CN104291759B - The preparation method that a kind of ceramic fibre strengthens high temperature insulation warming plate - Google Patents
The preparation method that a kind of ceramic fibre strengthens high temperature insulation warming plate Download PDFInfo
- Publication number
- CN104291759B CN104291759B CN201410496821.9A CN201410496821A CN104291759B CN 104291759 B CN104291759 B CN 104291759B CN 201410496821 A CN201410496821 A CN 201410496821A CN 104291759 B CN104291759 B CN 104291759B
- Authority
- CN
- China
- Prior art keywords
- ceramic fibre
- warming plate
- atmosphere
- add
- room temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Thermal Insulation (AREA)
Abstract
The present invention relates to a kind of method preparing high intensity, high-fire resistance thermal insulating plate by ceramic fibre and aluminous cement composite solidification molding then high temperature sintering.Take ultra-fine aluminous cement, add water, add carbon dust again or pyrolysis can generate the presoma of carbon dust, and add porcelain hollow bead, stir into slurry；The long ceramic fibre of layer overlay, note last layer slurry in mould；Repeatedly spread fiber, grout material, until meeting the thickness of design, at room temperature standing after one day the demoulding and drying, obtaining the green compact of high intensity, then divide three step atmosphere sinterings: the first step rises to about 270 DEG C in oxidizing atmosphere from room temperature；Second step rises to about 1000 DEG C at reducing atmosphere or inert atmosphere, is hereafter slowly decreased to about 800 DEG C；3rd step is at oxidizing atmosphere and about 800 DEG C insulation 1-3h.The warming plate intensity that prepared warming plate is more close than cost prepared by original technology is high, unit weight is low, thermal conductivity is low, good heat insulating.
Description
Technical field
The present invention relates to technical field of composite preparation.Specifically, a kind of method preparing high intensity, high-fire resistance thermal insulating plate by ceramic fibre and aluminous cement composite solidification molding then high temperature sintering is related to.
Background technology
High temperature insulation warming plate is high due to heat stability, and heat conductivity is low, is widely used in various high temperature occasion, including the continuous pallettype sintering machine of metallurgy industry, heat-treatment furnace, aluminium cell, pottery, building material calcining kiln, and various petrochemical industry heating furnaces etc..Such as certain Chinalco requires regulation for the technology of aluminium cell outer wall warming plate: specific insulation >=1.0 × 1012 Ω cm, indeformable at 600 DEG C of continuous 120h, do not ftracture.Even if adopting the most resistant to elevated temperatures organic resin such as organic siliconresin or organic fluorine, the requirement of high temperature resistant 600 DEG C also can not be met far away.Therefore the warming plate being almost made up of completely can only be adopted inorganic matter.
Application number is the patent document proposition of 201010150495.8, by mud, slag, the broken mixing and ball milling of expansion component, then alumina short fibre is added and mixture continues stirring, mist projection granulating, the pug of old mistake is loaded in mould and fires, generate the light fibre containing uniform closed porosity and strengthen ceramic thermal insulation material.This type of method can only use chopped fiber, and therefore prepared warming plate tensile strength is very low.
Application number is the Chinese patent application processing method that proposes calcium silicate substrate warming plate of 201310201984.5, the stirring that silica flour, Calx, fortifying fibre, inorganic filling material added water is modulated into slurry, slurry is poured in grinding tool, roll-in leveling under stress, get rid of moisture and be placed in pressure vessel, at saturated vapor pressure, molding after maintenance 5-15 hour at 120-200 DEG C.This type of material internal is mainly with afwillite for bonding agent, and at high temperature afwillite sloughs hydrone, and material internal structure is destroyed, so this type of material is difficult to meet the requirement of high temperature resistant 600 DEG C.
Application number is the Chinese patent application preparation method that proposes glass fiber reinforcement waterglass base silicon dioxide composite aerogel insulation material of 201310343119.4: mixed with water glass solution and water by methyl TMOS, make methyl TMOS be hydrolyzed in water and obtain solution A, add strongly acidic styrene's resin and carry out ion exchange, then sucking filtration obtains the solution of pH=2-3, glass fibre after heat treatment is added the solution that sucking filtration obtains, adding ammonia adjustment pH value is 8-8.5, obtain the silicon dioxide gel of fiber composite, it is then transferred in container and stands, obtain the silica hydrogel of compound, it is then immersed in ethanol solution and carries out the aging of gel and alcoholization, again the wet gel of gained after alcoholization is immersed in trim,ethylchlorosilane, in the mixed solution of dehydrated alcohol and normal hexane, carry out surface modification.Obviously, the cost of material of this preparation method and process costs are all significantly high.
Summary of the invention
Deficiency for existing high intensity, high-fire resistance thermal insulating plate technology of preparing, the present invention proposes following solution: is substrate with calcium aluminate, strengthens with pottery long fibre, add carbon dust or the presoma of carbon dust can be generated as pore creating material in pyrolysis under nonoxidizing atmosphere, and adding porcelain hollow bead.Preparation method is: first aluminous cement is carried out super-fine processing, adds water, adds carbon dust or can generate the presoma of carbon dust in pyrolysis under nonoxidizing atmosphere, and add porcelain hollow bead, stirs into slurry；The long ceramic fibre of layer overlay, note last layer slurry in mould；Repeatedly spread fiber, grout material, until meeting the thickness of design, at room temperature standing and waiting that aluminous cement completes the reaction of hydrated adhesive cure；Then the demoulding drying, obtain the green compact of high intensity, last point three step atmosphere sinterings in high temperature furnace: the first step is thoroughly got rid of the water entrainment in base substrate, absorption water in oxidizing atmosphere, second step makes calcium aluminate hydrates become anhydrous calcium aluminate and progressively sinter under reducing atmosphere or inert atmosphere, organic precursor becomes carbon simultaneously, oxidation of coal is volatilized by the 3rd step under oxidizing atmosphere, thus preparing high intensity, high-fire resistance thermal insulating plate.
Detailed description of the invention
First with super-fine processing machinery such as ball mill or jet mill etc., aluminous cement is carried out super-fine processing, make the ultra-fine aluminous cement of median 0.4-1.8 μm, add water, add carbon dust or the presoma of carbon dust can be generated in pyrolysis under nonoxidizing atmosphere, and add porcelain hollow bead, stir into slurry under room temperature；Often add 100g aluminous cement correspondence and add 80-270g water, 10-90g carbon dust or presoma, 10-100g porcelain hollow bead, 70-200g ceramic fibre；The long ceramic fibre of layer overlay, note last layer slurry in mould；Repeatedly spread fiber, grout material, until meeting the thickness of design, at room temperature standing and waiting that aluminous cement completes the reaction of hydrated adhesive cure；Room temperature demoulding after 1 day, then room temperature maintenance 2 days, then carry out three step atmosphere sinterings: the first step rises to about 270 DEG C from room temperature 2-12h under oxidizing atmosphere；Second step rises to about 600 DEG C with 3-17h under reducing atmosphere or inert atmosphere, about 1000 DEG C are risen to again with 2-12h, hereafter it is reduced to about 800 DEG C with 1-2h from about 1000 DEG C, during this, calcium aluminate hydrates becomes anhydrous calcium aluminate and steps up sintering degree, and organic precursor becomes carbon simultaneously；3rd step, at oxidizing atmosphere and about 800 DEG C insulation 1-3h, is brought down below about 200 DEG C with stove and takes out sample.
Described carbon dust, including coal dust, coke blacking, activated carbon powder, white carbon black.The particle diameter of carbon dust is desirably no more than 60 μm.
Described pyrolysis can generate the presoma of carbon dust and include: powder of straw, wood powder, mushroom bran, starch, furfural dregs, waste plastics powder, waste Crumb rubber, asphalt powder；The particle diameter of presoma powder is desirably no more than 120 μm.
Described long ceramic fibre includes: aluminium oxide long fibre, aluminium oxide-zirconium oxide composite long fiber, mullite long fibre, aluminium silicate long fibre, basalt long fiber, fibre length is not less than 50mm；According to ceramic fiber cloth, then forming process is easier to lay in mould.
Described porcelain hollow bead includes: alumina hollow ball, devitrified glass hollow ball, fly ash float, expanded perlite, expanded vermiculite；Its particle diameter should be not more than 2mm.
Below embodiments of the present invention are illustrated:
Embodiment 1
Take the ultra-fine aluminous cement 1kg of median 1.5 μm, add 1.2kg water, 0.3kg crosses 300 mesh standard sieves (particle diameter is not more than 45 μm) coal dust, and add 0.5kg expanded vermiculite, under room temperature, stir into slurry；Taking alumina fibre cloth and be cut into every 200mmX200mm, the quality of every is about 9.7g；It is of a size of in the mould of 200mmX200mmX70mm to inner chamber to spread a piece of alumina fibre cloth, note 130g slurry and paints brush handle slurry and shakeout；Repeatedly spreading fiber cloth, grout material, until gross thickness is 10mm, slip casting 12 times, spreads 13 layers of fiber cloth altogether.At room temperature stand and wait that aluminous cement completes the reaction of hydrated adhesive cure；Room temperature demoulding after 1 day, then room temperature maintenance 2 days, adopt three step atmosphere sinterings: the first step rises to 270 DEG C from room temperature 8h under air atmosphere (oxidizing atmosphere) in controlled atmosphere resistance furnace；Second step rises to 600 DEG C with 10h in a nitrogen atmosphere, hereafter rises to 1000 DEG C with 6h, then is down to 800 DEG C with 1h；3rd step is incubated 3h at air atmosphere and 800 DEG C, is brought down below 200 DEG C with stove and takes out sample.
Warming plate tensile strength prepared above is 143MPa, specific insulation 1.36 × 1012Ω cm, unit weight (apparent density) is 0.52g/cm3, heat conductivity is 0.091W m-1·℃-1。
Comparative example 1
Green compact are prepared by the dispensing of embodiment 1, forming method, put into the high-temperature electric resistance furnace of controlled atmosphere, adopt the intensification temperature control program identical with embodiment 1, simply take air atmosphere therebetween always, prepared warming plate tensile strength is 107MPa, specific insulation 1.15 × 1012Ω cm, unit weight is 0.88g/cm3, heat conductivity is 0.134W m-1·℃-1。
As can be seen here, for dispensing and the moulding process of the present invention, do not adopt three step atmosphere sintering methods cannot prepare into heat conductivity lower than 0.1W m-1·℃-1Warming plate.
Embodiment 2
Take the ultra-fine aluminous cement 1kg of median 1.16 μm, add 1.8kg water, 0.3kg crosses 200 mesh standard sieves (particle diameter is not more than 75 μm) mushroom bran becomes carbon matrix precursor as pyrolysis, and add 0.5kg fly ash float, under room temperature, stir into slurry；Taking basalt fiber cloth and be cut into every 200mmX200mm, the quality of every is about 8.2g；It is of a size of in the mould of 200mmX200mmX70mm to inner chamber to spread a piece of basalt fiber cloth, note 110g slurry and paints brush handle slurry and shakeout；Repeatedly spreading fiber cloth, grout material, until gross thickness is 10mm, slip casting 15 times, spreads 16 layers of fiber cloth altogether.At room temperature standing demoulding after 1 day, then room temperature maintenance 2 days, is then adopting three step atmosphere sinterings with natural gas for the shuttle kiln of fuel: it is 1.12(oxidizing atmosphere that the first step controls coefficient of excess air) rise to 270 DEG C from room temperature 5h；It is 0.97(weakly reducing atmosphere that second step controls coefficient of excess air) rise to 630 DEG C with 10h, hereafter rise to 1000 DEG C with 6h, then be down to 800 DEG C with 1.5h；It is 1.11(weak oxide atmosphere that 3rd step controls coefficient of excess air), insulation 3h at 800 DEG C, be brought down below 200 DEG C with stove and take out samples.
Warming plate tensile strength prepared above is 106MPa, specific insulation 1.09 × 1012Ω cm, unit weight (apparent density) is 0.56g/cm3, heat conductivity is 0.095W m-1·℃-1。
Embodiment 3
Take the ultra-fine aluminous cement 1kg of median 1.32 μm, add 1.6kg water, 0.37kg crosses 200 mesh standard sieves (particle diameter is not more than 75 μm) furfural dregs becomes carbon matrix precursor as pyrolysis, and add 0.43kg expanded perlite, under room temperature, stir into slurry；Take mullite fiber cloth and be cut into every 200mmX200mm；It is of a size of in the mould of 200mmX200mmX70mm to inner chamber and spreads a piece of mullite fiber cloth, note 120g slurry and paint brush handle slurry and shakeout；Repeatedly spreading fiber cloth, grout material, until gross thickness is 10mm, slip casting 15 times, spreads 16 layers of fiber cloth altogether.At room temperature standing demoulding after 1 day, then room temperature maintenance 2 days, is then adopting three step atmosphere sinterings with natural gas for the shuttle kiln of fuel: it is 1.13(oxidizing atmosphere that the first step controls coefficient of excess air) rise to 270 DEG C from room temperature 12h；It is 0.98(weakly reducing atmosphere that second step controls coefficient of excess air) rise to 630 DEG C with 8h, hereafter rise to 1000 DEG C with 5h, then be down to 800 DEG C with 2h；It is 1.12(weak oxide atmosphere that 3rd step controls coefficient of excess air), insulation 3h at 800 DEG C, be brought down below 200 DEG C with stove and take out samples.
Warming plate tensile strength prepared above is 115MPa, specific insulation 1.26 × 1012Ω cm, unit weight (apparent density) is 0.59g/cm3, heat conductivity is 0.097W m-1·℃-1。
Warming plate prepared by above-described embodiment, the cost of its every kilogram goods is about 10$, and the warming plate intensity more close than cost prepared by original technology is high, unit weight is low, thermal conductivity is low, good heat insulating.These embodiments are for the explanation to claim, but are not intended to limitations on the claims, and protection scope of the present invention should be as the criterion with claims.
Claims (5)
1. the preparation method that a ceramic fibre strengthens high temperature insulation warming plate, it is characterized in that: take median at the ultra-fine aluminous cement of 0.4-1.8 μm, add water, then add carbon dust or can pyrolysis generate carbon dust presoma, and add porcelain hollow bead, stir into slurry under room temperature；Often add 100g aluminous cement correspondence and add 80-270g water, 10-90g carbon dust or presoma, 10-100g porcelain hollow bead, 20-100g ceramic fibre；The long ceramic fibre of layer overlay, note last layer slurry in mould；Repeatedly spread fiber, grout material, until meeting the thickness of design, at room temperature standing demoulding after 1 day, then room temperature maintenance 2 days, then carry out three step atmosphere sinterings: the first step rises to 270 DEG C from room temperature 2-12h under oxidizing atmosphere；Second step rises to 600 DEG C with 3-17h under reducing atmosphere or inert atmosphere, 1000 DEG C are risen to again with 2-12h, hereafter being reduced to 800 DEG C with 1-2h from 1000 DEG C, during this, calcium aluminate hydrates becomes anhydrous calcium aluminate and steps up sintering degree, and organic precursor becomes carbon simultaneously；3rd step, at oxidizing atmosphere and 800 DEG C of insulation 1-3h, is brought down below 200 DEG C with stove and takes out sample.
2. the preparation method that ceramic fibre strengthens high temperature insulation warming plate according to claim 1, it is characterised in that: described carbon dust, including coal dust, coke blacking, activated carbon powder, white carbon black；Its particle diameter is not more than 60 μm.
3. the preparation method that ceramic fibre strengthens high temperature insulation warming plate according to claim 1, it is characterised in that: described pyrolysis can generate the presoma of carbon dust and include: powder of straw, wood powder, mushroom bran, starch, furfural dregs, waste plastics powder, waste Crumb rubber, asphalt powder；The particle diameter of presoma powder is not more than 120 μm.
4. the preparation method that ceramic fibre strengthens high temperature insulation warming plate according to claim 1, it is characterized in that: described long ceramic fibre includes: aluminium oxide long fibre and fiber cloth, aluminium oxide-zirconium oxide composite long fiber and fiber cloth, mullite long fibre and fiber cloth, aluminium silicate long fibre and fiber cloth, basalt long fiber and fiber cloth thereof, fibre length is not less than 50mm.
5. the preparation method that ceramic fibre strengthens high temperature insulation warming plate according to claim 1, it is characterised in that: described porcelain hollow bead includes: alumina hollow ball, devitrified glass hollow ball, fly ash float, expanded perlite, expanded vermiculite；Its particle diameter is not more than 2mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410496821.9A CN104291759B (en) | 2014-09-25 | 2014-09-25 | The preparation method that a kind of ceramic fibre strengthens high temperature insulation warming plate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410496821.9A CN104291759B (en) | 2014-09-25 | 2014-09-25 | The preparation method that a kind of ceramic fibre strengthens high temperature insulation warming plate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104291759A CN104291759A (en) | 2015-01-21 |
| CN104291759B true CN104291759B (en) | 2016-06-29 |
Family
ID=52311752
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410496821.9A Expired - Fee Related CN104291759B (en) | 2014-09-25 | 2014-09-25 | The preparation method that a kind of ceramic fibre strengthens high temperature insulation warming plate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104291759B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102015223443A1 (en) * | 2015-11-26 | 2017-06-01 | Robert Bosch Gmbh | Electric device with a wrapping compound |
| CN106284710B (en) * | 2016-07-29 | 2019-06-21 | 上海轩颂建筑科技有限公司 | A kind of silicate external-wall heat-insulation material |
| CN108358661A (en) * | 2017-07-01 | 2018-08-03 | 太仓安托建筑材料有限公司 | A kind of light-weight environment-friendly construction material |
| CN108484191A (en) * | 2018-04-12 | 2018-09-04 | 辽宁罕王绿色建材有限公司 | A kind of production technology of foamed ceramic partition plate activeness and quietness |
| CN108383535A (en) * | 2018-04-20 | 2018-08-10 | 钱万琦 | A kind of preparation method of light flyash refratory insulating brick |
| CN112876225B (en) * | 2021-02-08 | 2023-08-01 | 新疆硅质耐火材料有限公司 | Sintered high-temperature-resistant light heat insulation material and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH596109A5 (en) * | 1975-01-15 | 1978-02-28 | Activite Atom Avance | |
| US4442219A (en) * | 1981-10-19 | 1984-04-10 | Kennecott Corporation | Two part castable ceramic cement |
| JP3094149B2 (en) * | 1996-03-29 | 2000-10-03 | 長野県 | Manufacturing method of lightweight refractory |
| CN101659559B (en) * | 2009-08-07 | 2012-04-11 | 通达耐火技术股份有限公司 | 600kg-class energy-saving heat insulation lining material and preparation method thereof |
| CN103496957A (en) * | 2013-09-18 | 2014-01-08 | 韦仲华 | Light porous tourmaline composite ceramic and preparation method thereof |
-
2014
- 2014-09-25 CN CN201410496821.9A patent/CN104291759B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN104291759A (en) | 2015-01-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104291759B (en) | The preparation method that a kind of ceramic fibre strengthens high temperature insulation warming plate | |
| CN102059736B (en) | Method for producing insulating bricks by utilizing aluminum-electrolyzed waste refractory materials | |
| CN108585922B (en) | Aerogel ceramic fiber heat-insulating plate and preparation method thereof | |
| CN104003755B (en) | A kind of technique of utilizing polishing slag preparation to breathe brick | |
| CN105884394A (en) | Method for preparing porous silicon carbide support body at low temperature | |
| CN110092641A (en) | Half red mud permeable brick of one kind and preparation method thereof | |
| CN106518043B (en) | The preparation method of the siliceous bottom brick of molten tin bath of low-cost aluminum calcium | |
| CN107973619A (en) | Mullite-anorthite-corundum complex phase micropore heat-barrier material and preparation method thereof | |
| CN110655379A (en) | Nano composite heat insulation plate and preparation method thereof | |
| CN110002845A (en) | A kind of corundum-mullite insulating brick and preparation method thereof | |
| CN101786844A (en) | Light heat-preserving brick and fabrication method thereof | |
| CN109734388A (en) | A kind of mortar and its preparation method and application | |
| CN106431434B (en) | A kind of obturator-type alumina base mullite material and preparation method thereof | |
| CN106431458B (en) | The method that tailings in vanadium extraction prepares porous ceramics | |
| CN108017397A (en) | Refractory brick containing quartz sand and preparation method thereof | |
| CN108484127A (en) | A kind of highiy refractory brick and preparation method | |
| CN108314464A (en) | Method for preparing foam glass-aerogel heat insulation material | |
| CN112759363A (en) | Foamed ceramic composite additive, foamed ceramic and preparation method thereof | |
| KR20110125913A (en) | Bricks for interior containing stone sludge and methods for preparing thereof | |
| CN110498688A (en) | A kind of structural ceramics enhancing high silicon oxygen Aluminum sol powder and preparation method thereof | |
| CN108002851A (en) | Refractory brick containing mullite and preparation method thereof | |
| KR20050076271A (en) | An incombustible construction mineral material having coating surface, and the manufacturing method | |
| CN106396700A (en) | Production method of corundum composite polycrystalline mullite fiber light bricks | |
| CN106280658A (en) | A kind of insulation putty for architectural exterior wall | |
| CN108285350A (en) | A kind of tri compound SiC based refractories and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160629 Termination date: 20170925 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |