond and lubricant is added to be made pug.
The organic bond is polyvinyl alcohol, cellulose or dextrin；Lubricant is the one kind or two in glycerine or white oil
Kind.
The addition of the deionized water is the 5-20% of material quality；The addition of organic bond is material quality
1-10%；The addition of lubricant is the 1-10% of material quality.
During the extrusion molding, pug is extruded into the supporter of sheet, single tube and multichannel.
During the sintering, temperature is 1580-1620 DEG C, and heating rate is 0.5-3 DEG C/min, and soaking time is 1-3 hours.
The cost of raw material (>=20000 yuan/ton) high instant invention overcomes generally existing in industry, sintering temperature are high
(1650-1800 DEG C), the problems such as energy consumption is big, there is provided a kind of preparation method for preparing ceramic film support of low cost.
Using the plate diamond spar having stable high-temperature performance, its particle is the nearly spherical particle of 30-50 μm of diameter, particle to the present invention
Mobile performance and dispersive property are good in pug, therefore, have an opportunity to produce more contact point between particle and particle, in sintering
During, these contact points improve the power of solid-phase sintering, promote the formation of neck sintering, effectively reduce and burn till temperature
Degree.
The present invention carries out particle surface pretreatment to above plate diamond spar using surface modifier, modified by surface, gram
Taken the current material prepare supporter generally existing particle is loose, plasticity of slurry extreme difference, season cracking the problems such as so that
Supporter extrusion molding and blue or green base dry qualification rate and increase substantially.
Compared with prior art, the invention has the advantages that：
(1) present invention is prepared for a kind of low (the cost of material reduction of cost of material by the modified pretreatment in plate diamond spar surface
60-70%), high (pure water flux is 5- for sintering temperature low (1580-1620 DEG C), high mechanical strength (20-50MPa), permeance property
10m3·m-2·h-1·bar-1), the ceramic film support of fine corrosion resistance, its porosity be 30-40%, average hole
Footpath is 10 μm.
(2) preparation method is simple and easy to apply, beneficial to industrialized production.
(3) ceramic film support for preparing, for ceramic membrane series of products large-scale promotion at home, in the industry cost
Sustainable reduction, energy-saving and environmental improvement cost persistently reduce significant.
Specific embodiment
With reference to embodiment, the present invention is further illustrated, but it is not intended to limit implementation of the invention.
Embodiment 1
(1) hydraulic oil is persistently slowly added in plate diamond spar powder, is thoroughly mixed plate diamond spar to hydraulic oil
Grain surface penetration parcel.On the basis of plate diamond spar powder quality, the mass percent that it is added is 2% to hydraulic oil addition.
(2) by plate diamond spar 70%, alumina powder 25%, magnesia 3%, titanium oxide 2% mass ratio dispensing, plus
Enter batch mixer, stirring premix 1 hour.
(3) deionized water 10%, polyvinyl alcohol 1% and glycerine 5% is added to be made on the basis of the powder quality of step (2)
Pug, using the supporter of extruder shaping sheet, single tube and multichannel.
(4) it is supported body, 0.5 DEG C/min of heating rate, soaking time 1 hour in 1580 DEG C of high temperature sinterings.
(5) mechanical strength for measuring the supporter that plate diamond spar is prepared with three-point bending method is 29.8MPa, pure water flux
It is 7m3·m-2·h-1·bar-1, porosity is 34%, and average pore size is 10 μm.
Embodiment 2
(1) machine oil is persistently slowly added in plate diamond spar powder, is thoroughly mixed plate diamond spar particle table to machine oil
Face infiltration parcel.On the basis of plate diamond spar powder quality, the mass percent that it is added is 7% to machine oil addition.
(2) by plate diamond spar 85%, alumina powder 13%, lanthana 2% mass ratio dispensing, add batch mixer,
Stirring premix 1 hour.
(3) deionized water 20%, polyvinyl alcohol 10% and glycerine 1% is added to be made on the basis of step (2) powder quality
Pug, using the supporter of extruder shaping sheet, single tube and multichannel.
(4) it is supported body, 1 DEG C/min of heating rate, soaking time 2 hours in 1620 DEG C of high temperature sinterings.
(5) mechanical strength for measuring the supporter that plate diamond spar is prepared with three-point bending method is 31.5MPa, pure water flux
It is 10m3·m-2·h-1·bar-1, porosity is 38%, and average pore size is 10 μm.
Embodiment 3
(1) tung oil is persistently slowly added in plate diamond spar powder, is thoroughly mixed plate diamond spar particle table to tung oil
Face infiltration parcel.On the basis of plate diamond spar powder quality, the mass percent that it is added is 5% to tung oil addition.
(2) by plate diamond spar 80%, alumina powder 16%, magnesia 3%, lanthana 1% mass ratio dispensing, plus
Enter batch mixer, stirring premix 1 hour.
(3) deionized water 5%, cellulose 3%, glycerine 5% and white oil are added on the basis of the powder quality of step (2)
5% is made pug, using the supporter of extruder shaping sheet, single tube and multichannel.
(4) it is supported body, 0.5 DEG C/min of heating rate, soaking time 3 hours in 1610 DEG C of high temperature sinterings.
(5) mechanical strength for measuring the supporter that plate diamond spar is prepared with three-point bending method is 50MPa, and pure water flux is
5m3·m-2·h-1·bar-1, porosity is 30%, and average pore size is 10 μm.
Embodiment 4
(1) hydraulic oil is persistently slowly added in plate diamond spar powder, is thoroughly mixed plate diamond spar to hydraulic oil
Grain surface penetration parcel.On the basis of plate diamond spar powder quality, the mass percent that it is added is 3% to hydraulic oil addition.
(2) by plate diamond spar 78%, alumina powder 21.5%, magnesia 0.5% mass ratio dispensing, add batch mixing
Machine, stirring premix 1 hour.
(3) deionized water 8%, dextrin 4% and white oil 5% is added to be made pug on the basis of the powder quality of step (2),
Using the supporter of extruder shaping sheet, single tube and multichannel.
(4) it is supported body, 3 DEG C/min of heating rate, soaking time 1 hour in 1590 DEG C of high temperature sinterings.
(5) mechanical strength for measuring the supporter that plate diamond spar is prepared with three-point bending method is 20MPa, and pure water flux is
9m3·m-2·h-1·bar-1, porosity is 40%, and average pore size is 10 μm.
Embodiment 5
(1) tung oil is persistently slowly added in plate diamond spar powder, is thoroughly mixed plate diamond spar particle table to tung oil
Face infiltration parcel.On the basis of plate diamond spar powder quality, the mass percent that it is added is 6% to tung oil addition.
(2) by plate diamond spar 82%, alumina powder 15%, titanium oxide 2%, lanthana 1% mass ratio dispensing, plus
Enter batch mixer, stirring premix 1 hour.
(3) deionized water 11%, cellulose 3% and glycerine 3% is added to be made mud on the basis of the powder quality of step (2)
Material, using the supporter of extruder shaping sheet, single tube and multichannel.
(4) it is supported body, 2 DEG C/min of heating rate, soaking time 2 hours in 1600 DEG C of high temperature sinterings.
(5) mechanical strength for measuring the supporter that plate diamond spar is prepared with three-point bending method is 42MPa, and pure water flux is
7m3·m-2·h-1·bar-1, porosity is 36%, and average pore size is 10 μm.
Claims (10)
1. a kind of preparation method of plate diamond spar ceramic film support, it is characterised in that：With alumina powder, promote agglutinant and pre-
The plate diamond spar for the treatment of is raw material, and pug is made after stirring, then by pug extrusion molding and sintering, obtains described tabular firm
Beautiful ceramic film support；The pretreatment is that the particle surface of plate diamond spar is modified using surface modifier.
2. the preparation method of plate diamond spar ceramic film support according to claim 1, it is characterised in that：Surface modifier
It is hydraulic oil, machine oil or tung oil, addition is the 2-7% of plate diamond spar powder quality.
3. the preparation method of plate diamond spar ceramic film support according to claim 1, it is characterised in that：Plate diamond spar
Particle diameter is 30-50 μm；The particle diameter of alumina powder is 0.5-1 μm.
4. the preparation method of plate diamond spar ceramic film support according to claim 1, it is characterised in that：The raw material
In, the mass percent of the plate diamond spar of pretreatment is 70-85%, and the mass percent of alumina powder is 13-25%, promotees to burn
The mass percent for tying agent is 0.5-5%.
5. the preparation method of plate diamond spar ceramic film support according to claim 1, it is characterised in that：Promoting agglutinant is
One or more in magnesia, titanium oxide or lanthana.
6. the preparation method of plate diamond spar ceramic film support according to claim 1, it is characterised in that：After stirring 1h,
Deionized water, organic bond and lubricant is added to be made pug.
7. the preparation method of plate diamond spar ceramic film support according to claim 6, it is characterised in that：Organic bond
It is polyvinyl alcohol, cellulose or dextrin；Lubricant is one or two in glycerine or white oil.
8. the preparation method of plate diamond spar ceramic film support according to claim 6, it is characterised in that：Deionized water
Addition is the 5-20% of material quality；The addition of organic bond is the 1-10% of material quality；The addition of lubricant
It is the 1-10% of material quality.
9. the preparation method of plate diamond spar ceramic film support according to claim 1, it is characterised in that：Extrusion molding
When, pug is extruded into the supporter of sheet, single tube and multichannel.
10. the preparation method of plate diamond spar ceramic film support according to claim 1, it is characterised in that：During sintering, temperature
It is 1580-1620 DEG C to spend, and heating rate is 0.5-3 DEG C/min, and soaking time is 1-3 hours.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611055785.8A CN106747557A (en) | 2016-11-25 | 2016-11-25 | The preparation method of plate diamond spar ceramic film support |
| PCT/CN2017/111546 WO2018095277A1 (en) | 2016-11-25 | 2017-11-17 | Preparation method of plate-shaped corundum ceramic film support |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611055785.8A CN106747557A (en) | 2016-11-25 | 2016-11-25 | The preparation method of plate diamond spar ceramic film support |
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| CN106747557A true CN106747557A (en) | 2017-05-31 |
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| WO (1) | WO2018095277A1 (en) |
Cited By (1)
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| WO2018095277A1 (en) * | 2016-11-25 | 2018-05-31 | 山东硅元新型材料股份有限公司 | Preparation method of plate-shaped corundum ceramic film support |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109265148B (en) * | 2018-09-19 | 2023-10-24 | 洛阳科创新材料股份有限公司 | Preparation method of high-performance ceramic plate for air brick |
| CN112661520B (en) * | 2019-10-16 | 2023-07-14 | 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 |
| CN114249582B (en) * | 2020-09-25 | 2023-01-10 | 三达膜科技（厦门）有限公司 | Internal multi-runner disc type alumina ceramic membrane and preparation method thereof |
| CN114311232B (en) * | 2020-09-29 | 2023-02-10 | 三达膜科技（厦门）有限公司 | Preparation method of large-diameter combined honeycomb ceramic filter membrane |
| CN113648848B (en) * | 2021-08-05 | 2023-12-08 | 河北工业大学 | Hollow flat ceramic membrane and preparation method thereof |
| CN116477923B (en) * | 2023-03-22 | 2024-04-05 | 雅安沃克林环保科技有限公司 | Method for preparing ceramic connecting plate by utilizing ceramic membrane waste and ceramic connecting plate |
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| CN106747557A (en) * | 2016-11-25 | 2017-05-31 | 山东硅元新型材料有限责任公司 | The preparation method of plate diamond spar ceramic film support |
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2016
- 2016-11-25 CN CN201611055785.8A patent/CN106747557A/en active Pending
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2017
- 2017-11-17 WO PCT/CN2017/111546 patent/WO2018095277A1/en active Application Filing
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| CN103755328A (en) * | 2014-02-07 | 2014-04-30 | 刘旭红 | Preparation method of tubular ceramic membrane support body |
| CN105254323A (en) * | 2015-11-28 | 2016-01-20 | 郑州大学 | Micropore alumina and mullite ceramic separation film supporting body and preparation method thereof |
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| WO2018095277A1 (en) * | 2016-11-25 | 2018-05-31 | 山东硅元新型材料股份有限公司 | Preparation method of plate-shaped corundum ceramic film support |
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