CN104478451B - A kind of preparation method of different special-shaped alumina hollow ball insulation product - Google Patents
A kind of preparation method of different special-shaped alumina hollow ball insulation product Download PDFInfo
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- CN104478451B CN104478451B CN201410764225.4A CN201410764225A CN104478451B CN 104478451 B CN104478451 B CN 104478451B CN 201410764225 A CN201410764225 A CN 201410764225A CN 104478451 B CN104478451 B CN 104478451B
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- hollow ball
- alumina hollow
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Abstract
The invention belongs to technical field of refractory materials, being specifically related to a kind of preparation method of different special-shaped alumina hollow ball insulation product, take alumina hollow ball as aggregate, adds MgF
2powder, fused white corundum fine powder, α-Al
2o
3powder and AlF
3powder makes matrix, makes bonding agent with water soluble amino resin or Water-soluble phenolic resin solution, and after batch mixing, shaping and drying, high-temperature firing forms.The present invention utilizes low temperature bond intensity in water soluble amino resin or water soluble phenol resin high, in conjunction with AlF
3and MgF
2to short nodulizing, thus make different special-shaped goods of the present invention have the advantages such as refractoriness under load height and high volume good stability, there is substance large and complex-shaped, yield rate high simultaneously.
Description
Technical field
The invention belongs to technical field of refractory materials, be specifically related to a kind of preparation method of different special-shaped alumina hollow ball insulation product.
Background technology
Be used in the alumina hollow ball insulation product of the kiln tops such as superhard alloy vacuum intermediate-frequency stove thermofin, box-type furnace, ultrahigh-temperature hydrogen molybdenum wire furnace, more and more to special shape future development, to avoid adopting the general shape alumina hollow ball insulation product of mark to build caused constructional difficulties by laying bricks or stones and being difficult to change the defects such as maintenance; Require that alumina hollow ball insulation product has the performances such as refractoriness under load height and high volume good stability simultaneously, fall the defect such as brick and sinking to avoid the inner lining of kiln caused by high temperature deformation.
Marking general shape alumina hollow ball insulation product usually used as inner lining of kiln, take alumina hollow ball as aggregate, with α-Al
2o
3powder is matrix, makes bonding agent with Tai-Ace S 150 or phosphoric acid solution etc., after batch mixing, shaping and drying, burns till at 1650 ~ 1700 DEG C of insulation 2 ~ 8h.Make bonding agent with alum liquor, the low temperature bond intensity difference in base substrate when sintering process, the general shape alumina hollow ball insulation product of mark can only be produced.Adopt phosphoric acid solution to make bonding agent, though can produce different special-shaped insulating product, use temperature is restricted, and phosphorus containg substances, when more than 1680 DEG C, produces and decomposes, discharge P
2o
5steam, thus pollution is produced to kiln, insulating product volume shrinks again simultaneously, causes the high volume poor stability of insulating product, produces the situation such as brick and sinking.
Summary of the invention
The present invention utilizes AlF
3powder and MgF
2the short nodulizing of powder, the feature that in water soluble amino resin and water soluble phenol resin, low temperature bond intensity is high, produces a kind of different special type alumina hollow ball insulation product.Different special type alumina hollow ball insulation product prepared by this preparation method has the high and feature that yield rate is high of high volume good stability, refractoriness under load.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of preparation method of different special-shaped alumina hollow ball insulation product, the feed composition of described alumina hollow ball insulation product and weight percent are: granularity is the alumina hollow ball 55 ~ 70% of 0.2 ~ 3mm, α-the Al of fused white corundum fine powder 0 ~ 20%, the granularity < 0.044mm of granularity < 0.088mm
2o
3powder 20 ~ 35%, the AlF of granularity < 0.044mm
3powder 0.2 ~ 3%, the MgF of granularity < 0.044mm
2powder 0 ~ 3%; Add water soluble amino resin or Water-soluble phenolic resin solution makes bonding agent, add-on is 8 ~ 12% of above-mentioned raw materials gross weight, and water soluble amino resin or Water-soluble phenolic resin solution solid content are 20 ~ 60%; By fused white corundum fine powder, MgF
2powder, α-Al
2o
3powder and AlF
3powder is placed in mixing equipment and mixes, the powder mix be uniformly mixed; Alumina hollow ball and described bonding agent are stirred after soaking, then add powder mix and mix; Adopt pressurization vibration mode to prepare the base substrate of desired size, through 100 ~ 110 DEG C of dryings after 24 ~ 36 hours, within 6 ~ 10 hours, burn till in 1600 ~ 1700 DEG C of insulations.Goods yield rate >=98 obtained; Refractoriness under load >1700 DEG C; Under 1650 DEG C of insulations, 3 hours conditions, heating permanent line is changed to 0.
The present invention makes bonding agent with water soluble amino resin and water soluble phenol resin, make full use of water soluble amino resin and water soluble phenol resin decomposition temperature is high, ensure the middle low temperature bond intensity of different special-shaped alumina hollow ball insulation product base substrate, and water soluble amino resin and water soluble phenol resin are completely decomposed of volatile when high temperature burns till, not residual lower low melting point in insulating product; With the addition of AlF simultaneously
3powder and MgF
2powder, AlF
3powder produces decomposition under middle high temperature, forms activated alumina amylaceous substance, facilitates insulating product and burn till, simultaneously AlF
3in fluorin volatilization fall, also residual lower low melting point in insulating product, and MgF
2powder produces and is decomposed to form activated magnesia under middle high temperature, activated magnesia and α-Al
2o
3powder effect, synthesize magnesium-aluminium spinel material, also promote insulating product to burn till, magnesium-aluminium spinel fusing point is up to 2135 DEG C simultaneously, negative effect can not be produced to insulating product performance, above-mentioned substance ensure that burning till of the different special-shaped alumina hollow ball insulation product that substance is large and complex-shaped, and makes goods have the high and feature that yield rate is high of high volume good stability, refractoriness under load.Overcome the middle low temperature bond intensity difference adopting alum liquor or calcium lignosulfonate solution to make bonding agent to bring, the defect of different special-shaped insulating product cannot be produced.And use the general shape alumina hollow ball insulation product of mark bring constructional difficulties to kilns such as ultrahigh-temperature hydrogen molybdenum wire furnaces and be difficult to change the defects such as maintenance.Adopt the phosphorus containg substances such as phosphoric acid solution to make bonding agent, it is high that such bonding agent also has middle low temperature bond intensity, can produce different special-shaped insulating product, but when working conditions is more than 1680 DEG C, phosphorus containg substances produces and decomposes, and discharges P
2o
5steam, thus pollution is produced to kiln, insulating product volume shrinks again simultaneously, produces kiln and falls brick and sinking.After adopting bonding agent of the present invention and short agglutinating matter, then overcome the defect that the phosphorus containg substances such as phosphoric acid solution make the low and high volume poor stability of the refractoriness under load brought of insulating product that bonding agent produces.
A preparation method for different special-shaped alumina hollow ball insulation product, the Al of alumina hollow ball
2o
3>=99%.
A preparation method for different special-shaped alumina hollow ball insulation product, the Al of fused white corundum fine powder
2o
3>=99%.
A preparation method for different special-shaped alumina hollow ball insulation product, α-Al
2o
3the Al of powder
2o
3>=99%.
A preparation method for different special-shaped alumina hollow ball insulation product, AlF
3the AlF of powder
3>=99%.
A preparation method for different special-shaped alumina hollow ball insulation product, MgF
2the MgF of powder
2>=99%.
A kind of preparation method of different special-shaped alumina hollow ball insulation product, feed composition and weight percent be preferably: granularity is the alumina hollow ball 60 ~ 70% of 0.2 ~ 3mm, α-the Al of fused white corundum fine powder 0 ~ 15%, the granularity < 0.044mm of granularity < 0.088mm
2o
3powder 23 ~ 34.5%, the AlF of granularity < 0.044mm
3powder 0.5 ~ 2%, the MgF of granularity < 0.044mm
2powder 0 ~ 2%; Add water soluble amino resin or Water-soluble phenolic resin solution makes bonding agent, bonding agent add-on is 9 ~ 11% of above-mentioned raw materials gross weight, and water soluble amino resin or Water-soluble phenolic resin solution solid content are 20 ~ 50%.
Embodiment
The present invention carries out optimum matching according to the distribution of the continuous sized particles of heap sum of discontinuous sized particles and accumulation to alumina hollow ball, adds MgF
2powder, fused white corundum fine powder, α-Al
2o
3powder and AlF
3powder, makes bonding agent with water soluble amino resin or Water-soluble phenolic resin solution, produces different special-shaped alumina hollow ball insulation product.In the following embodiments, the Al of alumina hollow ball
2o
3>=99%; Fused white corundum powder particle size < 0.088mm, Al
2o
3>=99%; α-Al
2o
3powder Particle Size < 0.044mm, Al
2o
3>=99%; AlF
3powder Particle Size < 0.044mm, AlF
3>=99%; MgF
2powder Particle Size < 0.044mm, MgF
2>=99%; By fused white corundum fine powder, MgF
2powder, α-Al
2o
3powder and AlF
3powder is placed in mixing equipment and mixes, the powder mix be uniformly mixed; Alumina hollow ball and described bonding agent are stirred after soaking, then add powder mix and mix; Adopt pressurization vibration mode to prepare the base substrate of desired size, through 100 ~ 110 DEG C of dryings after 24 ~ 36 hours, within 6 ~ 10 hours, burn till in 1600 ~ 1700 DEG C of insulations.
Embodiment 1: a kind of preparation method of different special-shaped alumina hollow ball insulation product.Material proportion is as shown in table 1 below, and wherein, described alumina hollow ball particle is by being less than or equal to 3mm, being greater than 2mm, be less than or equal to 2mm, be greater than 1mm, be less than or equal to 1mm, be greater than 0.2mm and carry out grating, and account for 25% of alumina hollow ball insulation product raw material gross weight respectively, 20%, 20%; Water soluble amino resin solution solid content is 50%; Product properties sees the following form 1.
Table 1 embodiment 1 and comparative example 1
Embodiment 2: a kind of preparation method of different special-shaped alumina hollow ball insulation product.Material proportion is as shown in table 2 below, and wherein, described alumina hollow ball particle is by being less than or equal to 3mm, being greater than 2mm, be less than or equal to 2mm, be greater than 1mm, be less than or equal to 1mm, be greater than 0.2mm and carry out grating, and account for 15% of alumina hollow ball insulation product raw material gross weight respectively, 25%, 20%; Water soluble amino resin solution solid content is 20%; Product properties sees the following form 2.
Table 2 embodiment 2 and comparative example 2
Embodiment 3: a kind of preparation method of different special-shaped alumina hollow ball insulation product.Material proportion is as shown in table 3 below, and wherein, described alumina hollow ball particle is by being less than or equal to 3mm, being greater than 2mm, be less than or equal to 2mm, be greater than 1mm, be less than or equal to 1mm, be greater than 0.2mm and carry out grating, and account for 25% of alumina hollow ball insulation product raw material gross weight respectively, 15%, 25%; Water-soluble phenolic resin solution solid content is 50%; Product properties sees the following form 3.
Table 3 embodiment 3 and comparative example 3
Embodiment 4: a kind of preparation method of different special-shaped alumina hollow ball insulation product.Material proportion is as shown in following table 44, and wherein, described alumina hollow ball particle is by being less than or equal to 3mm, being greater than 2mm, be less than or equal to 2mm, be greater than 1mm, be less than or equal to 1mm, be greater than 0.2mm and carry out grating, and account for 25% of alumina hollow ball insulation product raw material gross weight respectively, 25%, 250%; Water soluble alkyd resin solution and water-soluble epoxy resin solution add-on are respectively above-mentioned raw materials gross weight 4.5%, and the solid content of water-soluble epoxy resin solution is 25%, and the solid content of water soluble alkyd resin solution is 25%; Product properties sees the following form 4.
Table 4 embodiment 4 and comparative example 4
Claims (7)
1. the preparation method of a different special-shaped alumina hollow ball insulation product, it is characterized in that: feed composition and the weight percent of described different special-shaped alumina hollow ball insulation product are: granularity is the alumina hollow ball 55 ~ 70% of 0.2 ~ 3mm, α-the Al of fused white corundum fine powder 0 ~ 20%, the granularity < 0.044mm of granularity < 0.088mm
2o
3powder 20 ~ 35%, the AlF of granularity < 0.044mm
3powder 0.2 ~ 3%, the MgF of granularity < 0.044mm
2powder 0.5 ~ 3%; Add water soluble amino resin or Water-soluble phenolic resin solution makes bonding agent, add-on is 8 ~ 12% of above-mentioned raw materials gross weight, and water soluble amino resin or Water-soluble phenolic resin solution solid content are 20 ~ 60%; By fused white corundum fine powder, MgF
2powder, α-Al
2o
3powder and AlF
3powder is placed in mixing equipment and mixes, the powder mix be uniformly mixed; Alumina hollow ball and described bonding agent are stirred after soaking, then add powder mix and mix; Adopt pressurization vibration mode to prepare the base substrate of desired size, through 100 ~ 110 DEG C of dryings after 24 ~ 36 hours, within 6 ~ 10 hours, burn till in 1600 ~ 1700 DEG C of insulations; Goods yield rate>=98% obtained; Refractoriness under load >1700 DEG C; Under 1650 DEG C of insulations, 3 hours conditions, heating permanent line is changed to 0.
2. the preparation method of different special-shaped alumina hollow ball insulation product according to claim 1, it is characterized in that: feed composition and weight percent are: granularity is the alumina hollow ball 60 ~ 70% of 0.2 ~ 3mm, α-the Al of fused white corundum fine powder 0 ~ 15%, the granularity < 0.044mm of granularity < 0.088mm
2o
3powder 23 ~ 34.5%, the AlF of granularity < 0.044mm
3powder 0.5 ~ 2%, the MgF of granularity < 0.044mm
2powder 0.5 ~ 2%; Bonding agent add-on is 9 ~ 11% of above-mentioned raw materials gross weight, and water soluble amino resin or Water-soluble phenolic resin solution solid content are 20 ~ 50%.
3. the preparation method of different special-shaped alumina hollow ball insulation product according to claim 1 and 2, is characterized in that: the Al of alumina hollow ball
2o
3>=99%.
4. the preparation method of different special-shaped alumina hollow ball insulation product according to claim 1 and 2, is characterized in that: the Al of fused white corundum fine powder
2o
3>=99%.
5. the preparation method of different special-shaped alumina hollow ball insulation product according to claim 1 and 2, is characterized in that: α-Al
2o
3the Al of powder
2o
3>=99%.
6. the preparation method of different special-shaped alumina hollow ball insulation product according to claim 1 and 2, is characterized in that: AlF
3the AlF of powder
3>=99%.
7. the preparation method of different special-shaped alumina hollow ball insulation product according to claim 1 and 2, is characterized in that: MgF
2the MgF of powder
2>=99%.
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CN201410764225.4A CN104478451B (en) | 2014-12-15 | 2014-12-15 | A kind of preparation method of different special-shaped alumina hollow ball insulation product |
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CN104478451B true CN104478451B (en) | 2016-04-20 |
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JP2003192339A (en) * | 2001-12-27 | 2003-07-09 | Showa Denko Kk | Alumina particle, manufacturing method for the same and composition containing the same |
CN1789197A (en) * | 2005-10-28 | 2006-06-21 | 王家邦 | Preparation method of corundum hollow ball |
CN100337975C (en) * | 2005-10-28 | 2007-09-19 | 浙江大学 | Preparation method of brown corundum bollow ball |
CN103044045B (en) * | 2013-01-17 | 2014-06-18 | 武汉科技大学 | High-strength aluminum oxide light-weight heat insulation brick and preparation method thereof |
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