CN105503216A - Preparation method of light and high-strength alumina bubble product - Google Patents
Preparation method of light and high-strength alumina bubble product Download PDFInfo
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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Abstract
The invention belongs to the technical field of insulating refractory materials and discloses a preparation method of a light and high-strength alumina bubble product. According to the preparation method of the light and high-strength alumina bubble product, alumina bubbles are adopted as aggregate of the light and high-strength alumina bubble product, and a porous substrate adopts calcium hexaluminate prepared from alumina and calcium oxide at the high temperature; the alumina is introduced by alumina micro powder; the calcium oxide is at least introduced by calcium aluminate cement; the alumina micro powder and the calcium aluminate cement are mixed, a pore-forming agent, a dispersing agent and water are added to the alumina micro powder and the calcium aluminate cement, and slurry is obtained after mixing; alumina bubbles are added to the slurry, and mixed slurry is obtained after mixing; then the mixed slurry is poured into a mold, left to stand and then demolded, and a green body is obtained; the green body is subjected to high-temperature sintering and natural cooling after drying. Shrinkage of the green body is reduced by use of volume expansion produced by synthesis of the calcium hexaluminate, and the high yield is realized.
Description
Technical field
The invention belongs to insulating refractory technical field, be specifically related to a kind of preparation method of high-strength light alumina hollow ball product.
Background technology
Alumina hollow ball insulation product is widely used in the high temperature kilns such as molybdenum silicide electric furnace, tungsten bar stove, high-temperature fuel gas periodic kiln and tunnel furnace as work liner; Usual alumina hollow ball insulation product is aggregate with alumina hollow ball, take alpha-aluminium oxide powder as matrix, adds appropriate bonding agent, through shaping, dry and burn till and be prepared from; After high temperature sintering, matrix is densifie state, causes the large (1.4 ~ 1.6g/cm of conventional aluminium oxide hollow ball insulating product density
3), thermal conductivity is high, and accumulation of heat is large, finally causes hot industry energy consumption too high.
For the problems referred to above, low density (0.6 ~ 1.0g/cm3) and the lower thermal conductivity (0.36 ~ 0.83Wm that pore realizes alumina hollow ball product is introduced in patent application (201410434384) in alumina host
-1k
-1); But porous alumina matrix causes alumina hollow ball product intensity lower, in sintering process base substrate shrinking percentage excessive (5 ~ 8%) easy to crack, distortion cause the problems such as yield rate is low.
Summary of the invention
For overcoming the deficiencies in the prior art, the object of this invention is to provide a kind of preparation method of high-strength light alumina hollow ball product.
The present invention adopts following technical scheme for completing above-mentioned purpose:
A preparation method for high-strength light alumina hollow ball product, described high-strength light alumina hollow ball product includes aggregate and porous matrix; Described aggregate adopts alumina hollow ball; Described porous matrix adopts the calcium hexaluminate for strengthening light aluminum oxide hollow ball product intensity; Described calcium hexaluminate is prepared from by aluminum oxide and calcium oxide high temperature; Described aluminum oxide is introduced by alumina powder; Described calcium oxide is at least introduced by aluminous cement; The add-on of described aluminous cement is 19.4 ~ 33.8% of alumina powder quality; By alumina powder, aluminous cement mixing, and add pore-forming material, dispersion agent and water in alumina powder, aluminous cement, after being uniformly mixed, obtain slurry; Alumina hollow ball is added in described slurry, after being uniformly mixed, obtains mixed slurry; Then mixed slurry is poured into mould leave standstill carry out the demoulding after 24 ~ 48 hours, obtain base substrate; After drying, high temperature sintering is carried out to base substrate, described alumina powder, aluminous cement, in the process of high temperature sintering Reactive Synthesis calcium hexaluminate, strengthen the intensity of light aluminum oxide hollow ball product, last naturally cooling obtains high-strength light alumina hollow ball product; The alumina hollow ball product density of preparation is 0.6 ~ 1.16g/cm
3, compressive strength is 4.83 ~ 13.42MPa, and thermal conductivity is 0.265 ~ 0.464Wm
-1k
-1.
Described alumina powder granularity is less than 325 orders, and purity is greater than 99%.
Described calcium oxide also can be introduced by calcium carbonate fine powder; The purity of described calcium carbonate fine powder is greater than 99%; The add-on of described calcium carbonate fine powder is 0 ~ 6% of alumina powder quality.
Described calcium oxide also can be introduced by calcium hydroxide micro mist; The purity of described calcium hydroxide micro mist is greater than 99%; The add-on of described calcium hydroxide micro mist is 0 ~ 4% of alumina powder quality.
Described water is deionized water, and add-on is 25 ~ 30% of alumina powder quality.
The composition of described aluminous cement and mass percent are: aluminum oxide 70%, calcium oxide 30%, granularity is less than 3000 orders.
Described pore-forming material is polystyrene spheres, and particle diameter is 0.1 ~ 0.5mm, and tap density is 0.04g/cm3, and add-on is 1.6 ~ 12.8% of alumina powder quality.
Described dispersion agent is the one in Sodium hexametaphosphate 99, polyoxyethylene glycol based polyalcohol FS10 and sodium polyacrylate, and add-on is 1 ~ 2% of alumina powder quality.
Described alumina hollow ball granularity is 1 ~ 3mm, and alumina content is greater than 99%, and add-on is 138.8 ~ 256.8% of alumina powder quality.
The sintering schedule of high-strength light alumina hollow ball product high temperature sintering is: with the ramp of 1 ~ 2oC/min, and is incubated 0.5 ~ 2h in 400 ~ 600oC; Then with the ramp of 1 ~ 3oC/min, and be incubated 3 ~ 6h in 1500 ~ 1650oC, naturally cool to room temperature.
A kind of preparation method of high-strength light alumina hollow ball product that the present invention proposes, adopts calcium hexaluminate as matrix, and in matrix, adds pore-forming material prepare light aluminum oxide hollow ball product; Aluminous cement aquation is utilized to realize base substrate solidification, utilize aluminum oxide and aluminous cement, calcium carbonate and calcium hydroxide at high temperature Reactive Synthesis calcium hexaluminate, strengthen the intensity of light aluminum oxide hollow ball product, the volumetric expansion utilizing synthesis calcium hexaluminate to produce reduces the contraction of base substrate, achieves high rate of finished products; Alumina hollow ball product density 0.6 ~ 1.16g/cm prepared by the present invention
3, compressive strength 4.83 ~ 13.42MPa, the low 0.265 ~ 0.464Wm of thermal conductivity
-1k
-1.
Embodiment
In conjunction with specific embodiments the present invention is illustrated:
Embodiment 1
1, weigh 1000g alumina powder, 388g aluminous cement, 64g pore-forming material, 20g polyoxyethylene glycol based polyalcohol FS10 and 270g water, be uniformly mixed 20 minutes, obtain slurry;
2, in slurry, add 1388g alumina hollow ball, be uniformly mixed 10 minutes, obtain mixed slurry; Mixed slurry pour into mould leave standstill carry out the demoulding after 24 hours, obtain base substrate;
3, after drying, base substrate is sintered, with the ramp of 2oC/min, and be incubated 0.8h in 500oC; Then with the ramp of 2oC/min, and be incubated 5h in 1550oC, naturally cool to room temperature; Through X-ray diffraction analysis, sample substrate part principal crystalline phase is calcium hexaluminate, and in addition containing small amounts aluminium and Calcium dialuminate, sample rate is 1.0g/cm3,1000oC thermal conductivity is 0.432Wm
-1k
-1, compressive strength 12MPa, shrinking percentage 0.1%, sample is without defects such as cracking, distortion.
Embodiment 2
1, weigh 1000g alumina powder, 194g aluminous cement, 60g calcium carbonate fine powder, 96g pore-forming material, 15g Sodium hexametaphosphate 99 and 280 water, be uniformly mixed 30 minutes, obtain slurry;
2, in slurry, add 1700g alumina hollow ball, be uniformly mixed 12 minutes, obtain mixed slurry; Mixed slurry pour into mould leave standstill carry out the demoulding after 36 hours, obtain base substrate;
3, after drying, base substrate is sintered, with the ramp of 1.5oC/min, and be incubated 1h in 400oC; Then with the ramp of 3oC/min and in 1500oC be incubated 6h, naturally cool to room temperature; Through X-ray diffraction analysis, sample substrate part principal crystalline phase is calcium hexaluminate, and in addition containing small amounts aluminium and Calcium dialuminate, sample rate is 0.82g/cm3,1000oC thermal conductivity 0.347Wm
-1k
-1, compressive strength is 7.6MPa, and shrinking percentage is 0.15%, and sample is without defects such as cracking, distortion.
Embodiment 3
1, weigh 1000g alumina powder, 194g aluminous cement, 40g calcium hydroxide micro mist, 128g pore-forming material, 10g sodium polyacrylate and 300 water, be uniformly mixed 40 minutes, obtain slurry;
2, in slurry, add 2080g alumina hollow ball, be uniformly mixed 15 minutes, obtain mixed slurry; Mixed slurry pour into mould leave standstill carry out the demoulding after 48 hours, obtain base substrate;
3, after drying, base substrate is sintered, with the ramp of 1oC/min, and be incubated 1h in 600oC; Then with the ramp of 1oC/min, and be incubated 4h in 1600oC, naturally cool to room temperature; Through X-ray diffraction analysis, sample substrate part principal crystalline phase is calcium hexaluminate, in addition containing small amounts aluminium and Calcium dialuminate, and sample rate 0.6g/cm3,1000oC thermal conductivity 0.265Wm
-1k
-1, compressive strength 4.83MPa, shrinking percentage is 0.18%, and sample is without defects such as cracking, distortion.
Embodiment 4
1, weigh 1000g aluminum oxide, 194g aluminous cement, 30g calcium carbonate, 20g calcium hydroxide, 16g pore-forming material, 18g polyoxyethylene glycol based polyalcohol FS10 and 250 water, be uniformly mixed 25 minutes, obtain slurry;
2, in slurry, add 2568g alumina hollow ball, be uniformly mixed 13 minutes, obtain mixed slurry; Mixed slurry pour into mould leave standstill carry out the demoulding after 30 hours, obtain base substrate;
3, after drying, base substrate is sintered, with the ramp of 1.2oC/min, and be incubated 0.5h in 450oC; Then with the ramp of 2.5C/min, and be incubated 3h in 1650oC, naturally cool to room temperature.Through X-ray diffraction analysis, sample substrate part principal crystalline phase is calcium hexaluminate, in addition containing small amounts aluminium and Calcium dialuminate, and sample rate 1.16g/cm3,1000oC thermal conductivity 0.464Wm
-1k
-1, compressive strength 13.42MPa, shrinking percentage is 0.11%, and sample is without defects such as cracking, distortion.
Claims (10)
1. a preparation method for high-strength light alumina hollow ball product, described high-strength light alumina hollow ball product includes aggregate and porous matrix; Described aggregate adopts alumina hollow ball; It is characterized in that: described porous matrix adopts the calcium hexaluminate for strengthening light aluminum oxide hollow ball product intensity; Described calcium hexaluminate is prepared from by aluminum oxide and calcium oxide high temperature; Described aluminum oxide is introduced by alumina powder; Described calcium oxide is at least introduced by aluminous cement; The add-on of described aluminous cement is 19.4 ~ 33.8% of alumina powder quality; By alumina powder, aluminous cement mixing, and add pore-forming material, dispersion agent and water in alumina powder, aluminous cement, after being uniformly mixed, obtain slurry; Alumina hollow ball is added in described slurry, after being uniformly mixed, obtains mixed slurry; Then mixed slurry is poured into mould leave standstill carry out the demoulding after 24 ~ 48 hours, obtain base substrate; After drying, high temperature sintering is carried out to base substrate, described alumina powder, aluminous cement be Reactive Synthesis calcium hexaluminate in the process of high temperature sintering, strengthen the intensity of light aluminum oxide hollow ball product, last naturally cooling obtains high-strength light alumina hollow ball product; The alumina hollow ball product density of preparation is 0.6 ~ 1.16g/cm
3, compressive strength is 4.83 ~ 13.42MPa, and thermal conductivity is 0.265 ~ 0.464Wm
-1k
-1.
2. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, is characterized in that: described alumina powder granularity is less than 325 orders, and purity is greater than 99%.
3. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, is characterized in that: described calcium oxide also can be introduced by calcium carbonate fine powder; The purity of described calcium carbonate fine powder is greater than 99%; The add-on of described calcium carbonate fine powder is 0 ~ 6% of alumina powder quality.
4. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, is characterized in that: described calcium oxide also can be introduced by calcium hydroxide micro mist; The purity of described calcium hydroxide micro mist is greater than 99%; The add-on of described calcium hydroxide micro mist is 0 ~ 4% of alumina powder quality.
5. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, it is characterized in that: described water is deionized water, add-on is 25 ~ 30% of alumina powder quality.
6. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, is characterized in that: the composition of described aluminous cement and mass percent are: aluminum oxide 70%, calcium oxide 30%, granularity is less than 3000 orders.
7. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, it is characterized in that: described pore-forming material is polystyrene spheres, particle diameter is 0.1 ~ 0.5mm, and tap density is 0.04g/cm3, and add-on is 1.6 ~ 12.8% of alumina powder quality.
8. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, it is characterized in that: described dispersion agent is the one in Sodium hexametaphosphate 99, polyoxyethylene glycol based polyalcohol FS10 and sodium polyacrylate, and add-on is 1 ~ 2% of alumina powder quality.
9. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, it is characterized in that: described alumina hollow ball granularity is 1 ~ 3mm, and alumina content is greater than 99%, add-on is 138.8 ~ 256.8% of alumina powder quality.
10. the preparation method of a kind of high-strength light alumina hollow ball product as claimed in claim 1, it is characterized in that: the sintering schedule of high-strength light alumina hollow ball product high temperature sintering is: with the ramp of 1 ~ 2oC/min, and be incubated 0.5 ~ 2h in 400 ~ 600oC; Then with the ramp of 1 ~ 3oC/min, and be incubated 3 ~ 6h in 1500 ~ 1650oC, naturally cool to room temperature.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107805081A (en) * | 2017-10-31 | 2018-03-16 | 湖南镭目科技有限公司 | A kind of porous ceramics and preparation method thereof |
| CN108675809A (en) * | 2018-07-02 | 2018-10-19 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of Ultralight corundum castable and preparation method thereof |
| CN110066166A (en) * | 2019-04-26 | 2019-07-30 | 无锡市亿洲耐火材料有限公司 | High-strength high fireclay insulating refractory of one kind and preparation method thereof |
| CN111018551A (en) * | 2020-01-10 | 2020-04-17 | 山东建筑大学 | Light heat-insulating castable for coke oven coal charging hole cover and preparation and use methods thereof |
| CN112209739A (en) * | 2020-09-29 | 2021-01-12 | 郑州大学 | Lightweight high-strength magnesium aluminate spinel hollow sphere porous ceramic and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805081A (en) * | 2017-10-31 | 2018-03-16 | 湖南镭目科技有限公司 | A kind of porous ceramics and preparation method thereof |
| CN108675809A (en) * | 2018-07-02 | 2018-10-19 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of Ultralight corundum castable and preparation method thereof |
| CN110066166A (en) * | 2019-04-26 | 2019-07-30 | 无锡市亿洲耐火材料有限公司 | High-strength high fireclay insulating refractory of one kind and preparation method thereof |
| CN111018551A (en) * | 2020-01-10 | 2020-04-17 | 山东建筑大学 | Light heat-insulating castable for coke oven coal charging hole cover and preparation and use methods thereof |
| CN111018551B (en) * | 2020-01-10 | 2021-12-07 | 山东建筑大学 | Light heat-insulating castable for coke oven coal charging hole cover and preparation and use methods thereof |
| CN112209739A (en) * | 2020-09-29 | 2021-01-12 | 郑州大学 | Lightweight high-strength magnesium aluminate spinel hollow sphere porous ceramic and preparation method thereof |
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