CN109437866A - A kind of corundum-mullite matter heat-barrier material and preparation method thereof - Google Patents
A kind of corundum-mullite matter heat-barrier material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of corundum-mullite matter heat-barrier materials and preparation method thereof.Its technical solution is: corundum fine powder, bauxite fine powder, aluminium hydroxide, quartz sand fine powder, ammonium metavanadate and thermosetting phenolic resin are uniformly mixed, compression moulding, it is heat-treated 3~5 hours under the conditions of neutral atmosphere and 900~1200 DEG C, through broken, ball milling and screening, ball milling material and particulate material are obtained.The ball milling material, the corundum fine powder, the bauxite fine powder, ferro-silicon nitride, hydroxyethyl cellulose and water are mixed again, ball milling obtains slurry.Then the particulate material, the corundum fine powder, the ball milling material, the slurry are uniformly mixed, compression moulding, it is dry, 3~5 hours are kept the temperature under the conditions of 1400~1600 DEG C, obtains corundum-mullite matter heat-barrier material.Raw material sources of the present invention are extensively and production cost is low, and prepared corundum-mullite matter heat-barrier material has the characteristics that bulk density is low, intensity is high, heat-proof quality is excellent.
Description
Technical field
The invention belongs to heat-barrier material technical fields.More particularly to a kind of corundum-mullite matter heat-barrier material and its preparation
Method.
Background technique
The military service performance of heat-barrier material, it is most important for the energy-saving of hot industry and safety in production, with high temperature
Industrial expansion, high-strength, micropore and the low performances such as thermally conductive have become the important directions of heat-barrier material research and development.With corundum and not
Carry out the corundum-mullite matter heat-barrier material that stone is principal crystalline phase, with high temperature resistance is good, thermal conductivity is low, thermal shock resistance is excellent
The different advantages such as low with thermal expansion coefficient, are used widely in the Thermal Equipments such as Industrial Stoves and high-temperature electric resistance furnace.
In the technology of preparing of existing corundum-mullite matter heat-barrier material, organic/inorganic foaming agent is usually introduced, burns and loses
Agent, or have the disadvantage in that is (1) introduced has though realizing the exploitation and production of heat-barrier material using characteristics such as salt decomposition
Machine additive, binder or bonding agent, charing under high temperature are decomposed, and are produced thick smoke and irritative gas, and environment is polluted；(2) introduce
Part material or additive fusing point it is lower, the low melting point liquid phase of generation exacerbates the contraction of material, reduces the use of product
Service life；(3) intensity is smaller, after the effects of external stress, mechanical oscillation, easily deforms, crackle, influences to keep the temperature liner body structure
Stability, reduction heat insulation effect.
Summary of the invention
The present invention is directed to overcome defect of the existing technology, it is therefore an objective to provide a kind of raw material sources extensively and production cost
Low corundum-mullite matter heat-barrier material, with this method prepare corundum-mullite matter heat-barrier material bulk density is low, intensity
High and heat-proof quality is excellent.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that:
The first step, by the corundum fine powder of 10~20wt%, the bauxite fine powder of 10~20wt%, 10~20wt% hydrogen-oxygen
The thermosetting phenolic resin for changing aluminium, the quartz sand fine powder of 20~40wt%, the ammonium metavanadate of 1~10wt% and 1~10wt% is mixed
It closes uniformly, then compression moulding under the conditions of 50~80MPa is heat-treated 3~5 under the conditions of neutral atmosphere and 900~1200 DEG C
Hour, then through broken, ball milling and screening, ball milling material of the granularity less than 0.088mm and granularity are obtained as of 0.088~0.5mm
Pellet.
Second step, by the ball milling material of 20~40wt%, the corundum fine powder of 10~30wt%, 1~10wt%
The bauxite fine powder, the ferro-silicon nitride of 1~10wt%, the water of the hydroxyethyl cellulose of 0.1~1wt% and 40~60wt% are mixed
It closes, ball milling obtains slurry.
Third step, by the particulate material of 60~80wt%, the corundum fine powder of 1~10wt%, 10~20wt%
The ball milling material, the slurry of 1~10wt% are uniformly mixed, then compression moulding under the conditions of 50~80MPa will be pressed into
The green body of type is 12~24 hours dry under the conditions of 80~110 DEG C, then keeps the temperature 3~5 hours under the conditions of being placed in 1400~1600 DEG C,
Obtain corundum-mullite matter heat-barrier material.
The corundum is plate diamond spar or is white fused alumina, Al in the corundum2O3Content be greater than 99wt%, the corundum
The granularity of fine powder is less than 0.088mm.
Al in the bauxite2O3Content be greater than 60wt%, the granularity of bauxite fine powder is less than 0.088mm.
Al (OH) in the aluminium hydroxide3Content be greater than 99wt%, granularity be less than 0.045mm.
SiO in the quartz sand2Content be greater than 98wt%, the granularity of quartz sand fine powder is less than 0.088mm.
The purity of the ammonium metavanadate is greater than 99wt%.
For the viscosity at ambient temperature of the thermosetting phenolic resin less than 10000 centipoises, the moisture content of thermosetting phenolic resin is small
In 15wt%.
The neutral atmosphere is nitrogen atmosphere or is argon atmosphere.
The content of Fe is 10-15wt% in the ferro-silicon nitride, and the granularity of ferro-silicon nitride is less than 0.088mm.
Ash content in the hydroxyethyl cellulose is less than 5wt%.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art:
(1) raw material sources of the present invention are extensive, and production cost is low.
(2) present invention is reasonably combined by different material, prefabricated ball milling material and particle with multistage pore-size distribution
Material, then by prefabricated slurry, different types of particle and powder are combined, then during the high temperature treatment process by not
Carry out being formed in situ for stone crystal whisker, further have adjusted the hole state in article construction, make prepared corundum-mullite matter every
Hot material not only has compared with low bulk density, and has lower thermal coefficient.
(3) preparation method is carried out substep control and effectively controls the hole of product in conjunction with stringent grain composition by the present invention
The intertexture distribution of gauge structure and mullite crystal whisker keeps prepared corundum-mullite matter heat-barrier material with higher strong
Degree.
Corundum-mullite matter heat-barrier material prepared by the present invention is through detecting: bulk density is less than 1.5g/cm3；Room temperature pressure resistance
Intensity is greater than 4MPa；Thermal coefficient is less than 0.25W/ (mK) within the scope of 200-1200 DEG C.
Therefore, raw material sources of the present invention are extensively and production cost is low, and prepared corundum-mullite matter heat-barrier material has
The features such as bulk density is low, intensity is high, heat-proof quality is excellent.
Specific embodiment
The invention will be further described With reference to embodiment, not to the limitation of its protection scope.
It is first that raw material Unify legislation involved in present embodiment is as follows to avoid repeating, it is no longer superfluous in embodiment
It states:
Al in the corundum2O3Content be greater than 99wt%, the granularity of the corundum fine powder is less than 0.088mm.
Al in the bauxite2O3Content be greater than 60wt%, the granularity of bauxite fine powder is less than 0.088mm.
Al (OH) in the aluminium hydroxide3Content be greater than 99wt%, granularity be less than 0.045mm.
SiO in the quartz sand2Content be greater than 98wt%, the granularity of quartz sand fine powder is less than 0.088mm.
The purity of the ammonium metavanadate is greater than 99wt%.
For the viscosity at ambient temperature of the thermosetting phenolic resin less than 10000 centipoises, the moisture content of thermosetting phenolic resin is small
In 15wt%.
The content of Fe is 10-15wt% in the ferro-silicon nitride, and the granularity of ferro-silicon nitride is less than 0.088mm.
Ash content in the hydroxyethyl cellulose is less than 5wt%.
Embodiment 1
A kind of corundum-mullite matter heat-barrier material and preparation method thereof.It is the step of preparation method described in the present embodiment:
The first step, by the corundum fine powder of 10~15wt%, the bauxite fine powder of 15~20wt%, 10~15wt% hydrogen-oxygen
The thermosetting phenolic resin for changing aluminium, the quartz sand fine powder of 30~40wt%, the ammonium metavanadate of 5~10wt% and 5~10wt% is mixed
It closes uniformly, then compression moulding under the conditions of 50~70MPa is heat-treated 3~5 under the conditions of neutral atmosphere and 1000~1200 DEG C
Hour, then through broken, ball milling and screening, ball milling material of the granularity less than 0.088mm and granularity are obtained as of 0.088~0.5mm
Pellet.
Second step, by the ball milling material of 20~30wt%, the corundum fine powder of 10~20wt%, 5~10wt%
The bauxite fine powder, the ferro-silicon nitride of 1~5wt%, the hydroxyethyl cellulose of 0.1~0.5wt% and 50~60wt% water
Mixing, ball milling obtain slurry.
Third step, by the particulate material of 60~70wt%, the corundum fine powder of 5~10wt%, 15~20wt%
The ball milling material, the slurry of 5~10wt% are uniformly mixed, then compression moulding under the conditions of 50~70MPa will be pressed into
The green body of type is 12~18 hours dry under the conditions of 80~100 DEG C, then keeps the temperature 3~5 hours under the conditions of being placed in 1500~1600 DEG C,
Obtain corundum-mullite matter heat-barrier material.
In the present embodiment: the corundum is plate diamond spar；The neutral atmosphere is nitrogen atmosphere.
Embodiment 2
A kind of corundum-mullite matter heat-barrier material and preparation method thereof.It is the step of preparation method described in the present embodiment:
The first step, by the corundum fine powder of 15~20wt%, the bauxite fine powder of 10~15wt%, 15~20wt% hydrogen-oxygen
The thermosetting phenolic resin for changing aluminium, the quartz sand fine powder of 25~35wt%, the ammonium metavanadate of 5~10wt% and 5~10wt% is mixed
It closes uniformly, then compression moulding under the conditions of 60~80MPa is heat-treated 3~5 under the conditions of neutral atmosphere and 900~1100 DEG C
Hour, then through broken, ball milling and screening, ball milling material of the granularity less than 0.088mm and granularity are obtained as of 0.088~0.5mm
Pellet.
Second step, by the ball milling material of 30~40wt%, the corundum fine powder of 12~25wt%, 1~5wt% institute
The water mixing of bauxite fine powder, the ferro-silicon nitride of 1~5wt%, the hydroxyethyl cellulose of 0.5~1wt% and 40~50wt% are stated,
Ball milling obtains slurry.
Third step, by the particulate material of 70~80wt%, the corundum fine powder of 5~10wt%, 10~15wt%
The ball milling material, the slurry of 1~5wt% are uniformly mixed, then compression moulding under the conditions of 60~80MPa will be pressed into
The green body of type is 18~24 hours dry under the conditions of 90~110 DEG C, then keeps the temperature 3~5 hours under the conditions of being placed in 1400~1500 DEG C,
Obtain corundum-mullite matter heat-barrier material.
In the present embodiment: the corundum is plate diamond spar；The neutral atmosphere is argon atmosphere.
Embodiment 3
A kind of corundum-mullite matter heat-barrier material and preparation method thereof.It is the step of preparation method described in the present embodiment:
The first step, by the corundum fine powder of 15~20wt%, the bauxite fine powder of 15~20wt%, 15~20wt% hydrogen-oxygen
The thermosetting phenolic resin for changing aluminium, the quartz sand fine powder of 20~30wt%, the ammonium metavanadate of 5~10wt% and 5~10wt% is mixed
It closes uniformly, then compression moulding under the conditions of 50~70MPa is heat-treated 3~5 under the conditions of neutral atmosphere and 1000~1200 DEG C
Hour, then through broken, ball milling and screening, ball milling material of the granularity less than 0.088mm and granularity are obtained as of 0.088~0.5mm
Pellet.
Second step, by the ball milling material of 20~30wt%, the corundum fine powder of 20~30wt%, 1~5wt% institute
The water for stating bauxite fine powder, the ferro-silicon nitride of 5~10wt%, the hydroxyethyl cellulose of 0.5~1wt% and 40~50wt% is mixed
It closes, ball milling obtains slurry.
Third step, by the particulate material of 65~75wt%, the corundum fine powder of 1~5wt%, 15~20wt% institute
State ball milling material, the slurry of 5~10wt% is uniformly mixed, compression moulding under the conditions of 50~70MPa, then by compression moulding
Green body dry 12~18 hours under the conditions of 80~100 DEG C, then keep the temperature 3~5 hours under the conditions of being placed in 1450~1550 DEG C, obtain
To corundum-mullite matter heat-barrier material.
In the present embodiment: the corundum is white fused alumina；The neutral atmosphere is nitrogen atmosphere.
Embodiment 4
A kind of corundum-mullite matter heat-barrier material and preparation method thereof.It is the step of preparation method described in the present embodiment:
The first step, by the corundum fine powder of 15~20wt%, the bauxite fine powder of 15~20wt%, 15~20wt% hydrogen-oxygen
Change the thermosetting phenolic resin mixing of aluminium, the quartz sand fine powder of 30~40wt%, the ammonium metavanadate of 1~5wt% and 1~5wt%
Uniformly, compression moulding under the conditions of 60~80MPa, then heat treatment 3~5 is small under the conditions of neutral atmosphere and 900~1100 DEG C
When, then through broken, ball milling and screening, ball milling material of the granularity less than 0.088mm and granularity are obtained as the particle of 0.088~0.5mm
Material.
Second step, by the ball milling material of 25~35wt%, the corundum fine powder of 10~20wt%, 5~10wt%
The bauxite fine powder, the ferro-silicon nitride of 5~10wt%, the hydroxyethyl cellulose of 0.1~0.5wt% and 40~50wt% water
Mixing, ball milling obtain slurry.
Third step, by the particulate material of 70~80wt%, the corundum fine powder of 1~5wt%, 10~15wt% institute
State ball milling material, the slurry of 5~10wt% is uniformly mixed, compression moulding under the conditions of 60~80MPa, then by compression moulding
Green body dry 18~24 hours under the conditions of 90~110 DEG C, then keep the temperature 3~5 hours under the conditions of being placed in 1450~1550 DEG C, obtain
To corundum-mullite matter heat-barrier material.
In the present embodiment: the corundum is white fused alumina；The neutral atmosphere is argon atmosphere.
Present embodiment has following good effect compared with prior art:
(1) raw material sources used by present embodiment are extensive, and production cost is low.
(2) present embodiment is reasonably combined by different material, the prefabricated ball milling with multistage pore-size distribution
Material and particulate material, then by prefabricated slurry, different types of particle and powder are combined, then in high-temperature process
In being formed in situ by mullite crystal whisker, further have adjusted the hole state in article construction, make present embodiment
The corundum-mullite matter heat-barrier material of preparation not only has compared with low bulk density, and has lower thermal coefficient.
(3) present embodiment effectively controls preparation method progress substep control in conjunction with stringent grain composition
The aperture structure of product and the intertexture distribution of mullite crystal whisker, the corundum-mullite matter for preparing present embodiment
Heat-barrier material intensity with higher.
The corundum-mullite matter heat-barrier material of present embodiment preparation is through detecting: bulk density is less than 1.5g/cm3；
Cold crushing strength is greater than 4MPa；Thermal coefficient is less than 0.25W/ (mK) within the scope of 200-1200 DEG C.
Therefore, present embodiment raw material sources are extensively and production cost is low, and prepared corundum-mullite matter is heat-insulated
Material has the characteristics that bulk density is low, intensity is high, heat-proof quality is excellent.
Claims (10)
1. a kind of preparation method of corundum-mullite matter heat-barrier material, it is characterised in that the step of preparation method is:
The first step, by the corundum fine powder of 10~20wt%, the bauxite fine powder of 10~20wt%, 10~20wt% hydroxide
The thermosetting phenolic resin mixing of aluminium, the quartz sand fine powder of 20~40wt%, the ammonium metavanadate of 1~10wt% and 1~10wt%
Uniformly, compression moulding under the conditions of 50~80MPa, then heat treatment 3~5 is small under the conditions of neutral atmosphere and 900~1200 DEG C
When, then through broken, ball milling and screening, ball milling material of the granularity less than 0.088mm and granularity are obtained as the particle of 0.088~0.5mm
Material；
Second step, will be described in the ball milling material of 20~40wt%, the corundum fine powder of 10~30wt%, 1~10wt%
The water mixing of bauxite fine powder, the ferro-silicon nitride of 1~10wt%, the hydroxyethyl cellulose of 0.1~1wt% and 40~60wt%,
Ball milling obtains slurry；
Third step, will be described in the particulate material of 60~80wt%, the corundum fine powder of 1~10wt%, 10~20wt%
Ball milling material, the slurry of 1~10wt% are uniformly mixed, compression moulding under the conditions of 50~80MPa, then by compression moulding
Green body is 12~24 hours dry under the conditions of 80~110 DEG C, then keeps the temperature 3~5 hours under the conditions of being placed in 1400~1600 DEG C, obtains
Corundum-mullite matter heat-barrier material；
The corundum is plate diamond spar or is white fused alumina, Al in the corundum2O3Content be greater than 99wt%, the corundum fine powder
Granularity be less than 0.088mm.
2. the preparation method of corundum-mullite matter heat-barrier material according to claim 1, it is characterised in that in the bauxite
Al2O3Content be greater than 60wt%, the granularity of bauxite fine powder is less than 0.088mm.
3. the preparation method of corundum-mullite matter heat-barrier material according to claim 1, it is characterised in that the aluminium hydroxide
Middle Al (OH)3Content be greater than 99wt%, granularity be less than 0.045mm.
4. the preparation method of corundum-mullite matter heat-barrier material according to claim 1, it is characterised in that in the quartz sand
SiO2Content be greater than 98wt%, the granularity of quartz sand fine powder is less than 0.088mm.
5. the preparation method of corundum-mullite matter heat-barrier material according to claim 1, it is characterised in that the ammonium metavanadate
Purity be greater than 99wt%.
6. the preparation method of corundum-mullite matter heat-barrier material according to claim 1, it is characterised in that the thermosetting property phenol
The viscosity at ambient temperature of urea formaldehyde is less than 15wt% less than 10000 centipoises, the moisture content of thermosetting phenolic resin.
7. the preparation method of corundum-mullite matter heat-barrier material according to claim 1, it is characterised in that the neutral atmosphere
It for nitrogen atmosphere or is argon atmosphere.
8. the preparation method of corundum-mullite matter heat-barrier material according to claim 1, it is characterised in that the ferro-silicon nitride
The content of middle Fe is 10-15wt%, and the granularity of ferro-silicon nitride is less than 0.088mm.
9. the preparation method of corundum-mullite matter heat-barrier material according to claim 1, it is characterised in that the ethoxy is fine
Ash content in dimension element is less than 5wt%.
10. a kind of corundum-mullite matter heat-barrier material, it is characterised in that the corundum-mullite matter heat-barrier material is according to power
Benefit require any one of 1~9 described in corundum-mullite matter heat-barrier material preparation method prepared by corundum-mullite matter
Heat-barrier material.
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| CN110526722A (en) * | 2019-09-02 | 2019-12-03 | 马鞍山利尔开元新材料有限公司 | A kind of moulding by casting high life corundum mullite rock collector nozzle of ladle brick and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381241A (en) * | 2008-10-16 | 2009-03-11 | 武汉科技大学 | Porous breathable refractory materials for upper nozzle and production method thereof |
| CN103553650A (en) * | 2013-10-11 | 2014-02-05 | 武汉科技大学 | Light mullite-silicon carbide refractory material and preparation method thereof |
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2018
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381241A (en) * | 2008-10-16 | 2009-03-11 | 武汉科技大学 | Porous breathable refractory materials for upper nozzle and production method thereof |
| CN103553650A (en) * | 2013-10-11 | 2014-02-05 | 武汉科技大学 | Light mullite-silicon carbide refractory material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110526722A (en) * | 2019-09-02 | 2019-12-03 | 马鞍山利尔开元新材料有限公司 | A kind of moulding by casting high life corundum mullite rock collector nozzle of ladle brick and preparation method thereof |
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