CN112079647B - Preparation method of ceramic fiber board - Google Patents
Preparation method of ceramic fiber board Download PDFInfo
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- CN112079647B CN112079647B CN202011088065.8A CN202011088065A CN112079647B CN 112079647 B CN112079647 B CN 112079647B CN 202011088065 A CN202011088065 A CN 202011088065A CN 112079647 B CN112079647 B CN 112079647B
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Abstract
The application discloses a ceramic fiber board and a preparation method thereof, wherein the ceramic fiber board is composed of aluminum silicate fibers, quartz fibers, magnesium hydroxide powder, high-purity aluminum oxide powder and low-temperature beta-type cordierite, the low-temperature beta-type cordierite is generated in the sintering process of the ceramic fiber board, and the low-temperature beta-type cordierite, part of the magnesium hydroxide powder and part of the high-purity aluminum oxide powder are filled in gaps between the aluminum silicate fibers and the quartz fibers. In the process of manufacturing the fiberboard containing aluminum silicate fibers and quartz fibers, magnesium hydroxide powder, high-purity aluminum oxide powder and silica sol are added to generate low-temperature beta-type cordierite after high temperature, and the low-temperature beta-type cordierite is combined with the fiber board of the aluminum silicate fibers and the quartz fibers to form a whole, so that the expansion coefficient is reduced, gaps between the quartz fibers and the aluminum silicate fibers are filled, beta-type cordierite is generated, and the ceramic fiberboard is pre-shrunk to achieve excellent thermal shock resistance and low-line shrinkage effects.
Description
Technical Field
The application relates to a preparation method of a ceramic fiber board.
Background
The aluminum silicate fiber has the advantages of lower price, high heat-resistant temperature, the highest long-term use temperature can reach 1100 ℃, but the shrinkage rate (linear shrinkage) of the fiber is higher, the shrinkage rate is less than or equal to 3 percent when tested at 1100 ℃, and the fiber has high heat shock resistance and higher expansion coefficient although the heat-resistant temperature is high: the ceramic fiber plate prepared by the method is 6 x 10 < -6 >, has extremely poor thermal shock resistance and is not suitable for being used in environments with high temperature difference (rapid cooling and rapid heating).
The quartz fiber has extremely excellent low expansion coefficient and thermal shock resistance, and the general quartz fiber can be used for a long time at 600-1050 ℃. The thermal expansion coefficient is also only: 0.54 x 10-6. However, the price is very expensive, the conventional price is 5-10 times and higher than that of aluminum silicate fibers, and if quartz fibers are used for replacing the high price, the long-term use temperature is lower than that of the aluminum silicate fibers, and the aluminum silicate fibers are not suitable for the requirements of a grade higher than the requirements of temperature resistance. However, in a reasonable application range, the quartz fiber cannot shrink seriously like other fibers, and experiments prove that the heat loss of the quartz fiber is not higher than 1.5 percent when tested at 1000 ℃.
How to combine the advantages of the two, the ceramic fiber board with high heat-resistant temperature, good thermal shock resistance and low cost is a problem to be solved.
Disclosure of Invention
The application aims to provide a preparation method of a ceramic fiber board with high heat-resistant temperature, good thermal shock resistance and low cost, which comprises the following steps:
step one: preparing the following components in percentage by weight, namely 10-60% of aluminum silicate fiber; 10-80% of quartz fiber; 5-25% of the sum of magnesium hydroxide powder and high-purity aluminum oxide powder, 5-20% of silica sol, and 5-40% of cationic starch accounting for the total weight of all components;
step two: crushing and mixing the aluminum silicate fibers and the quartz fibers, adding the silica sol, adding water to form a fiber mixture, fully mixing, simultaneously, fully mixing the magnesium hydroxide powder and the high-purity aluminum oxide powder with water, simultaneously, fully stirring the cationic starch with water to form a cationic starch aqueous solution, adding the mixed magnesium hydroxide powder and high-purity aluminum oxide mixture into the fiber mixture, fully mixing, and mixing the cationic starch aqueous solution into the fiber mixture to form an aggregate;
step three: vacuum adsorption molding is carried out on the agglomerate to manufacture a ceramic fiberboard blank;
step four: drying the ceramic fiber board blank;
step five: and sintering the dried ceramic fiber board blank to obtain the ceramic fiber board.
In certain embodiments, in the fifth step, the dried ceramic fiber board blank is heated to 960-1160 ℃ for at least 30min, and after the temperature of 960-1160 ℃ is maintained for at least 4 hours, the low-temperature beta-type cordierite is generated in the ceramic fiber board by high-temperature oxidation reaction of the magnesium hydroxide powder, the high-purity aluminum oxide powder and the silica sol, wherein the weight ratio of the low-temperature beta-type cordierite generated by the high-temperature oxidation reaction in the ceramic fiber board is 4-19%.
In certain embodiments, in the fifth step, the dried ceramic fiber board blank is heated to 650 ℃ from room temperature for not less than 2 hours, and the mixed air quantity is not less than 5 m/h; heating from 650 ℃ to 960-1160 ℃ to generate the low-temperature beta-cordierite, and ensuring the cooling rate to be less than or equal to 5 ℃/min before cooling to 200 ℃.
In certain embodiments, during the sintering of step five, the cationic starch is fully volatilized when the sintering temperature is greater than or equal to 650 ℃.
In certain embodiments, in step two, the fiber mixture is stirred for more than 10 minutes at a speed of more than or equal to 100r/min, the magnesium hydroxide powder and the high-purity aluminum oxide powder are added with water and stirred for more than 5 minutes, the cationic starch aqueous solution is stirred for more than 20 minutes at a speed of more than or equal to 150 revolutions per min, wherein the weight of water is more than or equal to 5 times that of the cationic starch, and the mixed magnesium hydroxide powder and the high-purity aluminum oxide mixture are added into the fiber mixture for continuous stirring for more than 5 minutes.
In certain embodiments, in step two, the cationic starch is mixed with the silica sol to agglomerate to form the agglomerates surrounding fibers and powder.
In certain embodiments, the aluminum silicate fiber has a density of 85-198kg/m, a total content of slag balls of not less than 0.212mm and not more than 55%, a permanent line change of heating of 1100 ℃ for 24hr and not more than 4%, the quartz fiber has a density of 100-210kg/m and a long-term temperature resistance of over 1200 ℃, wherein the content of silicon dioxide is not less than 98%, the magnesium hydroxide powder is 600-1200 meshes, the high-purity aluminum oxide powder is 500-1000 meshes, the purity requirement is not less than 99%, the content of sodium oxide in the silica sol is not more than 0.5%, and the pH value is 8-11.
The scope of the present application is not limited to the specific combination of the above technical features, but also covers other technical features formed by any combination of the above technical features or their equivalents. Such as those described above, and those disclosed in the present application (but not limited to) having similar functions, are replaced with each other.
Due to the application of the technical scheme, compared with the prior art, the application has the following advantages: in the process of manufacturing the fiberboard containing aluminum silicate fibers and quartz fibers, magnesium hydroxide powder, high-purity aluminum oxide powder and silica sol are added to generate low-temperature beta-type cordierite after high temperature, so that the low-temperature beta-type cordierite is combined with the fiberboard of the aluminum silicate fibers and the quartz fibers to form a whole, the gap between the quartz fibers and the aluminum silicate fibers is filled while the expansion coefficient is reduced, the beta-type cordierite is generated, and meanwhile, the ceramic fiberboard is pre-shrunk, so that the effects of excellent thermal shock resistance and low-line shrinkage are achieved, the heat-resistant temperature is high, the thermal shock resistance is good, and the cost is low.
Drawings
FIG. 1 is a schematic illustration of low temperature beta-cordierite filled in interstices between aluminum silicate fibers and quartz fibers;
wherein, 1, low temperature beta cordierite.
Detailed Description
The present application will be described in detail with reference to specific examples. The following examples are only illustrative of the present application and are not intended to limit the scope of the application.
The preparation method of the ceramic fiber board comprises the following steps:
step one: preparing the following components in percentage by weight, wherein the weight of the aluminum silicate fiber is 10-60%, and the fiber length is 3 mu m; 10% -80% of quartz fiber, and the fiber length is 5-10 mu m; 5-25% of the sum of magnesium hydroxide powder and alumina powder, wherein: the magnesium hydroxide powder is 2:1 compared with alumina powder, and then the cationic starch accounting for 5 to 40 percent of the total weight of all the components is added;
step two: crushing and mixing the aluminum silicate fibers and the quartz fibers, adding the silica sol, adding water to form a fiber mixture, fully mixing, stirring the fiber mixture for more than 10 minutes at the speed of more than or equal to 100r/min, simultaneously adding water with the weight of more than 10 times of the specific gravity of the powder into the magnesium hydroxide powder and the high-purity aluminum oxide powder, stirring and premixing for more than 5 minutes, fully mixing, simultaneously adding water into the cationic starch to form a cationic starch aqueous solution, fully stirring for more than 20 minutes at the speed of more than or equal to 150 r/min, wherein the weight of water is more than or equal to 5 times of that of the cationic starch, adding the mixed magnesium hydroxide powder and the high-purity aluminum oxide mixture into the fiber mixture, fully mixing, continuing stirring for more than 5 minutes, and mixing the cationic starch aqueous solution into the fiber mixture to form an agglomerate;
step three: vacuum adsorption molding is carried out on the agglomerate to manufacture a ceramic fiberboard blank;
step four: drying the ceramic fiber board blank;
step five: and sintering the dried ceramic fiber board blank to obtain the ceramic fiber board.
In the fifth step, the dried ceramic fiber board blank is heated to 960-1160 ℃ for at least 30min, and after the temperature of 960-1160 ℃ is kept for at least 4 hours, the low-temperature beta-cordierite is generated in the ceramic fiber board by high-temperature oxidation reaction of the magnesium hydroxide powder, the high-purity aluminum oxide powder and the silica sol.
In the fifth step, the dried ceramic fiber board blank is heated to 650 ℃ from room temperature for not less than 2 hours, and the mixed air quantity is not less than 5 m/h after preheating and sintering; heating from 650 ℃ to 960-1160 ℃ to generate the low-temperature beta-cordierite, and ensuring the cooling rate to be less than or equal to 5 ℃/min before cooling to 200 ℃.
The quartz fiber is preheated and sintered to ensure that the plate is preshrinked, so that the effects of excellent thermal shock resistance and low-line shrinkage are achieved.
The ceramic fiber board manufactured is high in heat-resistant temperature and good in thermal shock resistance, can be used for lining temperature wrapping of a high-temperature furnace, and can be applied to glass industry, flashboards of flues, lining temperature wrapping materials of shuttle kilns, glass forming dies and the like.
In the sintering process in the step five, when the sintering temperature is more than or equal to 650 ℃, the cationic starch is volatilized completely.
The silica sol is a dispersion of nano-scale silica particles in water or solvent, is a common raw material, and can be purchased without redundant description.
Embodiment one: the raw materials comprise the following components in parts by weight:
60% of aluminum silicate fibers;
10% of quartz fiber;
magnesium oxide powder + high purity alumina powder 20%;
10% of silica sol;
all the aforementioned components of the cationic starch account for 10% of the total weight.
In the ceramic fiber board, the weight ratio of the aluminum silicate fiber is 60%, the weight ratio of the quartz fiber is 10%, and the weight ratio of the generated low-temperature beta-type cordierite is 11.5%.
Note that: the following test results produced a difference value due to the difference in the grades of the raw materials used.
(1) When the ceramic fiber board obtained by the raw material preparation of example one had a molded volume weight of 300 kg/m:
the maximum long-term use temperature of the ceramic fiber board under the forming volume weight can reach 1100 ℃, which is equal to 1260 ceramic fiber board produced by ALCERA. And (3) performing a line shrinkage experiment at 1100 ℃ for 24hr, wherein the result value of the line shrinkage experiment is 1.9%, which is far lower than the national standard requirement value by less than or equal to 5%.
Thermal shock resistance test comparison: heating ceramic fiber plate in high temperature furnace to a certain temperature, keeping the temperature for 1hr, opening furnace door, pulling out ceramic fiber plate, exposing to air, cooling to 200deg.C, and rapidly heating (30deg.C/min). The steps are repeated.
Test results: the ceramic fiber board can be subjected to rapid cooling and rapid heating resistance test for more than 10 times at 800 ℃. The comparative panel was 1260 ceramic fiberboard produced by ALCERA and developed cracks after 1 test at 600 ℃.
(2) When the ceramic fiber board prepared by the raw material of example one had a molded volume weight of 400 kg/m:
the maximum long-term service temperature of the ceramic fiber board under the forming volume weight can reach 1100 ℃, which is equal to 1260 ceramic fiber board produced by ALCERA. And (3) performing a line shrinkage experiment at 1100 ℃ for 24hr, wherein the average value of the line shrinkage experiment results is 1.7%, which is far lower than the national standard requirement value by less than or equal to 5%.
Thermal shock resistance test comparison: heating ceramic fiber plate in high temperature furnace to a certain temperature, keeping the temperature for 1hr, opening furnace door, pulling out ceramic fiber plate, exposing to air, cooling to 200deg.C, and rapidly heating (30deg.C/min). The steps are repeated.
Test results: the ceramic fiber board can be subjected to rapid cooling and rapid heating resistance test for more than 10 times at the temperature of 750 ℃. The comparative panel was 1260 ceramic fiberboard produced by ALCERA and developed cracks after 1 test at 600 ℃.
(3) When the ceramic fiber board prepared by the raw material of example one had a molded volume weight of 600 kg/m:
the maximum long-term service temperature of the ceramic fiber board under the forming volume weight can reach 1100 ℃, which is equal to 1260 ceramic fiber board produced by ALCERA. And (3) performing a line shrinkage experiment at 1100 ℃ for 24hr, wherein the average value of the line shrinkage experiment results is 1.65%, which is far lower than the national standard requirement value by less than or equal to 5%.
Thermal shock resistance test comparison: heating ceramic fiber plate in high temperature furnace to a certain temperature, keeping the temperature for 1hr, opening furnace door, pulling out ceramic fiber plate, exposing to air, cooling to 200deg.C, rapidly heating (30deg.C/min), and repeating the steps.
Test results: the ceramic fiber board can be subjected to rapid cooling and rapid heating resistance test for more than 10 times at the temperature of 700 ℃. The comparative panel was 1260 ceramic fiberboard produced by ALCERA and developed cracks after 1 test at 600 ℃.
Embodiment two: the raw materials comprise the following components in parts by weight:
10% of aluminum silicate fibers;
60% of quartz fiber;
magnesium hydroxide powder and high-purity aluminum oxide powder 20%;
10% of silica sol;
all the aforementioned components of the cationic starch account for 10% of the total weight.
In the ceramic fiber board obtained through preparation, the weight ratio of the aluminum silicate fiber is 10%, the weight ratio of the quartz fiber is 60%, and the weight ratio of the low-temperature beta-type cordierite is 10.5%.
(1) When the ceramic fiber board prepared from the raw material of example two had a molded volume weight of 300 kg/m:
the maximum long-term use temperature of the ceramic fiber board under the forming volume weight can reach 1100 ℃, which is equal to 1260 ceramic fiber board produced by ALCERA. And (3) performing a line shrinkage experiment at 1100 ℃ for 24hr, wherein the average value of the line shrinkage experiment results is 1.5%, which is far lower than the national standard requirement value by less than or equal to 5%.
Thermal shock resistance test comparison: heating ceramic fiber plate in high temperature furnace to a certain temperature, keeping the temperature for 1hr, opening furnace door, pulling out ceramic fiber plate, exposing to air, cooling to 200deg.C, and rapidly heating (30deg.C/min). The steps are repeated.
Test results: the ceramic fiber board can be subjected to rapid cooling and rapid heating resistance test for more than 10 times at 1100 ℃. The comparative panel was 1260 ceramic fiberboard produced by ALCERA and developed cracks after 1 test at 600 ℃.
(2) When the ceramic fiber board prepared from the raw material of example two had a molded volume weight of 400 kg/m:
the maximum long-term use temperature of the ceramic fiber board under the forming volume weight can reach 1100 ℃, which is equal to 1260 ceramic fiber board produced by ALCERA. And (3) performing a line shrinkage experiment at 1100 ℃ for 24hr, wherein the average value of the line shrinkage experiment results is 1.4%, which is far lower than the national standard requirement value by less than or equal to 5%.
Thermal shock resistance test comparison: heating ceramic fiber plate in high temperature furnace to a certain temperature, keeping the temperature for 1hr, opening furnace door, pulling out ceramic fiber plate, exposing to air, cooling to 200deg.C, and rapidly heating (30deg.C/min). The steps are repeated.
Test results: the ceramic fiber board can be subjected to rapid cooling and rapid heating resistance test for more than 10 times at 1100 ℃. The comparative panel was 1260 ceramic fiberboard produced by ALCERA and developed cracks after 1 test at 600 ℃.
(3) When the ceramic fiber board prepared from the raw material of example two had a molded volume weight of 600 kg/m:
the maximum long-term service temperature of the ceramic fiber board under the forming volume weight can reach 1100 ℃, and the highest heat-resistant temperature of the ceramic fiber board produced by ALCERA is equal. And (3) performing a line shrinkage experiment at 1100 ℃ for 24hr, wherein the average value of the line shrinkage experiment results is 1.3%, which is far lower than the national standard requirement value by less than or equal to 5%.
Thermal shock resistance test comparison: heating ceramic fiber plate in high temperature furnace to a certain temperature, keeping the temperature for 1hr, opening furnace door, pulling out ceramic fiber plate, exposing to air, cooling to 200deg.C, and rapidly heating (30deg.C/min). The steps are repeated.
Test results: the ceramic fiber board can be subjected to rapid cooling and rapid heating resistance test for more than 10 times at 1100 ℃. The comparative panel was 1260 ceramic fiberboard produced by ALCERA and developed cracks after 1 test at 600 ℃.
The above embodiments are provided to illustrate the technical concept and features of the present application and are intended to enable those skilled in the art to understand the content of the present application and implement the same, and are not intended to limit the scope of the present application. All equivalent changes or modifications made in accordance with the spirit of the present application should be construed to be included in the scope of the present application.
Claims (5)
1. A preparation method of a ceramic fiber board is characterized in that: the method comprises the following steps:
step one: preparing the following components in percentage by weight, namely 10-60% of aluminum silicate fiber; 10-80% of quartz fiber; 5-25% of the sum of magnesium hydroxide powder and high-purity aluminum oxide powder, 5-20% of silica sol, and 5-40% of cationic starch accounting for the total weight of all components;
step two: crushing and mixing the aluminum silicate fibers and the quartz fibers, adding the silica sol, adding water to form a fiber mixture, fully mixing, simultaneously, fully mixing the magnesium hydroxide powder and the high-purity aluminum oxide powder with water, simultaneously, fully stirring the cationic starch with water to form a cationic starch aqueous solution, adding the mixed magnesium hydroxide powder and high-purity aluminum oxide mixture into the fiber mixture, fully mixing, and mixing the cationic starch aqueous solution into the fiber mixture to form an aggregate;
step three: vacuum adsorption molding is carried out on the agglomerate to manufacture a ceramic fiberboard blank;
step four: drying the ceramic fiber board blank;
step five: sintering the dried ceramic fiber board blank to obtain the ceramic fiber board; heating the dried ceramic fiber board blank from room temperature to 650 ℃ for not less than 2 hours, wherein the mixed air quantity is more than or equal to 5 m/h; heating from 650 ℃ to 960-1160 ℃ and maintaining the temperature of 960-1160 ℃ for at least 4 hours, generating low-temperature beta-type cordierite in the ceramic fiber board by high-temperature oxidation reaction of the magnesium hydroxide powder, the high-purity aluminum oxide powder and the silica sol, and ensuring the cooling rate to be less than or equal to 5 ℃/min after generating the low-temperature beta-type cordierite, wherein the weight ratio of the low-temperature beta-type cordierite generated by the high-temperature oxidation reaction in the ceramic fiber board is 4-19 percent.
2. The method for producing a ceramic fiber board according to claim 1, wherein: in the sintering process in the step five, when the sintering temperature is more than or equal to 650 ℃, the cationic starch is volatilized completely.
3. The method for producing a ceramic fiber board according to claim 1, wherein: in the second step, the fiber mixture is stirred for more than 10 minutes at the speed of more than or equal to 100r/min, the magnesium hydroxide powder and the high-purity alumina powder are added with water, stirred and premixed for more than 5 minutes, the cationic starch aqueous solution is stirred for more than 20 minutes at the speed of more than or equal to 150 revolutions per min, wherein the weight of water is more than or equal to 5 times that of the cationic starch, and the mixed magnesium hydroxide powder and the high-purity alumina mixture are added into the fiber mixture for continuous stirring for more than 5 minutes.
4. The method for producing a ceramic fiber board according to claim 1, wherein: in step two, the cationic starch is mixed with the silica sol to form agglomerates which encapsulate the fibers and powder.
5. The method for producing a ceramic fiber board according to claim 1, wherein: the density of the aluminum silicate fiber is 85-198kg/m, the total content of slag balls is more than or equal to 0.212mm and less than or equal to 55%, the permanent line change of heating is 1100 ℃ for 24hr and less than or equal to 4%, the density of the quartz fiber is 100-210kg/m, the long-term temperature resistance is above 1200 ℃, the content of silicon dioxide is more than or equal to 98%, the magnesium hydroxide powder is 600-1200 meshes, the high-purity aluminum oxide powder is 500-1000 meshes, the purity requirement is more than or equal to 99%, the content of sodium oxide in the silica sol is less than or equal to 0.5%, and the pH value is 8-11.
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| CN115611650A (en) * | 2022-10-10 | 2023-01-17 | 洛阳旭科新材料有限公司 | Method for manufacturing high-temperature-resistant ceramic fiber board |
| CN115557796A (en) * | 2022-11-10 | 2023-01-03 | 信阳中毅高热材料有限公司 | High-strength silicon fiber board and preparation method thereof |
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